FINAL REPORT - DTIC · 2015. 11. 5. · FINAL REPORT Shelf Stable Epoxy Repair Adhesive SERDP Project WP-1763 FEBRUARY 2015 . Michael Cushman . Infoscitex Corporation . Distribution

FINAL REPORT Shelf Stable Epoxy Repair Adhesive

SERDP Project WP-1763

FEBRUARY 2015

Michael Cushman Infoscitex Corporation

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10-06-2014 Final Report 2009-2013

SHELF STABLE EXPOXY REPAIR ADHESIVE W912HQ-10-C-0019

WP-1763Michael Cushman

Infocitex Corporation 303 Bear Hill Road Waltham MA 02451

Strategic Environmental Research and Development Program 4800 Mark Center Drive Alexandria, VA 22350

SERDP

WP-1763

DISTRIBUTION A. Approved for public release: distribution unlimited.

The objective of this SERDP-funded research and development effort was to address the shelf-life shortcomings of currently available composite repair film adhesives. At military repair depots, currently used one-part adhesives have such a short shelf life that significant amounts expire and need to be discarded, contributing to a financial and environmentally costly waste stream. This effort aims to develop a one-part epoxy film adhesive that is stable at ambient temperatures for up to one year or at freezer temperatures for two years or longer.

A A A none207

Michael Cushman

(781)890-1338

Reset

Infoscitex Corporation Shelf Stable Epoxy Resin Adhesive

WP-1763 ii FINAL REPORT

Table of Contents 1. Abstract ....................................................................................................................1

2. Objective ..................................................................................................................2

3. Background ..............................................................................................................3

4. Materials and Methods .............................................................................................4

4.1 Model Adhesive System ..........................................................................................6

4.2 Adhesive Formulation ..............................................................................................6

4.2.1 Microencapsulation ..................................................................................................7

4.2.1.1 Prior Work Background ...........................................................................................8

4.2.1.2 In-Situ Polymerization .............................................................................................8

4.2.1.2.1 Investigation of Processing Parameters for In-Situ Generation of DMA ................9

4.2.1.2.2 In-Situ Polymerization of Epoxy Shell on Urone Crystal Surface ........................10

4.2.1.2.3 In-Situ Encapsulation of Urones with Adhesive Formulation ...............................11

4.2.1.3 Complex Coacervation Encapsulation ...................................................................11

4.2.2 Adhesive Formulation ............................................................................................13

4.2.2.1 Small-Scale Mixing ...............................................................................................14

4.2.2.2 Laboratory-Scale Mixing .......................................................................................14

4.2.2.2.1 Two Blade Dispersion Impeller .............................................................................15

4.2.2.2.2 Six Blade Rushton Impeller ...................................................................................15

4.2.2.2.3 Three Blade Left-Hand Axial Impeller ..................................................................16

4.3 Film Processing ......................................................................................................16

4.3.1 Lab-Scale Film Line Setup ....................................................................................16

4.3.1.1 Method ...................................................................................................................17

4.3.1.1.1 Run Preparation .....................................................................................................17

4.3.1.1.2 Processing ..............................................................................................................18

4.3.1.1.3 Inspection ...............................................................................................................19

4.3.2 Development of Single Lap Joint Cure Protocol ...................................................20

4.4 Adhesive Characterization .....................................................................................22

4.4.1 Differential Scanning Calorimetry (DSC) Analysis ...................................................22

4.4.2 Viscosity Analysis ......................................................................................................24

4.4.3 Storage Analysis .........................................................................................................25


WP-1763 iii FINAL REPORT

4.5 Performance Testing ..............................................................................................26

4.5.1 Mechanical Screening ................................................................................................26

4.5.2 Validation Testing ......................................................................................................28

5. Results and Discussion ..........................................................................................33

5.1 Microencapsulation Results ...................................................................................33

5.1.1 In-Situ Encapsulation .................................................................................................33

5.1.2 Encapsulation Using the Complex Coacervation Method .........................................43

5.2 Film Processing ......................................................................................................45

5.3 Adhesive Characterization .....................................................................................46

5.3.1 DSC Analysis .............................................................................................................46

5.3.2 Viscosity Analysis Results .........................................................................................49

5.3.3 Short-term Storage Analysis ......................................................................................50

5.3.4 Long-term Storage Analysis .......................................................................................50

5.4 Mechanical Testing ................................................................................................51

5.4.1 Mechanical Screening ................................................................................................51

5.4.2 Mechanical Performance Testing ...............................................................................53

6. Conclusions ............................................................................................................62

7. Literature Cited ......................................................................................................64

Appendix 1: Requirements Document .....................................................................................65

Appendix 2A: Viscosity Data for Monuron Based Samples ...................................................73

Appendix 2B: Viscosity Data for Fenuron Based Samples .....................................................98

Appendix 3A: DSC Data for Monuron Based Samples.........................................................116

Appendix 3B: DSC Data for Fenuron Based Samples ..........................................................137

Appendix 4A: Apparent Shear Strength of Single-Lap-Joint Adhesively Bonded Metal

Specimens by Tension Loading .............................................................................................165

Appendix 4B: Strength Properties of Double Lap Shear Adhesive Joints ............................177

Appendix 4C: Climbing Drum Peel for Adhesives ...............................................................181

Appendix 4D: Core Shear Properties of Sandwich Constructions by Beam Flexure ............187

Appendix 4E: Flatwise Tensile Strength of Sandwich Constructions ...................................191

Appendix 5: List of Scientific/Technical Publications ..........................................................197


WP-1763 iv FINAL REPORT

List of Figures Figure 1. Flow diagram depicting interrelation of R&D threads ................................................... 5 Figure 2. General reaction scheme for the production of BPA derived epoxy resins such as DER 331................................................................................................................................................... 6 Figure 3. Chemical structures of DCDA, monuron, fenuron, and TDU ........................................ 7 Figure 4. Urone Encapsulation by In-situ Polymerization ............................................................. 9 Figure 5. Schematic of a typical microencapsulation process using the complex coacervation method........................................................................................................................................... 12 Figure 6. Complex coacervation process developed by Thies Technologies for microencapsulation of the curing accelerant in IST’s shelf-stable epoxy resin adhesive ............. 13 Figure 7. Blades used for preliminary mixing trials: A) two blade dispersion impeller, B) six blade Rushton impeller, and C) three blade left-hand axial impeller ........................................... 14 Figure 8. Schematic of the hot melt adhesive processing setup ................................................... 17 Figure 9. A) Hot melt processing set-up with scrim and release film feed rolls, B) Processing set-up with aligned scrim and release film ......................................................................................... 18 Figure 10. Hot melt trough with liquefied resin in reservoir (indicated by arrow) during processing ..................................................................................................................................... 19 Figure 11. Micrograph of film prepreg with visible voids, good impregnation and only moderate fiber wetting. Good fiber wetting is exemplified by low-to-no visibility of the scrim fiber. ...... 20 Figure 12. Data used to determine best cure protocol for mechanical samples. .......................... 21 Figure 13. Ultimate strength for specimens cured at 248⁰F (120⁰C) as compared to specimens from the same formulation cured at 284⁰F (140⁰C). .................................................................... 22 Figure 14. Sample DSC curve for neat monuron. ........................................................................ 23 Figure 15. Viscometer setup used to determine the time to cure of two samples simultaneously 24 Figure 16. Viscosity curves of baseline paste adhesive measured at 104⁰F (40⁰C), 140⁰F (60⁰C) and 176⁰F (80⁰C). Tests were concluded once the percent torque of the motor reached 99% ... 25


WP-1763 v FINAL REPORT

Figure 17. Close up of a lap shear sample after testing. The plate on the left retained nearly all of the adhesive, while the plate on the right had virtually no prepreg material. Also, significant number of voids can be in the remaining adhesive on the left. ..................................................... 27 Figure 18. Lap shear specimen alignment fixture and compression slugs ................................... 27 Figure 19. Form and dimensions of Shear Strength of single-lap-joint test specimens [10] ....... 28 Figure 20. Form and dimensions of Shear Strength of single-lap-joint test specimens [11] ....... 29 Figure 21. A) Diagram of laminated test specimen assembly, B) Assembly of peeling apparatus [12] ................................................................................................................................................ 30 Figure 22. A) diagram of construction of samples, B) image of test rig used to test samples. ... 31 Figure 23. A) Maximum permissible dimensions of flatwise tension samples B) Flatwise tension setup .............................................................................................................................................. 32 Figure 24. NCO production in monuron samples ......................................................................... 34 Figure 25. NCO production in fenuron samples ........................................................................... 34 Figure 26. NCO production in samples of TDU ........................................................................... 35 Figure 27. DSC data for IST Run-2, epoxy encapsulated monuron. Average onset of melt temperature = 173.05⁰C, average peak melt temperature = 174.25⁰C, average heat of melting = 159.00 J/g. Active monuron in sample (comparison of heat of melting of IST Run-2 to raw monuron) = 109.68% .................................................................................................................... 36 Figure 28. DSC data for IST Run-3, epoxy encapsulated monuron. Average onset of melt temperature = 173.17⁰C, average peak melt temperature = 174.49⁰C, average heat of melting = 142.10 J/g. Active monuron in sample (comparison of heat of melting of IST Run-3 to raw monuron) = 98.02% ...................................................................................................................... 37 Figure 29. Micrograph of monuron encapsulated via in-situ polymerization ............................. 38 Figure 30. DSC data for IST Run-6, epoxy encapsulated monuron. Average onset of melt temperature = 173.10⁰C, average peak melt temperature = 174.38⁰C, average heat of melting = 117.27 J/g. Active monuron in sample (comparison of heat of melting of IST Run-6 to raw monuron) = 80.89% ...................................................................................................................... 39 Figure 31. DSC data for IST Run-7, epoxy encapsulated monuron. Average onset of melt temperature = 167.67⁰C, average peak melt temperature = 169.97⁰C, average heat of melting = 187.23 J/g. Active monuron in sample (comparison of heat of melting of IST Run-7 to raw monuron) = 80.89% ...................................................................................................................... 41


WP-1763 vi FINAL REPORT

Figure 32. DSC data for IST Run-8, epoxy encapsulated monuron. Average onset of melt temperature = 184.85⁰C, average peak melt temperature = 186.97⁰C, average heat of melting = 107.57 J/g. Active monuron in sample (comparison of heat of melting of IST Run-7 to raw monuron) = 97.26% ...................................................................................................................... 42 Figure 33. Viscosity measurements for IST Run-3, IST Run-6 and neat monuron baseline mixtures. The time to 100% torque for each sample was: 28 hrs 5 mins (IST Run-3), 29 hrs 5 mins (IST Run-6) and 40 hrs 5 mins (Baseline) ........................................................................... 43 Figure 34. Photograph of film 005_142 ........................................................................................ 46 Figure 35. DSC exotherms for A) neat monuron, B) encapsulated monuron, C) neat fenuron and D) encapsulated fenuron ............................................................................................................... 47 Figure 36. Residual mechanical strength after short term storage exposure to 60⁰C for baseline and SSA film samples ................................................................................................................... 50 Figure 37. Residual mechanical strength after long term storage exposure to both ambient conditions and 90⁰F (32⁰C) for baseline and SSA film samples .................................................. 51 Figure 38. Comparison of performance of batches of capsules with regards to single-lap-joint strength and time to cure, as determined via viscosity analysis. .................................................. 53 Figure 39. Comparison of performance of large batches of capsules with regards to single-lap-joint strength and time to cure, as determined via viscosity analysis. .......................................... 54 Figure 40. Comparison of the results from the single-lap-joint testing for both the baseline formulation and the SSA formulation (CT-0013-117).. ............................................................... 55 Figure 41. Comparison of the results from the double lap shear testing for both the baseline formulation and the SSA formulation (CT-0013-117). ................................................................ 56 Figure 42. Comparison of the results from the climbing drum peel testing for both the baseline film and the SSA film (CT-0013-117). ......................................................................................... 57 Figure 43. Comparison of the core shear maximum facing strength for both the baseline film and the SSA film (CT-0013-117). ....................................................................................................... 59 Figure 44. Comparison of the core shear properties, specifically maximum facing strength for both the baseline formulation and the SSA formulation (CT-0013-117). .................................... 60 Figure 45. Graph of single lap shear tests (ASTM D1002-05) conducted on film samples stored side by side at 90°F (32⁰C) for incremented time intervals and cured at 284⁰F (140°C) ............ 62


WP-1763 vii FINAL REPORT

List of Tables Table 1. Baseline epoxy resin system used for viscosity trials. ................................................... 13 Table 2. Baseline epoxy resin system used for film production. ................................................. 26 Table 3. Summary of validation mechanical testing and post-curing conditions. ....................... 29 Table 4. Solubility of TDU in various solvents ............................................................................ 40 Table 5. Summary of capsules made via complex coacervation ................................................. 44 Table 6. Summary of films prepared ............................................................................................ 45 Table 7. Summary of encapsulated materials (complex coacervation method) .......................... 48 Table 8. Summary of viscosity results (time to cure) of all paste samples. Samples marked with an (*) were stopped before full cure was attained due to project time constraints. ...................... 49 Table 9. Summary of single-lap-joint strength of all films tested. .............................................. 52 Table 10. Shear strength of single-lap-shear results for both the baseline and SSA films. ......... 55 Table 11. Strength properties of double lap shear adhesive joints by tension loading. ............... 56 Table 12. Climbing drum peel strength of both the baseline film and the SSA film (CT-0013-117) ............................................................................................................................................... 58 Table 13. Core shear properties of sandwich samples for both the baseline and SSA (CT-0013-117) films. ..................................................................................................................................... 59 Table 14. Flatwise tensile strength of sandwich constructions of both the baseline and SSA (CT-0013-117) films. ............................................................................................................................ 61 Table 15. Test matrix for comparitive study between baseline and SSA formulations. A ‘Pass’ indicates that the SSA formulation had comparable or better mechanical test results as the baseline. ........................................................................................................................................ 63


WP-1763 viii FINAL REPORT

List of Acronyms ACN Acetonitrile ASTM American Society for Testing and Materials BPA Bisphenol A DCDA Dicyanamide DETA Diethylenetriamine DMA Dimethylamine DOD Department of Defense DSC Differential scanning calorimetry ECH Epichlorohydrin FTIR Fourier transform infrared IC Iota carrageenan ID Inner diameter IST Infoscitex Corporation KC Kappa carrageenan MET Minimal exposure time NCO Isocyanate NS Not soluble PDDACL Poly(dimethyldiallylammonium chloride) PD Partially decomposed PS Partially soluble R&D Research and development S Soluble SAE Society of Automotive Engineers SERDP Strategic Environmental Research and Development Program SSA Shelf Stable Adhesive SWRI Southwest Research Institute TDU 2,4-toluene bis dimethyl urea


WP-1763 ix FINAL REPORT

Keywords Shelf-stable, epoxy, microencapsulated, repair adhesive


WP-1763 x FINAL REPORT

Acknowledgements This research was supported fully by the Department of Defense, through the Strategic Environmental Research and Development Program (SERDP).


WP-1763 1 FINAL REPORT

1. Abstract The objective of this SERDP-funded research and development effort was to address the shelf-life shortcomings of currently available composite repair film adhesives. At military repair depots, currently used one-part adhesives have such a short shelf life that significant amounts expire and need to be discarded, contributing to a financial and environmentally costly waste stream. This effort aims to develop a one-part epoxy film adhesive that is stable at ambient temperatures for up to one year or at freezer temperatures for two years or longer. The technical program focused on enhancement of current epoxy resin-based film adhesives through modification of the accelerator package. This was accomplished through formulation of controlled release encapsulated accelerators into a one-part epoxy resin. Henkel Aerospace film adhesive product Hysol EA 9696 was chosen as the model epoxy resin system against which to develop accelerator modifications. A baseline was formulated using the primary components of the Hysol EA 9696 resin system matrix and fenuron accelerator. The experimental shelf-stable adhesive (SSA) was formulated in a manner identical to the baseline; the only differentiating factor was that the fenuron accelerator was encapsulated in a controlled release shell. Two sets of tests were performed to establish the feasibility of encapsulating the accelerant in a one-part epoxy adhesive system. The first set of tests focused on evaluating the long-term shelf stability of the SSA adhesive. The second set of tests focused on assessing the mechanical performance of the SSA adhesive. The tests performed were based upon both standard AMS-A-25463 [1] as well as input from technical advisors. This standard provides all requisite guidance for the chemical and physical performance of film adhesives. The model epoxy resin system selected is classified as a Type I adhesive. Accordingly, performance metrics for the SSA film was tested based on Type I requirements. The long-term stability of each adhesive was assessed at a sustained elevated temperature (32°C/90°F). The SSA and baseline formulations were compared at each time interval using single lap shear testing (ASTM D1002) [10] of cured specimens. Each sample set consisted of at least nine specimens. A matrix of five different mechanical tests was performed on the baseline and candidate SSAs under six test conditions. All of this testing was performed on samples that were prepared with new adhesive that was meticulously stored at 10°F. A summary of the test results are shown in Table 3. All operational mechanical tests were performed at third-party facilities. The combination of the results from both the operational mechanical and shelf stability tests show that the one-part SSA has potential as a viable upgrade for the currently available one-part adhesive systems. The SSA has been demonstrated to retain at least 75% of its adhesive strength when stored at 90°F for a year. When compared to the baseline formulated with an unencapsulated accelerant, the stability of the SSA formulation offers a significant advantage. If stored in a freezer, it is anticipated that the SSA will be stable for well over two years. The data confirms that the capsules are not having a deleterious effect on the performance of the adhesive. In every test, the mechanical properties of the conditioned SSA samples were comparable or better than those of the baseline formulation. The test program has shown that the SSA formulation with encapsulated accelerator provides a significant shelf stability advantage over the baseline without sacrificing mechanical performance.



2. Objective The objective of this SERDP funded research and development effort was to address the shortcomings of the currently available composite repair film adhesives, specifically with regards to the room temperature shelf life. Achieving this objective will contribute to SERDP’s charter to facilitate the development of environmentally-beneficial technology, as it promises to aid in the reduction of hazardous waste associated with aircraft repair processes. Specifically, this effort aimed to develop a one-part epoxy film adhesive that is stable at ambient temperatures for up to one year and meets the mechanical performance requirements for aerospace adhesives.



3. Background Conventional repair of composites used in military applications results in the generation of significant amounts of solid waste. In a SERDP funded research effort to quantify the environmental impact of composite repair operations, it was determined that millions of pounds of hazardous waste were generated. Hazardous waste disposal estimates for adhesives alone were estimated at 22 million pounds at a cost of over $100M [ARL-TR-2139, 1999]. Since the issuance of the report, the composite structures have proliferated in aerospace applications. Improvement of composite adhesive technologies is clearly needed to reduce environmental burdens and abatement costs. Repair facilities use one-part epoxy based adhesives extensively for metal to metal and honeycomb repairs. The costs associated with these processes are limiting the use of composite materials within the industry. One-part adhesive systems are primarily used within industry as they provide better control, reliability and take much less time to prepare than two-part systems. The major drawback, however, is that these systems slowly cure during storage and as a result have an extremely short shelf life (2-12 months), even when stored in freezers. Repair depots are required to employ extensive inventory and quality control to ensure that repair adhesives are not expired. Currently supplied film adhesives are only available in minimum quantities that are greater than the demands of the repair depot. Due to the combination of diverse quantity, poor shelf stability and large minimum quantity procurement requirements of military aerospace composite repair operations, much of the epoxy film adhesive is expiring before it can be used. According to Ogden ALC at Hill AFB, more than 50% of procured film repair adhesive is ultimately discarded because it has expired or was exposed to ambient temperatures for too long. No improvements have been achieved to remedy this inefficiency. A one-part epoxy film adhesive system with improved shelf stability would greatly reduce the environmental impact of repair operations and reduce materiel procurement costs across the DoD. Applications of this adhesive technology could be utilized at DoD facilities such as Ogden and Warner-Robbins ALC and at commercial repair facilities such as would be used by OEM companies like Boeing. Boeing uses one-part film adhesives for a wide variety of applications. Some manufacturing operations are more efficient, discarding less expired film. Commercial and military aircraft repair operations at Boeing experience very similar problems with film expiration and hazardous waste. At Ogden ALC over 720 pounds of EA 9696 film adhesive are purchased on contract every year. Individual small purchases that are less than $3,000 may be purchased via a government purchase card (GPC) and are not easily collected, so the total yearly purchase could be significantly higher. Robins ALC has purchased over 960 pounds of EA 9696 this year.



4. Materials and Methods The technical program focused on enhancement of current epoxy resin-based film adhesives through modification of the accelerator package. This was accomplished through formulation of controlled release encapsulated accelerators into a one-part epoxy resin. Henkel Aerospace film adhesive product Hysol EA 9696 was chosen as the model epoxy resin system against which to develop accelerator modifications. A baseline was formulated using the primary components of the Hysol EA 9696 resin system matrix and accelerator (fenuron). The experimental SSA material was formulated in a manner identical to the baseline; however, the only differentiating factor was that the fenuron accelerator was encapsulated in a controlled release shell (see Section 4.2.1 for details on this material). There were three primary thrusts to the research and development effort:

1. Adhesive Formulation 2. Film Processing 3. Performance Validation

The interrelation of these thrusts is shown schematically in Figure 1. Microencapsulant formulation was the foundation of adhesive development. Efforts during the first year of this project focused heavily on evaluating samples with various encapsulant shell materials produced via both complex coacervation and via in-situ polymerization. Activities during subsequent years focused on down-selecting the best candidate for validation activities, which included scaled-up batch production, shelf-stability testing, film production and mechanical testing. Film processing activities during the project involved laboratory-scale quantities. These films were used for the purpose of assessing the impact of candidate shell materials on resultant film mechanical properties. One key accomplishment was the demonstrated reproduction of scaled-up batches with consistent thermal and mechanical properties. A preliminary requirements document was drafted to ensure the technical program yielded meaningful results that could be effectively compared to the current state-of-the-art and guiding military specifications. Requirements were based upon AMS-A-25463 [1], an SAE standard that replaced MIL-A-25463B, Notice 1 [2] to provide guidance on adhesive films used in aerospace structural construction. Key property requirements incorporated into the document included: cure time, shelf-life, peel strength, flatwise tensile strength, flexural strength and resistance to heat, fuel and humidity. In addition, non-functional requirements for the adhesive were defined to include environmental impact, cost and domestic supply. The final Requirements Document is provided in Appendix 1.



Figure 1. Flow diagram depicting interrelation of research and development threads

Create Microencapsulant Formulation

" f f 0

~ ,-NO N "S - NO E ,. ~

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WYE~ ~ss? Charaet.;.riza Chme~r~• ~YES-+ Charaeta.riu M icrocapsule Adhes1ve Processibil~y

NO

~ ,---YES r.i echanical YES Tes<ing

! ! ! Film

Film Film Formulabon

Production Production

Opeimization Process R101

I? Optimizabon

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~ Mechanical ~ Q. Testing ( 1ST) YES

NO

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~ Mechan ical

~ Testing (NGC)



4.1 Model Adhesive System A commercially available product was selected as the model epoxy resin system to ensure the technical program yielded meaningful results that could be effectively compared to the current state-of-the-art and guiding military specifications. Henkel’s epoxy resin system, Hysol EA 9696 was selected as the model epoxy resin system. Hysol EA 9696 is a modified epoxy film adhesive designed for use at temperatures up to 250⁰F (121⁰C) in the joining of various structures, including metal sheet and honeycomb sandwich composite structures. Key features of this material include:

• Cure from 225⁰F to 265⁰F (107⁰C to 129⁰C) • 12-month shelf-life at 0⁰F (-18⁰C) • 60-day shelf-life at 77⁰F (25⁰C) • 30-day shelf-life at 90⁰F (32⁰C)

Based on AMS-A-25463 [1], this material would be classified as a Type I adhesive, having an intended long-term use at -67⁰F (-55⁰C) to 180⁰F (82⁰C). 4.2 Adhesive Formulation This project aimed to develop an epoxy resin film adhesive with improved shelf-stability. Focus was placed on a standard resin for the purposes of the development effort. Specifically, DOW D.E.R. 331 was selected as the primary epoxy resin. D.E.R. 331 is a liquid epoxy resin derived from the reaction of epichlorohydrin (ECH) and bisphenol A (BPA) (Figure 2). In addition to D.E.R. 331, IST identified DOW D.E.R. 661, a solid resin comparable to D.E.R. 331 in chemistry and performance, for use in controlling resin viscosity during film processing.

Figure 2. General reaction scheme for the production of BPA derived epoxy resins such as DER 331

+

O O[ [

n

O O

O O

ECH BPA

Epoxy Resin



The resin, catalyst, accelerator and other additives are machine mixed and stored (typically refrigerated or frozen) until use for standard one-part epoxy resin systems. In the interest of reducing the potential for confounding of results due to too many variables, it was decided that catalyst chemistry be held constant. Dicyanamide (DCDA) was selected for this function because it is an established curative. Its chemical structure is provided in Figure 3.

DCDA Monuron Fenuron TDU

Figure 3. Chemical structures of DCDA, monuron, fenuron, and TDU Three urone accelerators were identified for use in the project. Monuron (N-(4-chlorophenyl)-N,N-dimethyl urea), a legacy accelerator, served as the baseline accelerator. Data pertaining to adhesives featuring this accelerator provided valuable data for the project, however, it will not be directly useful for downstream commercialization and transition since monuron has been phased out of new product development. Two additional accelerators were encapsulated: fenuron (phenyl dimethyl urea) and 2,4-toluene bis dimethyl urea (TDU). Chemical structures of these selected accelerators can be seen in Figure 3. After initial microencapsulation studies with monuron, described in the next section, IST concentrated the rest of the development on fenuron containing formulations. Fenuron is a de-chlorinated version of monuron, thus representing a safer product. According to manufacturers, it has a higher activity than monuron. TDU was also recommended for use by Henkel based on its anticipated high activity.

Microencapsulation The materials and processes selected to microencapsulate the accelerant played a critical role in the efficacy of the encapsulation approach. During previous efforts, candidate encapsulant materials were evaluated in a system that used monuron as the accelerator. To make use of this benchmark performance data on the current project, IST screened encapsulant materials using monuron as well. This approach was deemed a viable path because monuron is chemically similar to fenuron. Encapsulation efforts focused on complex coacervation (performed by Thies Technologies) and in-situ polymerization (performed by Infoscitex). Complex coacervation efforts during the first year of the project focused primarily on using mixtures of kappa carrageenan (KC) or iota carrageenan (IC) with poly (dimethyldiallylammonium chloride) (PDDACL) while efforts during subsequent years focused on utilizing gelatin. KC and IC are polysaccharides extracted from seaweeds that form gels at room temperature. They were chosen to provide a more thermally stable barrier to premature migration or leakage of accelerant into the epoxy resin [3]. Monuron was successfully encapsulated at concentrations greater than 50 wt% within four

NN

=CC



formulations chosen: KC-PDDACL, IC-PDDACL, gelatin-KC-PDDACL and gelatin-gum arabic. The capsules were 10-25 µm in size. Analysis via differential scanning calorimetry (DSC) showed that the monuron within the capsules behaved very similarly to neat monuron, as evidenced by a sharp melting peak at its melting temperature of 350⁰F (178⁰C). The weight fraction of the microcapsules corresponding to monuron can be calculated by assuming that the enthalpy of melting (ΔH) is proportional to the amount of accelerator.

Prior Work Background Microencapsulation is used in a wide variety of applications to isolate materials from their surroundings. There are a multitude of techniques that have been developed to encapsulate solids, liquids and gases. Prior research has attempted to develop one-part, shelf-stable epoxy resin systems using microencapsulation of accelerators or latent curing agents. Southwest Research Institute (SWRI) developed a monuron encapsulate using a paraffinic wax shell material. This microencapsulated material was intended for use in an epoxy film adhesive [4]. The product suffered from two shortcomings: 1. Diffusion of epoxy resin through the shell limited the shelf-life – as storage temperature

increased, the rate of reaction increased and thus decreased the shelf-life of the adhesive.

2. Monuron was released from the microcapsule by melting the wax encapsulant – the wax became a contaminant in the adhesive and tended to migrate to the adhesive/substrate bond line thus adversely affecting adhesion strength.

Previous experience with film adhesive research [5, 6] indicated that the microcapsule shell must be capable of withstanding brief high temperature excursions (up to 250⁰F/121⁰C) for almost one minute to be processed into a hot-melt product on prototype film adhesive manufacturing lines. The microcapsule shell must have outstanding barrier properties and must completely cover the surface of the active material. Curing reactions will occur if as little as 1% of the accelerant escapes from the microcapsule. A highly cross-linked polymer is best for this application. It should be noted that these materials will not be amenable to release using a simple thermal trigger, such as the curing heat cycle itself. The microcapsule must be small enough to reside within an adhesive film during the repair process and the encapsulant material that remains within the resin after curing must not adversely affect the mechanical properties of the finished composite. Work from previous efforts found that particles with sizes of 20-50 μm, loaded into test paste adhesive specimens at a loading of 6 wt%, did not adversely impact the tensile lap shear and floating roller peel strength properties of the film adhesive [5, 6]. Since these particles are very small, they can be easily opened using a brief and temporary thermal spike to rupture the capsules and release the accelerant before the curing reaction begins.

In-Situ Polymerization The objective of this approach was to encapsulate accelerant particles in a controlled, reproducible manner in a uniform epoxy polymer shell compatible with the bulk of adhesive. Monuron heated in absence of DCDA can contain up to 0.8 % DMA [7]. It was hypothesized that this small amount of DMA could be used for in-situ formation of a protective capsule on the



surface of urone crystals. As shown in Figure 4, upon moderate heating of urone, DMA forms within a urone crystal and migrates to it surface via molecular diffusion. On the urone crystal surface, DMA reacts with an epoxy monomer, such as epichlorohydrin (ECH, 1-chloro-2,3-epoxypropane) or an epoxy resin. This triggers the formation and growth of epoxy polymer chains on the urone crystal surface. The in-situ polymerization process can be stopped via:

• Quenching/termination of the reaction (addition of reactive amine, such as diethylenetriamine (DETA));

• Exhaustion of available polymer precursor (monomer, resin) and quenching; • Removal of the polymer precursor (evaporation or draining) and quenching.

Figure 4. Urone Encapsulation by In-situ Polymerization To verify the proposed approach, three experiments were performed. First, determine the optimal processing parameters for the in-situ generation of DMA. Second, determine the feasibility of in-situ polymerization of an epoxy shell on the urone crystal surface. And finally, determine the feasibility of generating encapsulated urone within the body of an adhesive formulation. 4.2.1.2.1 Investigation of Processing Parameters for In-Situ Generation of DMA The in-situ method required the generation of a sufficient amount of DMA while preserving the bulk of the urone from thermal decomposition. Three urones were investigated during this experiment: monuron, fenuron and TDU. It was determined that the raw urone materials contained 5 to 10 wt% of insoluble organic matter, potentially proprietary stabilizers. Based on the literature available regarding monuron thermal decomposition, the optimal reaction temperature should be 122⁰F to 158⁰F (50⁰C to 70⁰C), with a minimal exposure time (MET) of less than one hour. Due to the similarity of each of the urone compounds, it was anticipated that



these reaction parameters would be comparable for all three of the urones investigated. For each of the reaction temperatures studied, urone samples weighing approximately 0.1 g were produced in triplicate at three different exposure times (30 minutes, 45 minutes, and 60 minutes). Preliminary analysis of the neat urone materials showed that they each contained residues that were insoluble in organic solvents. Additionally, Fourier transfer infrared spectroscopy (FTIR) analysis showed that the neat starting urones contained some small amounts of isocyanates. Therefore, it was necessary to treat the powders. Small samples (10-12 g) of each urone powder (monuron, fenuron and TDU) were weighed into borosilicate capped vials. The vials were tightly closed and incubated in a thermo-controlled convection oven for desired periods of time and under preset temperatures. Upon incubation, the vials were removed from the oven and immediately cooled to room temperature. Approximately 1.0 mL of acetonitrile (ACN) was added to each vial using a glass syringe. The bottles were then re-capped and gently shaken to dissolve the urones and isocyanates that were present in the neat material. The resultant suspensions were centrifuged at 21,000g, and their clear supernatants were collected. The decomposition of each urone was verified using FTIR spectroscopy by observing the stoichiometric decomposition of the ureas into DMA and nonvolatile aromatic isocyanate (NCO). 4.2.1.2.2 In-Situ Polymerization of Epoxy Shell on Urone Crystal Surface Upon defining the process parameters, it was necessary to determine the feasibility of in-situ polymerization of an epoxy shell on the urone crystal surface. The in-situ polymerization reaction was performed in a 300 mL, temperature-controlled round-bottom reaction flask equipped with stirrer and gas/vacuum inlets and outlets. Urone (15g to 30g) was added to a flask containing 270 g to 285 g of ECH under a nitrogen blanket. The contents were homogenously mixed at room temperature. The reaction was then started by slowly increasing the temperature from room temperature to the targeted reaction temperature. The reaction was exothermic; therefore, an immersion cooler was used to keep the reaction vessel at the desired temperature. Approximately 0.2 g of the reaction mixture was withdrawn from the reaction flask periodically and dispensed into 10 mL glass jars and dried under vacuum in a desiccator. Samples were drawn at three (3) time intervals: MET (as determined above), 1.5 x MET and 2.0 x MET. Dried capsules were quenched by the addition of 0.5 mL of DETA. The average size of individual encapsulated particles and shell thickness was determined using optical microscopy. The urone content in the collected samples was determined using DSC analysis. Once the desired capsule properties were determined, three batches of the encapsulated urone were generated under conditions determined above. More specifically, the reaction was scaled-up to produce 50 g batches of the encapsulated urone. The reaction was started by mixing 450.0 g of ECH with 50.0 g of the urone. The reaction was completed by maintaining the reaction mixture at the desired temperature and time. At the end of the reaction period, ECH was removed from the reaction mixture under vacuum and collected. Dried capsules were quenched by the addition of 100 mL of DETA. The unreacted DETA was collected under vacuum. The urone content in the collected samples was determined using DSC.



4.2.1.2.3 In-Situ Encapsulation of Urones with Adhesive Formulation Next, efforts were focused on determining the feasibility of generating encapsulated urone within the body of an adhesive formulation. As was the case for the in-situ polymerization of the epoxy monomer explained above, the driving force for this reaction was the formation of DMA from the urone particles. The shell formation process was initiated by heating the resin/urone mixture to the optimal release temperature of the DMA as previously determined. The shell formation process was terminated by directly adding the quencher into the mixture. Since the propagating epoxide polymer chain forming on the surface of the urone crystals contained the activated epoxide terminus, the quencher reacted with this epoxide group, while the bulk of the resin remained unreacted and thus available for future curing bonding applications. It was necessary to precisely control the amount of quencher added because it would have reacted with and consumed a large portion of the bulk resin if there was excess. Therefore, the optimal amount of reagents and reaction conditions were investigated. To do this, the in-situ resin polymerization reaction was carried out at room temperature in a temperature controlled Pyrex reaction round-bottom flask equipped with stirrer and gas/vacuum inlets and outlets. Urone (3 g) was added to a flask containing 100 g of the epoxy resin. The contents were homogenously mixed at room temperature. The reaction was then started by slowly increasing the temperature from room temperature to the release temperature of DMA. The reaction was exothermic; therefore, an immersion cooler was used to keep the reaction vessel at the desired temperature. Approximately 30 g of the reaction mixture was withdrawn from the reaction flask periodically and dispensed into glass jars and dried under vacuum in a desiccator. Samples were drawn at three time intervals: MET (as determined above), 1.5 x MET and 2.0 x MET. Dried capsules were quenched by the addition of 20% (molar) excess of DETA. The required amount of DCDA was then added to each of the resin/capsule mixtures (i.e. 5 g of DCDA to 100 g of resin/capsule mixture). These samples were thoroughly mixed manually, degassed and tested for urone loading using DSC analysis.

Complex Coacervation Encapsulation Complex coacervation was conceived in the 1930s by chemists at the National Cash Register Corporation as a means to make microcapsules for carbonless paper. A schematic of a typical complex coacervation process, using gelatin and gum arabic, can be seen in Figure 5. The method used during this project to encapsulate monuron in cross-linked gelatin is similar to one described by Fogle [8]. In this process, monuron is first dispersed into an aqueous solution of gelatin using mechanical agitation. For this emulsification process to be successful, the core material must be immiscible in the aqueous phase. Since monuron is insoluble in water, this approach is appropriate. A coacervating agent, such as sodium metahexaphosphate, is then added to this emulsion. After mixing, dilute acetic acid is added to adjust the pH. Addition of the acetic acid results in the phase separation of the emulsion into two immiscible liquid phases. One phase, the coacervate, has relatively high concentrations of both the accelerant and encapsulant. The second phase, the supernatant, has low concentrations. The compositions of these two phases and the pH at which phase separation occurs are governed by factors such as the ionic strength of the initial solutions, temperature, and the molecular weight of the core and shell materials. The coacervate preferentially adsorbs onto the surface of the dispersed monuron,



forming a coating that fully encapsulates the particles. The mixture is cooled and an agent such as gluteraldehyde is then added to cross-link the gelatin coating. These irregularly shaped coated particles can then be separated from the rest of the mixture. A second cross-linking step can then be performed using tannic acid. This produces a relatively hard, smooth surface to the gelatin coating and prevents agglomeration of the microcapsules.

Figure 5. Schematic of a typical microencapsulation process using the complex coacervation method [9] Complex coacervation is influenced by many highly interrelated factors. For example, the phase separation process affects the composition of the encapsulant, which in turn affects the ability of the encapsulant to wet the core phase, the barrier properties of the encapsulant and the release characteristics of the microcapsule. Due to these multifaceted interactions, it is very difficult to quantify the influence of the process parameters on the coacervation process, despite extensive research. Many existing industrial processes that rely on complex coacervation have been developed based on experience and qualitative observations of the process. Figure 6 illustrates steps involved in microencapsulation via the complex coacervation process used in this project.



Figure 6. Complex coacervation process developed by Thies Technologies for microencapsulation of the curing accelerant in IST’s shelf-stable epoxy resin adhesive

Adhesive Formulation The model epoxy resin formulation is a three-part system that consists of an epoxy resin, a curative and an accelerator. Pastes were formulated according to the recipe in Table 1. Table 1. Baseline epoxy resin system used for viscosity trials.

Adhesive component Mass ratio DER 331 liquid epoxy resin 100 Omnicure DDA5 (DCDA) 5 Accelerant 3 Fumed silica 3

A standard mixing procedure was established to ensure consistent sample production. The standard mixing procedure was developed using raw materials rather than encapsulated material to expedite the process and reduce costly waste. A small-scale (15-25 g) mixing procedure was developed first. This process was used to create paste adhesive samples for DSC analysis and



viscosity analysis. A laboratory-scale (50-100 g) mixing process was also developed. This process was used to create material for film coating.

Small-Scale Mixing Hand mixing was performed on small-scale mixtures. The material from these small batches (15-25 g) was used for DSC analysis, long-term shelf stability testing, and viscosity analysis. These samples were made using the baseline mixing ratio of epoxy (D.E.R. 331): curative (DCDA, DDA5, Omnicure): accelerator (monuron, Sigma Aldrich): fumed silica (Cabot Corporation). The epoxy was measured out into a small glass jar and heated to 104⁰F (40⁰C) to reduce its viscosity so as to more easily mix solid particles. Each powder was added to the epoxy and then mixed via the Painter’s method using a glass stir rod. Small amounts of the mixture were used for DSC analysis, as described in Section 4.4.1. The remainder of the mixture was poured into cylinders for viscosity testing and allowed to de-gas overnight in a convection oven at 104⁰F (40°C). After approximately 10 hours, the samples were removed from the oven and their viscosity was measured, as described in Section 4.4.2, to determine the time to cure of each mixture.

Laboratory-Scale Mixing A laboratory-scale mixing process was devised and demonstrated to yield a homogeneous dispersion of solid particles while minimizing the amount of entrained air in the fully formulated adhesive system. Preliminary mixing trials were performed using a 100:5:3 ratio of epoxy (D.E.R. 331): curative (DCDA, DDA5, Omnicure): accelerator (monuron, Sigma Aldrich). A water bath was used to maintain the samples at 35⁰C during mixing. The efficacy of three types of impeller blades (two blade dispersion impeller, six blade Rushton impeller and three blade left-hand axial impeller) as seen in Figure 7, was investigated. As described in the following subsections, several trials were performed to determine appropriate mixing parameters, such as impeller type, impeller speed and mixing duration.

Figure 7. Blades used for preliminary mixing trials: A) two blade dispersion impeller, B) six blade Rushton impeller, and C) three blade left-hand axial impeller After impeller selection, the next step was to create samples of the fully formulated mixture. Fumed silica was added to the mixture to help to keep the accelerator from falling out of solution. To develop a standardized mixing procedure, samples were produced using a 100:5:3:3 ratio of epoxy (D.E.R. 331 and D.E.R. 661): curative (DCDA, DDA5, Omnicure): accelerator (monuron, Sigma Aldrich): fumed silica (Cabot Corporation). Due to the increased viscosity of



this mixture, it was necessary to work at an elevated temperature (194⁰F /90°C). 120g of D.E.R. 331 and 180 g of D.E.R. 661 were added to a 600 mL beaker, creating a 40:60 mixture of 331:661. The mixture was allowed to heat in a convection oven at 194⁰F (90⁰C) for 2 hours. Meanwhile, the water bath in the mixing apparatus was allowed to reach 194⁰F (90⁰C) and the solid components (DCDA, monuron and fumed silica) were weighed and set aside. The beaker with the epoxy mixture was then removed from the convection oven and suspended in the water bath, allowing the water to rise above the level of the mixture within the beaker, thus ensuring that the mixture is blanketed in heat while mixing. The epoxy resin was mixed at a speed of 250 RPM for 20 minutes. The speed was then increased to 1000 RPM and the sample was allowed to mix for an additional 30 minutes. The speed was then decreased and the fumed silica was added using a plastic funnel. Once the fumed silica was completely incorporated, the speed was increased to 2000 RPM and the sample was allowed to mix for an additional 10 minutes. The speed was once again decreased to 1000 RPM and the DCDA as well as the monuron was added. After they were incorporated, the speed was increased to 1500 RPM and mixed for 5 minutes. Once mixing was complete, the mixture was poured into a Teflon mold and set aside until it was needed for film processing. 4.2.2.2.1 Two Blade Dispersion Impeller The first impeller investigated was a two-blade dispersion impeller (as seen in Figure 7A). This type of impeller is typically used when mixing paint or dispersions. The water bath was filled and allowed to reach 95⁰F (35⁰C). A 600 mL beaker was filled with approximately 500 g of epoxy resin. The beaker was then suspended in the water bath, allowing the water to rise above the level of epoxy in the beaker, thus ensuring that the mixture was blanketed in heat while mixing. The impeller was then lowered into the epoxy such that the head was approximately 1 inch from the bottom of the beaker. The speed of the impeller was gradually increased until a well-developed vortex was observed. This speed was determined to be 2000 RPM. After approximately 30 minutes, the impeller speed was slowed to 1000 RPM and the pre-weighed curative and accelerator agents were slowly added using a plastic funnel to ensure that all of the power would transfer directly into the epoxy resin. Once the curative was added, the speed of the impeller was increased to 2000 RPM and allowed to mix for 30 minutes. After mixing, the impeller was slowly stopped and removed from the beaker. The mixture was analyzed for homogeneity. Upon visual inspection, large particle agglomerates were evident; therefore the selected mixing parameters did not yield a well-blended mixture. To overcome this, a high shear impeller was investigated. 4.2.2.2.2 Six Blade Rushton Impeller Rushton impellers, as seen in Figure 7B, are commonly used for applications that require intense mixing. Observations made during the first mixing trial indicated that an increase in impeller speed from 2000 RPM to 2500 RPM was required to maintain the desired vortex. Otherwise, the mixing process was identical to that described above. Visual inspection of the samples prepared using the Rushton impeller indicated that fewer agglomerates were present, however, the mixing was not as homogenous as desired. Additionally, it was hypothesized that the high shear imparted by the impeller on the sample was causing the capsules to burst during mixing. Therefore, an axial impeller was investigated.



4.2.2.2.3 Three Blade Left-Hand Axial Impeller These impellers, as seen in Figure 7C, are used to impose bulk motion during mixing. It was hypothesized that an axial impeller would yield a homogenous mixture and not rupture any of the capsules. Several samples were prepared as described previously in Section 4.2.2.2. Visual inspection of the samples prepared using the axial impeller showed the best mixing out of the three blades that were examined. 4.3 Film Processing Adhesive formulations prepared as described in previous sections were used to create adhesive films. Films typically have fiberglass scrim with appropriate sizing and are 0.005-0.080” in thickness. The adhesive films must cure according to the prescribed profile to reach full strength. One of the primary reasons to make adhesive films during this effort was to determine if the adhesive strength of the films was degraded in any way due to the inclusion of encapsulated catalyst. Thus it was important to create very consistent films to minimize variability in the strength. Complete scrim wetting and impregnation was imperative. To achieve the adhesive film objectives stated above, IST devised a custom hot-melt film processing setup and method. The following sections describe the setup and method and are followed by a description of established inspection methods.

Lab-Scale Film Line Setup A film casting setup was constructed with the purpose of producing consistent small batches of composite adhesives films. The primary film drawing components and heaters were available as a pre-packaged system from ChemInstruments. The hot melt coater system consisted of a feed spool holder, heated polymer trough, high-tolerance milled steel rollers and a heater/controller unit. As delivered, the system was designed expressly for manual, batch operation without a feed spool for release ply. It was desired to have mechanized film rolling capabilities to improve film consistency. As a result several modifications and additional hardware components were integrated:

• Two tensioned 1-¾” ID feed rolls: necessary to integrate a release ply with the adhesive film for ease of handling

• Variable speed motor and gearbox: provided mechanized consistent rolling at slow speeds

• Conveyer line stand: maintained requisite -10° pitch of film drawn from rollers A schematic diagram of the setup can be seen in Figure 8.



Figure 8. Schematic of the hot melt adhesive processing setup

Method To keep the film products consistent, established processing methods were followed for each run. Run preparation, processing and clean-up methods are listed below. 4.3.1.1.1 Run Preparation The rollers and trough were cleaned using a single wipe of an acetone-soaked cloth to ensure any residual material from previous runs was removed. Once clean, the rollers, trough, and top roller tensioner were inserted. When inserting the top roller tensioner, special attention was paid to ensure they were level with mounting brackets and that standoff screws were in place. In most instances, Teflon flow constriction blocks were required. Next, the rolls of scrim (Type E glass scrim with a weight 4oz/sq. yd. from Fibreglast) and Teflon release ply were mounted. Cutting tape (from Fibreglast) used to make the roll was left in place. The scrim roll was mounted above the release layer. The roll of scrim was about 8 inches wide, two inches less wide than the release film. The 1 inch excess release film on either side of the scrim kept the melter clean and allowed the Teflon blocks to keep the melted resin on the part in process. Figure 9A shows the rollers mounted on the setup. The scrim and release film were pulled past the directional roller and between the two hot melt rollers. Approximately four (4) inches of extra material was allowed to hang out past the rollers.



This material was taped to a wooden dowel for pulling film to the mechanical winder. It was important to have the scrim layer, as opposed to the Teflon, in tension when pulling the film, otherwise wrinkling and bunching may occur. Two (2) metal shims were inserted over the scrim layer and under the top heated roller to space the rollers and specify the desired film thickness. It was important to make sure there are no bunches or folds in the scrim under the shims and to space the shims on the far ends of the scrim cloth. Typical shim thicknesses were 8-20 mils. With the shims still in place, the four roller set screws and two tensioner bar set screws were tightened. The heating elements were inserted into the trough and two rollers to allow the system to preheat. The heaters were set to 195⁰F (91⁰C). The heaters were typically allowed to heat the system for approximately 15 minutes before the addition of the adhesive formulation. The melter and stand were aligned with the roller frame to make sure the film will wind in the center of the mechanized roller at the bottom of the setup. A picture of the aligned system is provided Figure 9B.

Figure 9. A) Hot melt processing set-up with scrim and release film feed rolls, B) Processing set-up with aligned scrim and release film 4.3.1.1.2 Processing The epoxy resin in the trough was brought to the processing temperature (in most cases 195⁰F/91⁰C). Effort was made to start processing runs as soon as the batch formulation was at temperature so as to reduce additional thermal history witnessed by the capsules when heating from ambient to processing temperature. Depending on film thickness, 100-200 g of the adhesive paste was melted per film run. A picture of fully liquefied and heated resin in the melting trough can be seen in Figure 10. Once the resin was ready to be applied, the wooden dowel taped to the leading edge of the scrim was drawn very slowly in such a way to maintain a less than a -10⁰ angle out of the heated rollers. The dowel was brought over the conveyer roller and attached to the motorized roller.

A B



Once attached to the roller, the motor was set to 1-2 RPM. The slow speed was necessary to ensure that the film resin cools by the time it reached the rollers and to facilitate better impregnation of the scrim fiber during coating. To clean the apparatus, parts were wiped down with acetone or soaked overnight if particularly gummed up with resin. Cleaning with acetone immediately after the last run prevented the resin from curing on the hardware.

Figure 10. Hot melt trough with liquefied resin in reservoir (indicated by arrow) during processing 4.3.1.1.3 Inspection Film quality was determined by visual inspection, which targeted the following defects:

• Large scrim weave gaps • Poor fiber wetting indicated by highly visible scrim fiber • Full impregnation of the scrim on both sides • Voids or particulate contamination

Microscopy was used as appropriate to determine the degree of wetting of the scrim fibers. A sample with good impregnation and moderate fiber wetting can be seen in Figure 11.



Figure 11. Micrograph of film prepreg with visible voids, good impregnation and only moderate fiber wetting. Good fiber wetting is exemplified by low-to-no visibility of the scrim fiber.

Development of Single Lap Joint Cure Protocol Initial samples were cured in accordance to manufacturer’s recommendations; however, single-lap-joint test results were not as expected. Therefore, an experimental test matrix was devised to determine the optimal cure conditions for the adhesive films that would ensure that samples made from both the model formulation and the SSA formulation were properly cured prior to testing while not degrading their mechanical performance. Examining uncured or partially cured samples could lead to faulty results and inaccurate conclusions. Mechanical samples of both the baseline and experimental SSA films were prepared in accordance with ASTM D1002 [10]. Samples were fabricated and subsequently heated at 41⁰F/hr (5⁰C/hr) and held at various elevated temperatures (248⁰F (120⁰C), 266⁰F (130⁰C), 275⁰F (135⁰C) and 284⁰F (140⁰C)) for two (2) hours. This range was selected based upon the epoxy resin matrix. The lower limit of the temperature range selected for investigation was based upon the manufacturer’s curing protocol (hold at 248⁰F (120⁰C) for two hours). The upper limit was selected based upon thermogravimetric analysis (TGA) which suggested 284⁰F (140⁰C) was the highest temperature that the parts could be safely cured without danger of thermal decomposition. Upon completion of the cure cycle, the samples were removed from the oven and their shear strength was tested. The results were graphically compared, as seen in Figure 12. A temperature of 284⁰F (140⁰C) was designated as the curing temperature because samples cured at this temperature from both the baseline (neat fenuron) as well as the encapsulated fenuron (CT012612A1) demonstrated the highest shear strength results. The baseline neat fenuron sample appeared to be completely cured at 266⁰F (130⁰C) and maintained mechanical integrity from 130⁰C (266⁰F) to 284⁰F (140⁰C) with no apparent loss in strength. The encapsulated sample did not show appreciable strength until cured at 284⁰F (140⁰C), thus indicated that curing at lower temperatures only allowed for a partial cure. It was hypothesized that the additional thermal energy was required for the DCDA to breach the shell wall of the encapsulated accelerator particles. A cure temperature of 284⁰F (140⁰C) was used as the standard cure temperature for all future sample preparation.



Figure 12. Data used to determine best cure protocol for mechanical samples. Samples that were previously tested for single-lap-joint strength that were constructed using the old cure protocol (cured at 248⁰F (120⁰C)) were remade and cured according to the new cure protocol at 284⁰F (140⁰C). Results from both tests were then compared to one another to determine if a sample was fully cured or if curing at an elevated temperature had resulted in a decrease in mechanical performance. As seen in Figure 13, the ultimate strength of both formulations increased as the cure temperature increased. The increase in strength is much more drastic for the SSA specimens, increasing nearly six (6) fold.



Figure 13. Ultimate strength for specimens cured at 248⁰F (120⁰C) as compared to specimens from the same formulation cured at 284⁰F (140⁰C). 4.4 Adhesive Characterization Accurate and relevant characterization is vital to any materials development effort. Characterization activities focused on the following:

• Assessment of urone content of encapsulated accelerators • Assessment of encapsulation material/process on activity of accelerator in terms of both

shelf life and time to cure • Assessment of impact of encapsulated accelerator on resultant film adhesive properties

Three primary characterization tools have been used to characterize materials:

• Differential scanning calorimetry (Section 2.4.1) • Viscometry (Section 2.4.2) • Mechanical testing (Section 2.4.3)

Differential Scanning Calorimetry (DSC) Analysis



A TA Q200 Differential Scanning Calorimeter (DSC) was utilized to analyze the temperatures and heats required to melt encapsulated urone materials. Each material was scanned in triplicate from 257⁰F (125⁰C) to 482⁰F (250⁰C) at a constant ramp rate of 41⁰F/minute (5°C/minute). An example DSC curve can be found in Figure 14. Once the urone content of the encapsulated materials was calculated, the materials were incorporated into adhesive pastes and analyzed for cure temperature and cure energy. Each adhesive paste was mixed thoroughly and then scanned on the DSC in triplicate from 122⁰F (50⁰C) to 482⁰F (250⁰C) at a constant ramp rate of 41⁰F/minute (5°C/minute).

Figure 14. Sample DSC curve for neat monuron.



Viscosity Analysis Curves for viscosity as a function of temperature (104⁰F (40⁰C), 140⁰F (60⁰C) and 176⁰F (80⁰C)) were generated for baseline paste adhesive formulations using neat monuron. This information was used to determine appropriate test parameters to evaluate the time to initiate cure and to identify benefits imparted by the encapsulated accelerators. Two Brookfield DV-II+ PRO Digital Viscometers, as seen in Figure 15, were used to simultaneously gather data. The models used allow for continuous sensing, temperature measurement and data output to a computer. A spindle speed of 0.3 RPM was selected so minimal mechanical mixing would be imparted on the samples. Measurements were taken at 5 minute intervals.

Figure 15. Viscometer setup used to determine the time to cure of two samples simultaneously

The test was concluded once the measured percent torque on the motor reached 99%. Samples tested at 176⁰F (80°C) reached this value after 4 hours and 25 minutes while samples tested at 140⁰F (60⁰C) reached this value after 38 hours and 30 minutes. The tests that were conducted at 104⁰F (40⁰C) were concluded after 95 hours and 20 minutes, well before this value was reached. The results of a typical test can be seen in Figure 16. Viscosity testing was standardized at 140⁰F (60⁰C) because it is an intermediate temperature that results in curing over days, as opposed to weeks at 104⁰F (40⁰C) (too long for practical down-selection) or hours at 176⁰F (80⁰C) (potentially too short to ensure discernable differences).



Figure 16. Viscosity curves of baseline paste adhesive measured at 104⁰F (40⁰C), 140⁰F (60⁰C) and 176⁰F (80⁰C). Tests were concluded once the percent torque of the motor reached 99%

Storage Analysis The initial project plan specified that viscometry would be the primary tool utilized to analyze shelf-stability; however, during viscosity tests, which were conducted at 140⁰F (60°C), it was noted that the due to the inviscid nature of the epoxy resin system at the conditions, the fumed silica settled at the bottom of samples and may have impacted the curing mechanism. Thus, stability tests via viscosity analysis were only used as a means to screen a large number of samples with relatively low confidence. High confidence results were determined by mechanical testing films stored under controlled conditions for extended periods as described below.

Short-term Storage Stability Analysis Epoxy films were produced and held in an oven for predetermined amounts of time to validate the results obtained from viscosity measurements. The films, which were held at 140⁰F (60°C), were formulated with a solid epoxy component, ensuring that there was no settling of the additives, as seen in Table 2. This experiment was performed with one baseline epoxy film and other SSA films utilizing gelatin encapsulated fenuron. SSA films were made with two different batches of capsules (CT012612A3 and 1-0013-115). Single lap shear film samples (0.5” by 1” film strips) were prepared for each of the two (2) formulations to be removed from the oven every 20 hours for up



to 100 hours. In total, 27 film samples were prepared for each formulation. Upon removal from the oven at defined time intervals, the film samples were laid out on Q Panel aluminum panels for lap shear testing. The samples were cured at 284⁰F (140°C) for two hours and their single lap shear strength was determined using a mechanical tester. The samples were tested in accordance with ASTM D1002 [10] and the load at break was recorded to determine if exposure to elevated temperature lead to any degradation in mechanical strength within the first 100 hours of storage at 140°F (60°C). Table 2. Baseline epoxy resin system used for film production.

Adhesive component Parts per resin DER 331 liquid epoxy resin 60 DER 661 solid epoxy resin 40 Omnicure DDA5 (DCDA) 5 Accelerant 3 Fumed silica 3

Long-term Storage Stability Analysis The long-term stability test was performed both at room temperature and at a minimally elevated temperature (32°C (90°F)). Due to limited supply of material, capsules from batch number CT012612A1 were used in this test. These capsules had similar thermal and mechanical properties as capsules from the CT012612A3 batch used to make the SSA film in the short-term storage stability analysis testing described above. Single lap shear film samples (0.5” by 1” film strips) were prepared for both the baseline formulation and the SSA formulation. These films were removed from the oven at three month intervals up to one year. A final set of film samples was removed from the oven and tested after two years of exposure. 4.5 Performance Testing Mechanical screening tests were performed to help rank the relative strength and performance of each of the candidate capsule batches. Two sets of specimens were fabricated using the baseline adhesive formulation and the most promising experimental formulation was sent to a third-party vendor (Intertek, Pittsfield, MA).

Mechanical Screening Initially, samples were prepared from 0.008” thick prepreg under vacuum, with no compression or immobilization. The specimens produced in this manner had large voids and poor adhesion to the aluminum substrate, as seen in Figure 17. The mechanical data from baseline neat accelerator specimens such as these was typically very scattered and had poor maximum load at break values. A typical baseline load at break average was about 1300 psi using unrefined processing conditions. The optimized baseline processing method yielded much more consistent data with higher yield at break values. A typical baseline load at break average was about 2400 psi using optimized processing conditions.



The optimized method used the following parameters: • Resin solid to liquid ratio (D.E.R. 331 and D.E.R. 661, respectively): 40/60 • Film thickness: 0.016” • Film post processing: additional heat was applied to prepreg increase fiber wetting • Cure atmosphere: cured under ambient pressure • Specimen compression: a 100 g steel slug was placed on each sample • Specimen immobilization: a fixture was devised to keep the specimens in alignment (shown

in Figure 18)

Figure 17. Close up of a lap shear sample after testing. The plate on the left retained nearly all of the adhesive, while the plate on the right had virtually no prepreg material. Also, significant number of voids can be in the remaining adhesive on the left.

Figure 18. Lap shear specimen alignment fixture and compression slugs



Adhesive film samples were tested for shear strength of single-lap-joints in accordance with ASTM D 1002 [10]. Type 2024 T3 aluminum samples were purchased from Q-Lab. Each panel had the dimensions 4.0 ± 0.005 in. x 1 ± 0.005 in x 0.064 ± 0.005 in (101.6 ± 0.25 mm x 25.4 ± 0.25 mm x 1.62 ± 0.125 mm). Before applying the film, the panel was cleaned with acetone. Samples were prepared as illustrated in Figure 19. A 1 in x 0.5 in strip of adhesive film is applied to one end of the panel and a second panel is adhered. Samples were then placed in a programmable oven and cured according to the protocol discussed in Section 2.3.3. Samples were removed from the oven at the end of the cure cycle and then the shear strength of the film is measured using an Instron Testing Machine. The panels were secured into the Instron Testing Machine and pulled at a rate of 0.1 in/min until the adhesive breaks.

Figure 19. Form and dimensions of Shear Strength of single-lap-joint test specimens [10]

Validation Testing Five (5) separate mechanical tests were performed under six (6) post-cure aging conditions, as outlined in Table 3. Nine (9) of each specimen, baseline and SSA, were submitted for each test indicated below (except the climbing drum peel, only three (3) SSA samples were submitted for each set of test conditions). Each test is described in further detail in the following subsections.

Shear Strength of Single-Lap-Joint This test was performed to validate results obtained during screening tests as well as to quantify the shear strength of the SSA in austere conditions. Samples were prepared and tested as described in Section 2.5.1.1. Samples were placed in a programmable oven, cured according to the protocol discussed in Section 2.3.3, and then removed from the oven at the end of the cure cycle. Samples of both the baseline adhesive material and the SSA material were sent to Intertek where they were conditioned as outlined in Table 3 and subsequently tested at ambient temperature, -67⁰F (-55⁰C) and 180⁰F (82.2⁰C). The shear strength of single-lap-joint samples, as measured by Intertek, was compared to those obtained by Infoscitex to confirm that they were comparable prior to performing additional validation tests. This was done to determine reliability in data obtained from Intertek and to help determine consistency in batches of capsules made.



Table 3. Summary of validation mechanical testing and post-curing conditions.

ASTM D1002

ASTM D3528

ASTM D1781

ASTM C393ASTM C297

Post-Cure AgingTest

ConditionsSingle Lap

ShearDouble Lap

ShearClimbing

Drum Peel

3-Point Sandwich

Flex

Flatwise Tensile

Control none ambient x x x x x

Dry Extreme Temperature none -67°F x -- -- -- x

Dry Extreme Temperature none 180°F x -- -- -- x

Long Term Hot/Wet Testing90 days @ 120°F,

50% RH180°F x -- -- -- --

Accelerated Aging90 days @ 120°F,

50% RHambient x -- x -- x

High Humidity Accelerated Aging30 days @ 90°F,

95% RHambient x x x x x

Objective

Conditioning

Strength Properties of Double Lap Shear Joints by Tension Loading Strength properties of double lap shear joint by tension loading were evaluated in accordance with ASTM D 3528 [11]. Type 2024 T3 aluminum samples were purchased from Q-Lab. Each panel had the dimensions 4.25± 0.01 in x 1.0 ± 0.01 in x 0.125 in ± 0.005 in (108 ± 0.25 mm x 25.4 ± 0.25 mm x 3.24 mm ± 0.125 mm). Before applying the film, each panel was cleaned with acetone. Samples were then prepared as illustrated in Figure 20. Two strips of adhesive film measuring 1” x 0.5” were applied to either side of one end of a panel. Two additional panels were then adhered to the first panel. Samples were then placed in a programmable oven and cured according to the protocol discussed in Section 2.3.3. Samples were removed from the oven at the end of the cure cycle. Samples of both the baseline adhesive material as well as the SSA material were sent to Intertek where they were conditioned as outlined in Table 3 and subsequently tested at ambient temperature. The strength of the film by tension loading was then measured using an Instron Testing Machine. The panels were secured into the Instron Testing Machine and pulled at a rate of 0.1 in/min until the adhesive broke.

Figure 20. Form and dimensions of Shear Strength of single-lap-joint test specimens [11]



Climbing Drum Peel for Adhesives Samples were tested for peel resistance of adhesive bonds between an aerospace-grade foam core and metal substrate in accordance with ASTM D 1781 [12]. Type 2024 T3 aluminum samples were purchased from Q-Lab. Each panel had the dimensions 12.0 ± 0.005 in x 3.0 ± 0.005 in x 0.020 ± 0.005 in (304.8 ± 0.25 mm x 76.2 ± 0.25 mm x 0.50 ± 0.125 mm). Before applying the film, each panel was cleaned with acetone. Samples were then prepared as illustrated in Figure 21A. Two strips of adhesive film measuring 12” x 3” were applied to two separate cleaned aluminum substrates. The aluminum/film was then applied to the foam core and the samples were then placed into a specially constructed fixture to ensure proper alignment during curing. Samples were then placed in a programmable oven to be cured according to the protocol discussed in Section 2.3.3 and then removed from the oven at the end of the cure cycle. Cured samples were sent to Intertek for conditioning as outlined in Table 3 above. The peel resistance of the film by tension loading was then measured using an Instron Testing machine at ambient temperature and 180⁰F (82.2⁰C) as seen in Figure 21B. The sandwiches were pulled at a rate of 1.00 ± 0.10 in/min (25.40 ± 2.54 mm/min) until failure was observed.

Figure 21. A) Diagram of laminated test specimen assembly, B) Assembly of peeling apparatus [12]

Core Shear Properties of Sandwich Constructions by Beam Flexure Samples were tested for core shear properties of sandwich construction by being subjected to flexure in such a manner that the applied moments produce curvature of the sandwich facing planes in accordance with ASTM C393 [13]. This test method was used to determine the core shear properties of flat sandwich constructions. Type 2024 T3 aluminum samples were purchased from Q-Lab. Each panel had the dimensions 8.0 ± 0.005 in x 3.0 ± 0.005 in x 0.064 ± 0.005 in (200 ±0.25 mm x 75 ± 0.25 mm x 1.62 ± 0.125 mm). According to ASTM C393, permitted core materials include those with continuous bonding surfaces (such as balsa wood and foams) as well as those with discontinuous bonding surfaces (such as honeycomb). The material that was selected for this evaluation was aerospace-grade closed cell foam. Before applying the film, each panel was cleaned with acetone. Samples were then prepared as illustrated in Figure 22A. Two strips of adhesive film measuring 8” x 3” were applied to two separate cleaned aluminum substrates. The aluminum/film was applied to the foam core and the samples were then placed into a specially constructed fixture to ensure proper alignment during curing. Samples were then placed in a programmable oven to be cured according to the protocol

A B



discussed in Section 2.3.3 and then removed from the oven at the end of the cure cycle. Cured samples were sent to Intertek for conditioning as outlined in Table 3 above. The core shear properties of the sandwich due to beam flexure was measured using an Instron mechanical testing machine at ambient temperature. The sandwiches were then subjected to a bending moment normal to the plane of the sample, as seen in Figure 22B. The only acceptable failure modes, according to ASTM C393, are core shear or core-to-facing bond: failure of the sandwich facing preceding failure of the core or core-to-facing bond is not an acceptable failure mode

Figure 22. A) diagram of construction of samples, B) image of test rig used to test samples.

Flatwise Tensile Strength of Sandwich Constructions Samples were tested for flatwise tensile strength of the core-to-facing bond of the adhesive in accordance with ASTM C 297 [14]. Type 2024 T3 aluminum samples were purchased from Q-Lab. Each panel had the dimensions 1.0 ± 0.005 in x 1.0 ± 0.005 in x 0.020 ± 0.005 in (25.4 ± 0.25 mm x 25.4 ± 0.25 mm x 0.50 ± 0.125 mm). The foam selected was aerospace-grade closed cell foam. Before applying the film, each panel was cleaned with acetone. Samples were then prepared as illustrated in Figure 23A. Two strips of adhesive film measuring 1” x 1” were applied to two separate cleaned aluminum substrates. The aluminum/film was applied to the foam core and the samples were then placed into a specially constructed fixture to ensure proper alignment during curing. Samples were then placed in a programmable oven to be cured according to the protocol discussed in Section 2.3.3 and then removed from the oven at the end of the cure cycle. Cured samples were sent to Intertek for conditioning as outlined in Table 3 above. The peel resistance of the film by tension loading was measured using an Instron mechanical testing machine at ambient temperature, -67⁰F (-55⁰C) and 180⁰F (82.2⁰C). The sandwich construction samples were then subjected to a uniaxial tensile force normal to the plane of the sandwich which was transmitted to the sample through thick loading blocks which are bonded to the sandwich, as seen in Figure 23B. The sandwiches were pulled at a head



displacement rate of 0.020 in/min (0.50 mm/min) until failure is observed. The only acceptable failure modes for flatwise tensile strength, according to ASTM C297, are those which are internal to the sandwich construction: failure of the loading block-to-sandwich bond is not an acceptable failure mode.

Figure 23. A) Maximum permissible dimensions of flatwise tension samples B) Flatwise tension setup [14]

A

B



5. Results and Discussion This effort has served to establish an isolated fenuron accelerator for use in a stable one-part epoxy film. Specifically, results are summarized as follows: • Two (2) methods of encapsulating urone accelerators were investigated, in-situ

polymerization and complex coacervation. Results strongly indicated that complex coacervation yielded encapsulated accelerators with targeted stability and activity.

• Three (3) urone accelerators were investigated: monuron, fenuron and TDU. Ultimately, due to environmental safety concerns, fenuron was selected for incorporation in the final formulation.

• Three types of shell materials were investigated: KC- PDDACL, IC- PDDACL and gelatin. Gelatin was selected due to observed batch-to-batch consistency, ease of scalability, and excellent formulation stability.

• The ability to produce adhesive films featuring encapsulated accelerants was demonstrated. • The initial scale-up of the encapsulation process was demonstrated from 25g batches to 75g

batches. • Shelf stability of the formulation was demonstrated to be greater than one year at 90°F. • Mechanical performance tests have demonstrated that the candidate SSA formulation has

strength similar to or greater than the baseline after aging and hot/wet testing. 5.1 Microencapsulation Results

In-Situ Encapsulation In-Situ Generation of DMA

The production of DMA and isocyanate as a function of temperature, incubation time and urone type was determined using FTIR analysis. Samples were compared to each other using a ratio of the area beneath the absorbance peaks for NCO (2290 to 2230 cm-1) to the area beneath the absorbance peaks for CH bonds (3000 to 2800 cm-1) as described in literature [15]. For monuron samples, there was no change after incubation at 158⁰F (70°C). However, as seen in Figure 24, the monuron samples showed an increase in the NCO content after incubation at 212⁰F (100⁰C) for 30 minutes. These conditions led to the most statistically significant increase in the NCO content. At longer incubation periods and high incubation there was samples exhibited a loss of NCO content. This can be explained by gradual loss of isocyanate due to its further decomposition. The data obtained with fenuron did not show a distinctive pattern within the explored condition ranges, as seen in Figure 25. The samples of TDU demonstrated an increase in the NCO content after incubation at elevated temperatures, however, the statistical significance of the change was less pronounced than for the monuron based samples, as seen in Figure 26. Similar to monuron, there was a loss of NCO content with longer incubation times and higher incubation temperatures. This can be explained by gradual loss of isocyanate due to its further decomposition.



From these experiments, it was determined that it was possible to perform the in-situ encapsulation of monuron (at 212⁰F (100⁰C) for 30 minutes) and TDU (at 158⁰F (70⁰C) to 185⁰F (85⁰C) for 60 minutes). However, the in-situ encapsulation of fenuron could not be performed at temperatures below 221⁰F (105⁰C) and incubation periods under 4 hours.

Figure 24. NCO production in monuron samples

Figure 25. NCO production in fenuron samples



Figure 26. NCO production in samples of TDU

In-situ Polymerization of Epoxy Shell on Urone Crystal Surface The first in-situ polymerization attempt was performed in ECH, as described in Section 2.2.1.2. The reaction was started by rising the temperature to reach the target 212⁰F (100⁰C) (the optimal monuron decomposition temperature). Samples of the reaction mixture were withdrawn from the flask prior to heating and once the mixture reached 104⁰F (40⁰C). It was observed that almost complete dissolution of monuron in the solvent occurred when the temperature of the reaction mixture reached 158⁰F (70⁰C) and heating was discontinued. The reaction mixture was collected and stored in a flask. No analysis of the product was performed because no monuron crystals were present during incubation at elevated temperature. To decrease solubility of monuron in the heated reaction mixture, several different solvents were identified, such as toluene, cyclohexane, and decane [16]. The solubility of monuron at room temperature in each of these solvents is: 0.001155, 0.00005088, and 0.00010076 mole fraction, respectively. Toluene was selected as the first solvent for investigation. The in-situ polymerization reaction in excess toluene was performed as outlined in Section 2.2.1.2. The initial reaction mixture sample was collected. The reaction was started by bringing the temperature to the 212⁰F (100⁰C) (the optimal monuron decomposition temperature). Samples of the reaction mixture were withdrawn from the flask prior to heating and once the mixture reached 104⁰F (40⁰C). It was observed that some dissolution of monuron in the co-solvent occurred when the temperature of the reaction mixture reached 212⁰F (100⁰C). The incubation was continued for 2 hours. Samples of the reaction mixture were collected when the temperature reached 212⁰F (100⁰C) and every 30 minutes after. The reaction samples were dried under vacuum overnight and quenched in 0.5 mL DETA. The quenched samples were kept for potential investigation of the reaction course.



After the 2 hour incubation period, heating was discontinued. It was observed that an abundant amount of newly formed monuron crystals was produced during cooling. The precipitate was collected by vacuum filtration, washed twice with toluene and mixed with DETA to quench the in-situ epoxy and dissolve unreacted monuron. A sample of the end product was further washed once with DETA and twice with toluene, dried and subjected to DSC analysis for monuron content. The DSC analysis, as seen in Figure 27, of the encapsulated material (IST Run-2) when compared with raw monuron showed 110% content of monuron in the final product. It was concluded that possible chemical modification of monuron could have occurred in the toluene-ECH solution. Based on the observed dissolution and re-crystallization of monuron, as well as its potential chemical modification, it was concluded that the in-situ encapsulation reaction should be performed at lower temperatures to maintain monuron non-dissolved and to avoid undesired chemical modification of monuron.

Figure 27. DSC data for IST Run-2, epoxy encapsulated monuron. Average onset of melt temperature = 173.05⁰C, average peak melt temperature = 174.25⁰C, average heat of melting = 159.00 J/g. Active monuron in sample (comparison of heat of melting of IST Run-2 to raw monuron) = 109.68% To further decrease solubility of monuron in the heated reaction mixture, the reaction temperature was decreased to 176⁰F (80⁰C). It was determined that moderate decomposition of dry monuron at 176⁰F (80⁰C) started after approximately 19 hours of incubation. The in-situ



polymerization reaction in excess toluene was performed as outlined in Section 2.2.1.2. A violent reaction occurred and an exotherm was observed when the temperature in the reaction mass reached 167⁰F (75⁰C), thus heating was discontinued. The reaction mass temperature reached 181⁰F (83⁰C) and a color change was observed (bisque color). When the reaction mass cooled to 176⁰F (80⁰C), heating was resumed. Reaction mixture samples were collected when the mixture temperature reached 176⁰F (80⁰C) and after 6, 24, 32 and 39 hours of reaction. These samples were dried, quenched with DETA, and kept for further investigation. After the 39 hour incubation period, the heat was discontinued. Once the reaction mass reached room temperature, the precipitate was collected by vacuum filtration, washed twice with toluene, collected and mixed with DETA to quench the in-situ epoxy polymerization and dissolve unreacted monuron. The end product was further washed once with DETA and twice with toluene, dried and subjected to DSC analysis for the monuron content. A total of 5.00 g of the reaction product was obtained. The DSC analysis, as seen in Figure 28, of the encapsulated material (IST Run-3) when compared with raw monuron showed 98% content of monuron in the final product. Optical microcopy showed a thin encapsulated layer on the surface of the product, as seen in Figure 29.

Figure 28. DSC data for IST Run-3, epoxy encapsulated monuron. Average onset of melt temperature = 173.17⁰C, average peak melt temperature = 174.49⁰C, average heat of melting = 142.10 J/g. Active monuron in sample (comparison of heat of melting of IST Run-3 to raw monuron) = 98.02%



Figure 29. Micrograph of monuron encapsulated via in-situ polymerization

Encapsulation of Urones within the Adhesive Formulation The encapsulation of monuron crystals in an epoxy shell formed by D.E.R. 331 and DETA was attempted. The reaction mixture containing monuron and D.E.R. 331 in toluene was prepared as previously described (Section 2.2.1.2); however, the mixture was not heated. The mixture was stirred to allow D.E.R. 331 adsorption on the surface of monuron crystals for one (1) hour. Then 0.3 g of DETA was added to the mixture. The mixture was then stirred for 72 hours. The sediment was collected by vacuum filtration and washed 3 times with toluene. This resulted in collection of 16.6 g of wet product. The product was dried under vacuum and yielded 12.7 g of product. The DSC analysis, as seen in Figure 30, of the encapsulated material (IST Run-6) when compared with raw monuron showed 80% content of monuron in the final product. Similarly to the encapsulation of monuron using D.E.R. 331, the in-situ polymerization was to be conducted in excess of a solvent incapable of TDU solubilization while maintaining D.E.R. 331 in solution. Information regarding the solubility of TDU in organic solvents was not readily available. A quick visual solubility test was performed using small amounts of candidate solvents, TDU and D.E.R. 331. Mixtures were placed in sealed vials and incubated at room temperature and in a temperature-controlled bath at 70.0⁰C for 60 min. The results of the solubility tests are shown in Table 4.



Figure 30. DSC data for IST Run-6, epoxy encapsulated monuron. Average onset of melt temperature = 173.10⁰C, average peak melt temperature = 174.38⁰C, average heat of melting = 117.27 J/g. Active monuron in sample (comparison of heat of melting of IST Run-6 to raw monuron) = 80.89% As shown in Table 4, almost all of the solvents readily dissolved D.E.R. 331. Some solvents did not dissolve TDU; however, the powder was slightly discolored which was indicative of decomposition. Several solvents (n-decane, n-hexadecane, and xylenes) did not visibly dissolve TDU and did not cause discoloration; however, they completely dissolved D.E.R. 331 at 70 °C. Among those solvents, xylenes had the lowest boiling point. Thus, this solvent was selected for ease of its evaporation during drying of the final reaction product. In-situ encapsulation of TDU was conducted in excess xylenes at 70°C as described in Section 2.2.1.2. Two experiments were performed. The DSC analysis for the first trail, as seen in Figure 31, of the encapsulated material (IST Run-7) when compared with raw monuron showed 129% content of monuron in the final product. The DSC analysis for the first trail, as seen in Figure 32, of the encapsulated material (IST Run-8) when compared with raw monuron showed 97% content of monuron in the final product.



Table 4. Solubility of TDU in various solvents

Solvent Room Temperature 70⁰C Boiling

point (⁰C) TDU D.E.R. 331 TDU D.E.R.

331 1-Methyl-2-pyrrolidone S S S S 202-204 Cyclohexanone NS PS S S 155.6 Ethylacetate NS S S to PS S 77.1 Ethylacetoacetate NS S PS S 180.8 Cyclohexane NS PS PD S 80.7 n-Decane NS NS NS S 174.1 n-Pentadecane NS NS NS PS 268-270 n-Hexadecane NS PS NS S 287 Dichloromethane NS S n/a n/a 39.6 Chloroform S S n/a n/a 62.1 Dimethylsulfoxide S S S S 189 Benzene NS S PD S 80.1 Toluene PS S PD S 110.6 Xylenes NS S NS S 137

*S – soluble, PS – partially soluble, NS – not soluble, PD – partially decomposed. Based upon their favorable thermal properties, capsules from IST Run-3 and IST Run-6 were used to make small paste batches, as described in Section 2.2.2. Samples were allowed to degas overnight and then tested for time to cure at 60⁰C based upon viscosity measurements. Measurements were taken until the viscometer reached 100% of allowable torque. The IST Run-3 sample, which contained encapsulated monuron produced via in-situ polymerization of an epoxy shell on the crystal, cured after 28 hours and 25 minutes. The IST Run-6 sample, which in which the encapsulation of the monuron occurred within D.E.R. 331 cured after 29 hours and 5 minutes. The baseline sample, which contained neat monuron, cured after 40 hours and 5 minutes. These results can be seen in Figure 33.

Due to their poor thermal properties, in comparison with capsules made via the complex coacervation method and inferior stability, this procedure was deemed to be an unattractive method to encapsulate accelerators.









Figure 33. Viscosity measurements for IST Run-3, IST Run-6 and neat monuron baseline mixtures. The time to 100% torque for each sample was: 28 hrs 5 mins (IST Run-3), 29 hrs 5 mins (IST Run-6) and 40 hrs 5 mins (Baseline)

Encapsulation Using the Complex Coacervation Method A total of 42 encapsulated samples were created using the complex coacervation method as described in Section 2.2.1.3. These samples are summarized in Table 5. There were 15 encapsulated monuron samples, of which, seven (7) had a gelatin-based shell, one sample had a gelatin + IC shell, seven (7) samples had a PDDACL + KC shell and one (1) sample had a PDDACL + IC shell. There were 27 encapsulated fenuron samples, of which two (2) had a PDDACL + KC shell and the remaining 25 had a gelatin derived shell. The thermal properties, cure properties, shelf-life and mechanical strength of samples made with these capsules are discussed in the subsequent sections.



Table 5. Summary of capsules made via complex coacervation Accelerant Sample I.D. Shell Material Yield (g)

CT121110E PDDACL + k-carragenan 25.9CT122910A gelatin 25.0CT123010B gelatin 29.4CT123110A gelatin 33.6CT010511A PDDACL + i-carragenan 28.3CT011211D gelatin 25.3CT011411B gelatin 25.4CT011211E repeat 1 PDDACL + k-carragenan 25.0CT011211E repeat 2 PDDACL + k-carragenan 25.0CT011211E repeat 3 - under 63 um PDDACL + k-carragenan 22.0CT011211E repeat 3 - 63-106 um PDDACL + k-carragenan 23.0CT011211E repeat 4 - under 63 um PDDACL + k-carragenan 10.0CT011211E repeat 4 - 63-106 um PDDACL + k-carragenan 32.4CT012612B gelatin 20.0CT012612C gelatin 23.0

CT112211B gelatin 27.8CT121911A k-carragenan 25.0CT121911B k-carragenan 19.0CT123011B gelatin 25.0CT010512A gelatin 10.3CT010512B gelatin 20.5CT012612A1 gelatin 25.0CT012612A2 gelatin 25.4CT012612A3 gelatin 27.0CT060512 - jar 1 gelatin 41.0CT060512 - jar 2 gelatin 34.0CT022612B2 gelatin 26.0JCT071412A gelatin 55.0JCT071412B gelatin 55.0JCT071412C gelatin 20.0CT082612-1 gelatin 43.0CT082612-2 gelatin 45.0CT082612-3 gelatin 50.0CT1-0013-111 gelatin 26.0CT1-0013-112 gelatin 25.0CT1-0013-113 gelatin 24.0CT1-0013-114 gelatin 26.0CT1-0013-115 gelatin 75.0CT1-0013-116 gelatin 75.0CT1-0013-117 gelatin 75.0CT1-0013-118 gelatin 75.0CT1-0013-119 gelatin 75.0

Monuron

Fenuron



5.2 Film Processing Development of a film process and specimen layup procedure was required to effectively evaluate adhesive performance. Lap shear mechanical strength data was used as the primary metric to validate the consistency and reliability of the processing methods. The second phase of testing used optimized preparation methods for consistent specimens and films to compare different film compositions. The results of the process development and composition comparison are described in the following subsections. Several different parameters were varied to determine the optimal film processing and lap shear specimen production process: • Resin solid to liquid ratio (D.E.R. 331 and D.E.R. 661, respectively) • Film thickness • Film post processing • Cure atmosphere • Specimen compression • Specimen immobilization The cure conditions were not varied. Each sample was cured according to the established protocol: from room temperature the temperature was increased at 36⁰F/min (2⁰C/min) to 284⁰F (140⁰C) and held for two hours. A summary of the film samples fabricated to date is given in Table 6. Table 6. Summary of films prepared

Film Designation

Resin ratio (liq/solid) Accelerator Thickness

(inches) Film Product Description

058_102 40/60 Neat Monuron 0.008 Excellent wetting, some bubbles, good tack 058_103 45/55 Neat Monuron 0.008 Excellent wetting, acceptable uniformity, excessive tack 058_103 45/55 Neat Monuron 0.008 Excellent wetting, acceptable uniformity, excessive tack 058_104 50/50 Neat Monuron 0.008 Excellent wetting, acceptable uniformity, excessive tack 058_105 55/45 Neat Monuron 0.008 Excellent wetting, acceptable uniformity, excessive tack 058_106 60/40 Neat Monuron 0.008 Excellent wetting, acceptable uniformity, excessive tack 058_107 40/60 CT122910A 0.008 Excellent wetting, good uniformity, good tack 058_108 50/50 CT122910A 0.008 Excellent wetting, good uniformity, good tack

005_128_1 40/60 Neat Monuron 0.012 Excellent wetting, good uniformity, good tack 005_128_2 40/60 CT011411B 0.012 Excellent wetting, good uniformity, good tack 005_128_3 40/60 Neat Monuron 0.016 Excellent wetting, good uniformity, good tack 005_128_4 40/60 CT011411B 0.016 Excellent wetting, good uniformity, good tack 005_142 40/60 Neat Fenuron 0.016 Acceptable wetting, some bubbles, good tack 005_140 40/60 CT011211E-R1 0.016 Excellent wetting, good uniformity, good tack 058_112 40/60 CT011211D 0.016 Acceptable wetting, good uniformity, good tack

As an example of the film product, film 005_142 is shown in Figure 34. It was determined from the level of tack and the acceptable wetting properties that the 40/60 liquid-solid epoxy blend would be used as the standard formulation. This resin ratio was used in all formulations moving forward.



Figure 34. Photograph of film 005_142 5.3 Adhesive Characterization

DSC Analysis Analysis showed that the accelerant within the capsules behaved similarly to the neat accelerant as evidenced by the sharp endothermic melt peak lying in the graphs seen in Figure 35. The peak melt temperature of the encapsulated materials is slightly lower than that of the neat materials but this difference was deemed to be inconsequential with regards to the cure effectiveness within an epoxy resin. The weight fraction of the microcapsules corresponding to the active accelerant content can be calculated by assuming the enthalpy of melting (ΔH) is proportional to the amount of accelerator. The results of this testing are shown in Table 7. Plots of the DSC results for all batches of monuron and fenuron capsules can be found in Appendix 2A and Appendix 2B, respectively. The peak temperatures did not vary drastically between the neat accelerants and the same encapsulated accelerants. Therefore, it was possible to calculate the amount of active accelerant in each batch of capsules by comparing the enthalpy value for SSA samples to baseline values.



Figure 35. DSC exotherms for A) neat monuron, B) encapsulated monuron, C) neat fenuron and D) encapsulated fenuron



Table 7. Summary of encapsulated materials (complex coacervation method)

Neat Monuron 167.90 175.04 144.97 100.00% 133.75 140.67 351.30CT121110E 165.86 169.61 93.16 64.26% 143.32 154.86 337.53CT122910A 166.86 172.29 98.68 68.07%CT123010B 167.10 169.05 92.58 63.86%CT123110A 167.41 168.94 98.56 67.99%CT010511A 166.25 168.99 90.41 62.36%CT011211D 167.12 169.61 89.37 61.65%CT011411B 165.99 169.09 95.04 65.56%CT011211E repeat 1 165.97 170.24 107.00 73.81% 133.68 142.09 347.90CT011211E repeat 2 165.88 169.16 120.30 82.98% 133.67 141.17 310.77CT011211E repeat 3 - under 63 um 164.86 169.10 94.45 65.15% 135.29 142.57 333.50CT011211E repeat 3 - 63-106 um 164.65 168.86 95.87 66.13% 137.08 143.24 357.53CT011211E repeat 4 - under 63 um 164.76 168.93 97.95 67.57% 137.85 146.07 325.03CT011211E repeat 4 - 63-106 um 164.70 168.93 99.19 68.42% 136.93 144.58 323.00CT012612B 166.16 172.00 91.33 63.00% 157.51 168.78 275.97CT012612C 166.59 172.07 95.33 65.76%

IST Run #2 173.05 174.25 159.00 1.10IST Run #3 173.17 174.49 142.10 0.98IST Run #6 (unwashed) 173.10 174.38 117.27 0.81IST Run #6 (washed) 173.13 174.73 144.40 1.00IST Run #7 167.67 169.97 187.23 1.29IST Run #8 184.85 186.97 107.57 0.74

Neat Fenuron 127.56 129.81 151.17 100.00% 134.69 140.20 359.97CT112211B 126.73 130.86 82.45 54.54% 153.53 157.44 290.73CT120311B 125.42 129.82 75.96 50.25%CT121911A 128.77 131.74 88.76 58.72% 150.36 154.14 346.33CT121911B 128.71 131.52 76.73 50.76% 139.68 145.77 329.87CT010512A 128.67 131.24 57.09 37.77%CT010512B 124.55 129.56 54.55 36.09%CT012612A1 126.36 130.90 93.06 61.56% 155.52 158.88 348.60CT012612A2 126.25 130.76 96.47 63.82% 157.70 160.96 367.03CT012612A3 126.47 130.67 89.07 58.92% 159.73 162.69 337.57CT060512 - jar 1 125.87 130.88 63.61 42.08%CT060512 - jar 2 125.74 130.74 65.97 43.64%CT022612B2 125.15 129.96 78.56 51.97%JCT071412A 126.90 130.43 80.04 52.95%JCT071412B 125.76 130.09 84.21 55.71%JCT071412C 119.20 128.41 61.58 40.74%CT082612-1 127.07 130.90 95.85 63.40%CT082612-2 128.14 131.19 49.17 32.53%CT082612-3 126.89 130.57 92.79 61.38%CT1-0013-111 127.76 130.58 83.69 55.36%CT1-0013-112 127.93 130.42 76.84 50.83%CT1-0013-113 126.43 129.98 81.48 53.90%CT1-0013-114 126.67 130.10 74.82 49.50%CT1-0013-115 126.95 130.82 84.75 56.06%CT1-0013-116 127.16 130.58 83.88 55.49%CT1-0013-117 126.64 130.73 83.25 55.07%CT1-0013-118 126.73 130.89 83.73 55.39%

Raw Material Hand-mixed PasteM

onur

onM

onur

on Not testedNot testedNot testedNot tested

Fenu

ron

Not tested

Not testedNot testedNot testedNot testedNot tested

Not tested

Not testedNot tested

Not Tested

Not Tested

Not TestedNot Tested

Not TestedNot TestedNot Tested

Not TestedNot TestedNot TestedNot TestedNot Tested

Not TestedNot TestedNot TestedNot TestedNot Tested

Not Tested

Onset Temp (⁰C)

% ActiveHeat (⁰C)

Peak Temp (⁰C)

Heat (⁰C)

Peak Temp (⁰C)

Onset Temp (⁰C)

Not Tested

Not Tested



Viscosity Analysis Results Based upon the accelerant content as determined via DSC analysis, small-scale paste adhesive samples of 49 different batches of samples and two baselines were analyzed for the time to initiate cure. Results for these samples can be seen in Table 8. Viscosity curves can be found in Appendix 3A (monuron based samples) and Appendix 3B (fenuron based samples). All samples had to have a time to cure longer than 100 hours to be considered “promising.” Samples in Table 8 marked with an asterisk (*) were deemed to be very stable and stopped before the onset of cure. Table 8. Summary of viscosity results (time to cure at 60°C) of all paste samples prepared with Fenuron accelerant. Samples marked with an (*) were stopped before full cure was attained due to project time constraints.



Short-term Storage Analysis Based upon high active accelerant content, demonstrated long shelf stability as measured by viscosity measurements, and high single-lap-joint shear strength, two batches of capsules (CT012612A3 and CT-0013-115) were down-selected as the best performing SSA candidates and used for storage analysis testing. Film samples of both the baseline and the SSA films were held at 60⁰C for various lengths of time and the residual strength was measured via single lap shear. Results for these tests can be seen in Figure 36. The SSA samples exhibited superior mechanical strength over the baseline sample: the baseline sample lost all mechanical strength within 20 hours of exposure while the SSA samples showed no discernable decline in mechanical strength after 100 hours of exposure.

Figure 36. Residual mechanical strength after short term storage exposure to 60⁰C for baseline and SSA film samples

Long-term Storage Analysis Based upon high active accelerant content, demonstrated long shelf stability as measured by viscosity measurements, and high single-lap-joint shear strength, one batch of capsules (CT012612A3) was down-selected as the best performing SSA candidate. Due to limited quantity of this initial batch, a batch with similar physical characteristics (CT012612A1) was used for this experiment. Film samples of both the baseline and the SSA film (CT012612A1)



were stored at both ambient conditions and 90⁰F (32⁰F) for various lengths of time in controlled environments and the residual mechanical strength (single lap shear) was measured. Results for these tests can be seen in Figure 37. The SSA sample exhibited superior mechanical strength over the baseline sample at the elevated temperature. The baseline sample lost all mechanical strength after only 6 months of exposure while the SSA sample showed a slight decline in mechanical strength after one year of storage at 90⁰F (32⁰C). At ambient conditions, both sets of films appear to have no dramatic loss in single-lap-joint strength over the duration of the long-term storage test.

Figure 37. Residual mechanical strength after long term storage exposure to both ambient conditions and 90⁰F (32⁰C) for baseline and SSA film samples 5.4 Mechanical Testing

Mechanical Screening Batches of capsules that were considered to have desirable shelf-stability as determined via DSC analysis (Section 3.3.1) and viscosity analysis (Section 3.3.2) were made into films for mechanical screening. The shear strength of single-lap-joint of 28 samples was evaluated over the course of the project. These results can be found in Table 9. Overall, the fenuron samples demonstrated higher single-lap-joint strength than the monuron samples. Additionally several



films made from the encapsulated accelerant materials showed comparable strength to those created using neat accelerants. Table 9. Summary of single-lap-joint strength of all films tested.

Average Load at

Break (psi) Std. Dev

Monuron

Neat Monuron 2192.50 ± 388.75 CT121110E 1320.46 ± 100.22 CT011211D 326.14 ± 48.74 CT011411B 1790.76 ± 259.93 CT011211E repeat 1 2151.87 ± 97.64 CT012612B 335.73 ± 61.86

Fenuron

Neat Fenuron 2422.37 ± 351.77 CT112211B 400.97 ± 144.05 CT121911A 1585.84 ± 1139.72 CT121911B 2244.40 ± 270.47 CT012612A1 1225.07 ± 1068.94 CT012612A2 481.88 ± 99.72 CT012612A3 1662.84 ± 614.49 CT060512 - jar 1 2563.41 ± 224.04 CT022612B2 2576.34 ± 242.06 JCT071412A 2831.19 ± 216.06 JCT071412B 2412.18 ± 268.36 JCT071412C 2660.82 ± 354.65 CT082612-2 2447.83 ± 301.41 CT1-0013-111 2518.29 ± 567.94 CT1-0013-112 2653.71 ± 469.14 CT1-0013-113 2420.97 ± 360.09 CT1-0013-114 2917.18 ± 311.29 CT1-0013-115 2483.91 ± 425.02 CT1-0013-116 2572.67 ± 259.71 CT1-0013-117 2665.23 ± 449.73 CT1-0013-118 2497.48 ± 272.77 CT1-0013-119 2659.77 ± 188.00



Mechanical Performance Testing Selection of Shelf-Stable Adhesive Candidate

The single-lap-joint strength and shelf-stability via viscosity of all batches of encapsulated candidates were compared in Figure 38. A target performance zone was defined as any candidate encapsulated formulation that demonstrated both:

1. Minimum lap-joint strength of approximately 1600 psi 2. Minimum shelf-life, as determined via viscosity analysis of 250 hours

As seen on the graph, the batch of capsules that was selected for long-term storage analysis (CT0126122A3) does not fall within the target performance zone; however, at the time of the selection for that particular test, this batch of capsules was the most promising. To improve performance of the samples, capsule fabrication procedures were optimized. The first of these optimized capsule batches, sample CT-0013-111, fell in the target zone. This batch was repeated three times (CT-0013-112, CT-0013-113 and CT-0013-114) to replicate results. When tested, all fell within the target performance zone. As seen in Figure 38 these four batches all demonstrated a smaller range of variance with regards the single-lap-joint strength.

Figure 38. Comparison of performance of batches of capsules with regards to single-lap-joint strength and time to cure, as determined via viscosity analysis. Production of these capsules was scaled-up from a batch size of roughly 25 g to 75 g. These new batches (CT-0013-115, CT-0013-116, CT-0013-117, CT-0013-118 and CT-0013-119) were then



screened for thermal properties via DSC, storage stability via DSC and single-lap-joint strength. All batches examined were within the target performance zone, as seen in Figure 40. Based upon the observed results, CT-0013-117 was selected as the material that would be used for validation testing. This batch of capsules demonstrated thermal and mechanical properties that were closest to the average values for the large batches of capsules. Two (2) manufacturing goals were demonstrated with these batches: first, the ability to scale-up small (25 g) batches to larger (75 g) batches was demonstrated. Secondly, each batch of capsules demonstrated comparable performance to each other with regards to the metrics that were evaluated (thermal analysis, shelf-stability as measured via viscosity analysis and single-lap-joint strength).

Figure 39. Comparison of performance of large batches of capsules with regards to single-lap-joint strength and time to cure, as determined via viscosity analysis.

Shear Strength of Single-Lap-Joint Single-lap-joint samples were tested at several conditions: control, dry extreme temperature (high), dry extreme temperature (low), long term hot/wet testing, accelerated aging and high humidity accelerated aging. Results from Intertek for all samples tested can be found in Appendix 4A. A comparison between the average shear strength at break for both the baseline formulation and the SSA formulation (CT-0013-117) can be found in Figure 40 as well as Table 10. The overwhelming mode of failure for both types of samples under all testing conditions was the adhesion of the film to the metal substrate. Overall, the SSA formulation demonstrated



higher shear strength than the baseline formulation for every testing condition. The mode of failure for all tests performed for both types of films tested was the adhesion to metal, except for the SSA films that were subjected to dry temperature extreme (high) - those samples demonstrated adhesion/cohesive failure mechanisms.

Figure 40. Comparison of the results from the single-lap-joint testing for both the baseline formulation and the SSA formulation (CT-0013-117). Table 10. Shear strength of single-lap-shear results for both the baseline and SSA films.

Strength Properties of Double Lap Shear Joints by Tension Loading Double lap shear samples were tested under two conditions: control and high humidity accelerated aging. Results from Intertek for all samples tested can be found in Appendix 4B. A comparison between the average apparent shear strength at break for both the baseline formulation and the SSA formulation (CT-0013-117) can be found in Figure 41 and Table 11.



As seen for the single-lap-joint samples, the overwhelming mode of failure for both types of samples under all testing conditions was the adhesion of the film to the metal substrate. There was no statistical difference between the baseline and the SSA formulations under control test conditions. The SSA formulation outperformed the baseline formulation under high humidity aging testing conditions, demonstrating a higher retention rate of residual strength after exposure to high temperatures (90⁰F (32⁰C)) and high levels of humidity (95% relative humidity) for 30 days.

Figure 41. Comparison of the results from the double lap shear testing for both the baseline formulation and the SSA formulation (CT-0013-117). Table 11. Strength properties of double lap shear adhesive joints by tension loading.

Climbing Drum Peel for Adhesives Climbing drum peel tests were performed under three conditions: control, accelerated aging and high humidity accelerated aging. Results from Intertek for all samples tested can be found in



Appendix 4C. Due to limitation of SSA film material, only three (3) samples were submitted for each of the climbing drum peel tests, whereas nine (9) samples of the baseline formulation were submitted for each test. A comparison between the average peel torque for both the baseline and the SSA formulation (CT-0013-117) can be found in Figure 42 and Table 12. The failure mode for both the baseline formulation and SSA samples tested under the control conditions was both a cohesive failure within the adhesive as well as a failure within the core material. The mode of failure for the baseline formulations samples under high humidity accelerated aging conditions was only adhesion to the facing whereas for the SSA samples, two failure modes were observed: cohesive failure within the adhesive as well as adhesion to the facing. As seen with the double lap shear results, the baseline formulation performed marginally better than the SSA formulation under control test conditions, however, the SSA formulation outperformed the baseline formulation under high humidity aging testing conditions, demonstrating a higher retention rate of residual strength after exposure to high temperatures (90⁰F (32⁰C)) and high levels of humidity (95% relative humidity) for 30 days.

Figure 42. Comparison of the results from the climbing drum peel testing for both the baseline film and the SSA film (CT-0013-117).



Table 12. Climbing drum peel strength of both the baseline film and the SSA film (CT-0013-117)

Core Shear Properties of Sandwich Constructions Core shear properties of the films were evaluated under three conditions: control, hot/wet and high humidity accelerated aging. Results from Intertek for all samples tested can be found in Appendix 4D. A comparison between the maximum facing stress for both the baseline and the SSA formulation (CT-0013-117) can be found in Figure 43 and Table 13. The failure mode for both the baseline formulation and the SSA films was unknown under control testing conditions. The failure mode for both sets of films under high humidity accelerated aging conditions was due to skin to core delamination on the top facing. Overall, results showed that there was no discernable difference in performance for either film tested.



Figure 43. Comparison of the core shear maximum facing strength for both the baseline film and the SSA film (CT-0013-117). Table 13. Core shear properties of sandwich samples for both the baseline and SSA (CT-0013-117) films.

Flatwise Tensile Strength of Sandwich Constructions Flatwise tensile samples were tested at several conditions: control, dry extreme temperature (high), dry extreme temperature (low), hot/wet testing, accelerated aging and high humidity accelerated aging. Results from Intertek for all samples tested can be found in Appendix 4E. A comparison between the flatwise tensile stress for both the baseline formulation and the SSA formulation (CT-0013-117) can be found in Figure 44 and Table 14. Several modes of failure were noted under each of the tests performed. Both the baseline formulation and the SSA films



failed for several reasons under control testing conditions: cohesive failure, core failure and adhesive failure. The failure modes observed under the extreme temperature (low) test conditions were core/cohesive failure and bond to facing failure for both sets of films. The bond to facing failure is an observed failure of the bonded block to the facing of the sample and does not indicate a failure in the films tested, rather a failure in the strength of the commercially available adhesive that was used to bond test specimens to the block needed to be used in the testing rig. The overwhelming mode of failure for the baseline formulation under extreme temperature (high) testing conditions was bond to facing, while for the SSA film, the failure modes included bond to facing as well as core/cohesive failure. Finally, for the high humidity accelerated aging for both the baseline formulation and the SSA film, the observed mode of failure was an adhesive failure of the core-facing adhesive. According to the ASTM governing this test, all specimens tested are supposed to be tested at a speed that will produce failure in 3 to 6 minutes; however, all of the samples from the high humidity accelerated aging tests failed in less than 3 minutes.

Figure 44. Comparison of the flatwise tensile strength for both the baseline formulation and the SSA formulation (CT-0013-117).



Table 14. Flatwise tensile strength of sandwich constructions of both the baseline and SSA (CT-0013-117) films.



6. Conclusions This program demonstrated the potential of a SSA film system for DoD repair operations. To facilitate rapid insertion into repair operations, IST worked with Henkel to develop the baseline formulation based on its Hysol EA9696 film adhesive. Incorporation of the stabilizing technology into an existing, approved product is anticipated to reduce the time to market. The shelf stability of film adhesives was improved with the SSA system through modification of the accelerator package. This was accomplished through formulation of controlled release encapsulated accelerators into the one-part epoxy resin. The reactivity of the one-part epoxy SSA film is preserved for extended periods of time through the microencapsulation of the curing accelerant. A complex coacervation technique was developed to isolate the accelerant using an exclusive polymeric formulation for the encapsulant material, thus inhibiting the cure process until its intended use. No additional activation steps were required; the accelerant shell ruptures when exposed to the autoclave thermal energy. A baseline was formulated using the primary components of the Hysol EA 9696 resin system matrix and accelerator (fenuron). The experimental SSA material was formulated in a manner identical to the baseline; however, the only differentiating factor was that the fenuron accelerator was encapsulated in a controlled release shell. The SSA has been demonstrated to retain at least 75% of its adhesive strength when stored at 90°F (32⁰C) for a year. As seen in Figure 45, when compared to the baseline formulated with a neat accelerant, the stability of the SSA formulation offers a significant advantage. If stored in a freezer, it is anticipated that the SSA will be stable for well over two years.

Figure 45. Graph of single lap shear tests (ASTM D1002-05) conducted on film samples stored side by side at 90°F for incremented time intervals and cured at 284⁰F.



The mechanical properties of the SSA system were also assessed to verify that the encapsulant material would not adversely affect the adhesive performance during operational use. Tests were performed according to the AMS-A-2546 standard. Under this standard, the model epoxy resin system selected was classified as a Type I adhesive. Accordingly, performance metrics for the SSA film were determined based on Type I requirements. Table 15 shows the test matrix performed on the SSA material relative to the baseline. These tests were conducted at Intertek Plastics Technology Laboratories (Pittsfield, MA). The 90-day environmental conditioning test confirmed that the capsules do not have a deleterious effect on the performance of the adhesive. In every test, the mechanical properties of the conditioned SSA samples were comparable or better than those of the baseline formulation. Table 15. Test matrix for comparitive study between one-part epoxy baseline and SSA formulations. A ‘Pass’ indicates that the SSA formulation had comparable or better mechanical test results as the baseline.

IST recommends two follow-on activities to push the SSA environmental technology towards commercialization. First, the encapsulated accelerator should be formulated and integrated into commercial film adhesive formulations. Mechanical testing of the SSA accelerators in the fully formulated film adhesive is a necessary conformational step before demonstration/validation trials on aircraft. In parallel with this, IST recommends scaling up the complex coacervation production process for the encapsulated accelerator. These validation studies will bring the SSA technology to a technology readiness level appropriate for repair operations testing and demonstration validation flight trials on military aircraft.



7. Literature Cited 1. AMS-A-25463 “Adhesive, Film Form, Metallic Structural Sandwich Construction” 2. MIL-A-25463B, Notice 1 “Adhesive, Film Form, Metallic Structural Sandwich

Construction” 3. Bornhoft, M., Thommes M., Leinebudde P. "Preliminary assessment of carrageenan as

excipient for extrusion/spheronisation." European Journal of Pharmaceuticals and Biopharmaceuticals 59 (2005): 127-131.

4. Hoffman, D.K., D.V. Dellar, M.L. Deviney and H.W. Schlameus. ""Storage Stable Epoxy Resin Adhesives Based on Encapsulated Curatives"." Proceedings of the 28th International SAMPE. Technical Conference. Seattle, WA, 4-7 Nov. 1996. 481-494.

5. Kovar, Robert F., Carolyn Westmark, Marina Temchenko and Thomas Tiano. "Shelf Stable Epoxy Film Adhesive for On-Aircraft Bonded Repair." Society for the Advancement of Material and Process Engineering. Long Beach, CA, 2005.

6. Westmark, C., M. Temchenko, J. Player, T. Tiano and R.F. Kovar. Shelf-Stable, Low Temperature Cure Epoxy Adhesive for On-Aircraft Bonded Repair. Phase I Final Report. Waltham, MA: Foster Miller, Inc., 2003.

7. Son, P. N., C.D. Weber. "Some Aspects of Monuron-Accelerated Dicyandiamide Cure of Epoxy Resins." Journal of Applied Polymer Science 17 (1973): 1305-1313.

8. Fogle, Mark V., Georg Horger. Encapsulation Process by Complex Coacervation Using Polyphosphates and Capsule Product Therefrom. Canada: Patent 882632. 5 October 1971.

9. Gate2Tech. 30 August 2011 <http://www.gate2tech.com/article.php3?id_article=12>. 10. ASTM International, “Standard Test Method for Apparent Shear Strength of Single-Lap-

Joint Adhesively Bonded Metal Specimens by Tension Loading (Metal-to-Metal)”, Standard D 1002-05 (2005).

11. ASTM International, “Standard Test Method for Strength Properties of Double Lap Shear Adhesive Joints by Tension Loading”, Standard D 3528-96 (2008).

12. ASTM International, “Standard Test Method for Climbing Drum Peel for Adhesives”, Standard D 1781-98 (2004).

13. ASTM International, “Standard Test Method for Core ShearProperties of Sandwich Constructions by Beam Flexure”, Standard C393/C393M-06 (2011).

14. ASTM International, “Standard Test Method for Flatwise Tensile Strength of Sandwich Constructions”, Standard C297/C297M – 04 (2010).

15. Cole, K.C., P. Van Gheluwe. "Flexible Polyurethane Foam - FTIR Analysis of Residual Isocyanate." Journal of Applied Polymer Science 34.1 (1987): 395-407.

16. De Fina K.M., Sharp T.L., Chuca I., Spurgin M.A., Acree Jr. W.E., Green C.E., Abraham M.H. "Solubility of the Pesticide Monuron in Organic Nonelectrolyte Solvents. Comparison of Observed Versus Predicted Values Based upon Mobile Order Theory." Physics and Chemistry of Liquids 40.3 (2002): 255-268.



Appendix 1: Requirements Document

Shelf Stable Adhesive Requirements Document

Version: 1.2 Print Date: March 31, 2014 Release State: Revised Draft Approval State: Draft Approved by: M. Cushman Prepared by: J. Belcher Reviewed by: N.A. File Name: WP-1763 Final Report - DRAFT - mc - CF



Document Change Control

Version Date Authors Summary of Changes 1.0 5 June 11 M. Cushman Original Draft 1.1 15 Aug 11 M. Cushman Revised Draft to highlight adhesive type of Hysol EA

9696 1.2 31 Mar 14 J. Belcher 1) Revised Overview to reflect technology updates

2) Added additional reference document 3) Revised non-functional requirements

Document Sign-Off Name (Position) Signature Date



1. Introduction 1.1 Purpose This document details the requirements for materials under consideration for use as film adhesives with improved shelf stability. Such adhesives are intended for use in composite repair. 1.2 Overview Conventional repair operations for composites used in military applications results in the generation of significant amounts of hazardous waste from unused expired film adhesives. Improvement of composite repair technologies is clearly needed to reduce environmental burdens and abatement costs. To address this need, Infoscitex is developing an innovative no-shelf-stable repair adhesive that will reduce the amount of waste generated during composite repair operations. Such an adhesive promises to revolutionize repair processes with respect to waste minimization, cost savings, and protection of the environment. The objective of this three-year program is to develop one-part epoxy film adhesive that is stable at ambient temperatures for over one year. Our approach leverages novel microencapsulant formulations that do not interfere with the epoxy curing process and produce an adhesive that is compatible with existing film formulations and processes. The shelf stable adhesive (SSA) does not require activation or any other major departure from standard processes (TO-1-1-690) and can be rapidly, safely, and reliably used to repair military and commercial composite and metal structures found in aircraft, ships, amphibious and tactical vehicles. 1.3 References Please refer to the following documents for more information about qualification of materials: • AMS-A-25463 (replaces MIL-A-25463B, Notice 1). This document provides guidance on

adhesive films for use in structural construction. • ASTM C 297. Provides guidance on flatwise tensile strength testing. • ASTM C 393. Provides guidance on sandwich flexure testing. • ASTM D 1781. Provides guidance on sandwich peel strength testing. • MIL-A-25463B. For perspective only, and is not to be used as a guiding document. • MIL-A-83377. Provides guidance on structural adhesive bonding for aerospace systems. • MIL-B-22191. Provides guidance on transparent barrier materials. • MIL-C-7438. Provides guidance on aluminum core materials for sandwich construction. • MIL-F-22191. Provides guidance on packaging materials with vapor barrier properties. • MIL-T-5624. Provides guidance on aviation fuel properties, specifically JP-4 and JP-5. • PPP-B-636. Provides guidance on boxes for packaging. • T.O. 1-1-690 General advanced composite repair process manual



2. Requirements Specification 2.1 Chemical and Physical Property Requirements AMS-A-25463 provides all requisite guidance for the chemical and physical performance of film adhesives. The baseline adhesive, Henkel Aerospace Hysol EA 9696 is classified as a Type I adhesive. Accordingly, performance metrics for the film adhesive featuring encapsulated accelerator will be based on Type I requirements. These performance metrics are summarized in Table 1 below.



Table 1. Chemical and physical property requirements for shelf-stable adhesives Property Adhesive

Type* Acceptable Range Test Method‡ Minimum Maximum

Application Temperature (ºF) All 65 85 N/A Cure Time

if at 100ºF or below All N/A 7 days DSC if at 100ºF to 200ºF All N/A 24 hrs DSC if at 200ºF to 300ºF All N/A 2 hrs DSC if at 300ºF or above All N/A 2 hrs DSC

Shelf-Life (months) at 40ºF All 12 N/A DSC at 0ºF All 24 N/A DSC

Sandwich Peel Strength (lb-in./in. width)

70-80ºF I II

III, IV

12.5 10.0 3.5

N/A ASTM D 1781

180±2ºF I, II III, IV

10.0 3.5 N/A ASTM D 1781

-67±2ºF All 10 N/A ASTM D 1781 Flatwise Tensile Strength (psi)

70-80ºF All 750 N/A ASTM C 297 180±2ºF I 400 N/A ASTM C 297 300±5ºF II 350 N/A ASTM C 297 500±5ºF III, IV 220 N/A ASTM C 297 -67±2ºF All 800 N/A ASTM C 297

Flexural Strength (lbs) 70-80ºF All 2100 N/A ASTM C 393 180±2ºF I 1275 N/A ASTM C 393 300±5ºF II 1500 N/A ASTM C 393 500±5ºF III, IV 1200 N/A ASTM C 393 -67±2ºF All 2150 N/A ASTM C 393

Flexural Strength (lbs) after 192 hrs Exposure 180±2ºF I 1500 N/A ASTM C 393 300±5ºF II, III 1200 N/A ASTM C 393 500±5ºF IV 600 N/A ASTM C 393

Fluid Immersion Resistance 30 days ±2 hrs at 70-80ºF fully immersed in JP-4 complying with MIL-T-5624

All 2100 N/A ASTM C 393

High Humidity Resistance 30 days±2 hrs at 120±5ºF and 95-100%RH

All 2100 N/A ASTM C 393 Test at 70-80ºF

Creep Deflection in Flexure after 192 hrs under Load (in.) 100 lb Load, 70-80ºF All N/A 0.025 ASTM C 393 800 lb Load, 180±2ºF I N/A 0.05 ASTM C 393

1000 lb Load, 300±5ºF II, III N/A 0.05 ASTM C 393 500 lb Load, 500±5ºF IV N/A 0.05 ASTM C 393

* Type I: for long-time exposure to -67 to 180ºF; Type II: for long-time exposure to -67 to 300ºF; Type III: for long-time exposure to -67 to 300ºF and short-time exposure to 300 to 500ºF; Type IV: for long-time exposure to -67 to500ºF ‡ All tests shall be performed upon reaching equilibrium as defined on Page 19 in AMS-A-25463



2.2 Non-functional Requirements In addition to the chemical and physical property requirements listed in Section 2.1, the shelf-stable adhesive must meet several non-functional requirements. These include: • Environmental. Must not emit more VOC or HAP than current Hysol EA 9696 product. • Cost. The material must present economic sense when compared to the current state of the

art. This target is not presently defined; however, material selection should be done with cost factored.

• Domestic Source. Supply chain security is of high concern for the US Government. All materials shall be sourced domestically where practical.



3. Dictionary 5.5 Terms and Abbreviations

Term Definition ASTM American Society for Testing and Materials DSC differential scanning calorimetry ⁰F degrees Fahrenheit ⁰C degrees Celsius HAP hazardous air pollutant HRS hours IN inch JP-4 jet propellant 4 JP-5 jet propellant 5 LB pound LBS pounds PSI pounds per square inch SSA Shelf-stable adhesive US United States VOC Volatile organic compound



5.6 Notation/Formula

Notation Definition



Appendix 2A: Viscosity Data for Monuron Based Samples

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0 0

0 0 0 0 0 0 0

\'--r----1--r-+-+----L_

00 0 0 0 0

~ Ill n 0 Ill -< c DJ -DJ

s: 0 ::s £:

"""'' 0 ::s V» DJ 3

"C tD N



c.. s::::

iiJ .... o· :::l -:::l" .... ~

0

...... 0

N 0

OJ 0

~ 0

U1 0

-...J 0

00 0

...... N OJ 0 0 0 0 0

0 0

0 0

0 0 0 0

Viscosity (cP) ~ U1 (J) -...J 00 0 0 0 0 0 0 0

0 0

0 0

0 0

0 0

0 0 0 0 0

~ U'l n 0 U'l ;:::;: < c QJ -QJ

n -t ~ N ~ ~ ~ 0 m

tn QJ

3 "t:l tD ~



-:T .... ~

0

...... 0

N 0

w 0

U1 0

CXl 0

0

...... N w 0 0 0 0 0

0 0

0 0

0 0 0

Viscosity (cP) .J::> U1 (j) 0 0 0 0 0

0 0

0 0

0 0 0

-....J 00 0 0 0 0

0 0

0 0

"' OJ

3 "'C tD N



-:T .... ~

0

...... 0

N 0

w 0

U1 0

CXl 0

...... N 0 0 0 0

0 0

0 0 0

Viscosity (cP) w .J::> U1 (j) -....J 00 0 0 0 0 0 0 0 0

0 0

0 0

0 0

0 0

0 0

0 0 0 0 0 0



a.. c: iil ... o· ::J -:T .... ~

0

U'1

...... 0

...... U'1

N 0

N U'1

w 0

w U'1

0

...... 0 0 0 0

N 0 0 0 0

w 0 0 0 0

"" ~ ----

Viscosity (cP) .J::> 0 0 0 0

U1 0 0 0 0

(j) 0 0 0 0

-....J 0 0 0 0

00 0 0 0 0

~ (I) n 0 (I) -· -< c OJ -OJ



a.. c: iil ... o· ::J -:T .... ~

0

U'1

...... 0

...... U'1

N 0

N U'1

w 0

w U'1

0

...... 0 0 0 0

\

N 0 0 0 0

w 0 0 0 0

~ 1----


U1 0 0 0 0

(j) 0 0 0 0

-....J 0 0 0 0

00 0 0 0 0

~ (I) n 0 (I) -· -< c OJ -OJ

~ OJ 3

"'C I'D N



0.. c D1 ... c;· :::J -:::T .... ~

0

...... 0 0

N 0 0

w 0 0

~ 0 0

U'1 0 0

en 0 0

-...J 0 0

...... N 0 0 0 0 0 0

0 0 0

~ r------

Viscosity (cP) w ~ U'1 en -...J 00 0 0 0 0 0 0

8 0 0 0 8 0 0 0 0 0

0 0 0 0 0 0

~ Ill n 0 Ill ;::;: < c cu ,... cu

n ..... 0 ... 0 U'1 ... ... )>

"" cu 3

"C ~ ...



D. s::: iil -a· ::;, -::r ~ -

0

...... 0

N 0

OJ 0

~ 0

U'1 0

0'\ 0

...... N 0 0 0 0 0 0

0 0 0

\ 1'-----

Viscosity (cP) w ~ U'1 en -...J 00 0 0 0 0 0 0

8 0 0 0 8 0 0 0 0 0

0 0 0 0 0 0

~ Ill n 0 Ill ;:;: < c aJ .. aJ

n ..... 0 ..... 0 U1 ..... ..... l> (,/) aJ

3 "C ~ ,...,



a.. c: iil ... o· ::J -:T .... ~

0

Ul

I-" 0

I-" Ul

N 0

N Ul

w 0

w Ul

Ul 0

0

I-" N w 0 0 0 0 0

0 0

0 0

0 0 0

Viscosity (cP) .J::> U1 (j) -....J 00 0 0 0 0 0 0 0

0 0

0 0

0 0

0 0

0 0 0 0 0

~ (I) n 0 (I) -· -< c OJ -OJ

n -4 0 ~ 0 U1 ~ ~ )>

~ OJ 3

"'C I'D w



a.. c: iil ... o· ::J -:T .... ~

0

...... 0

N 0

w 0

+:-0

U1 0

C)) 0

-....J 0

00 0

1.0 0

0

,

...... 0 0 0 0

N 0 0 0 0

"' "----... ---

w 0 0 0 0


U1 0 0 0 0

(j) 0 0 0 0

-....J 0 0 0 0

00 0 0 0 0

:5 VI n 0 VI -< c OJ -OJ



0

...... 0

N 0

w 0

D. ~ s::: 0 iil r+ a· ::;, -:::r v; V1

- 0

m 0

00 0

0

Viscosity (cP) ...... N w ~ U'1 en -....J 0 0 0 0 0 0 0 0 0 8 0 0 0 8 0 0 0 0 0 0 0 0 0 0 0 0

\1'-----~-T--+--+--~

00 0 0 0 0

~ (I)

n 0 (I) ... < c cu ... cu



c.. c: iii ~. 0 :I -:r .., Ill -

0

..., 0 0

N 0 0

w 0 0

~ 0 0

U"1 0 0

CJ)

0 0

..., N w 0 0 0

0 8 0

0 0 0

8 0

Viscosity (cP) ~ U"1 CJ) -...J 00 0 0 0 0 0 0 0 0

8 0

0 0 0

0 0 0

0 0 0

~ II' n 0 II' ;:+ < 0 QJ .... QJ

n ..... 0 .. .. ~ .. .. CD

"' QJ

3 "'C tD ..



Q. c iil ,.. a· ::J -:r .., Ill -

0

...... 0

N 0

N 01

w 0

w U'1

01 0

0

...... 0

8 0

~

N 0 8 0

Viscosity (cP) w ~ 0 0 8 8 0 0

1'-----~

U'1 0 0 0 0

en 0 0 0 0

-...J 0

8 0

00 0

8 0

< iii' n 0

"' ;::;; < c cu "" cu

V') cu 3 'C ~ N



c.. c iil ... o· :::1 -::r .... ., -

0

U'1 0

...... 0 0

...... V1 0

N 0 0

N V1 0

w 0 0

w <.n 0

-1=:> 0 0

~ U'1 0

V1 0 0

0

~

...... 0

8 0

N 0 8 0

\ ~ ----

w 0

8 0

Viscosity (cP) ~ 0 8 0

U'1 0 0 0 0

en 0 0 0 0

-....J 0

8 0

00 0

8 0

~ VI n 0 VI ;:::;: < c cu ,... cu



c. s:::: iil r+ c;· ::J -::r .... Ill -

0

U1

....... 0

....... U1

N 0

N U'1

w 0

w U1

0

I

r

t ~

~

~

....... 0

8 0

t~

_jj ,_

N 0 8 0

w 0

8 0

~ 1'---.._____

Viscos ity (cP) ~ 0 8 0

U1 0 0 0 0

en 0 0 0 0

-...J 0

8 0

00 0

8 0

~ Ill n 0 Ill r+ < 0 Ql r+ Ql



Q. s::: iil -

0

...... 0

...... V1

a· N ::::J 0 -:::r iit -

N (11

w 0

w V1

0

Viscosity (cP) ...... N w ~ U'1 en -...J 0 0 0 0 0 0 0 0 0 8 0 0 0 8 0 0 0 0 0 0 0 0 0 0 0 0

~~---..____1--t--t-----+---L-

00 0 0 0 0

~ VI n 0 VI ;:::;: < c t:U .... t:U



Q. s::: iil -

0

...... 0

...... U"1

a· N ::;, 0 -::r ~

N (11

w 0

w U"1

0

Viscosity (cP) ...... N w ~ U'1 en -...J 0 0 0 0 0 0 0 0 0 8 0 0 0 8 0 0 0 0 0 0 0 0 0 0 0 0

~~------lt------1---+-_j__

00 0 0 0 0

~ VI n 0 VI ;:::;: < c t:U .... t:U

n d .... .... N .... .... m I

~ N

V) t:U 3

"C Cl)

N



Q. r::: ii'l ... a· ::I -:r iii -

0

U1

...... 0

...... U1

N 0

N U1

w 0

w U1

0

I

j

r

...... 0 0 0 0

N 0 0 0 0

w 0 0 0 0

\ "---1-----

Viscosity (cP) ,J:. 0

8 0

U1 0

8 0

en 0

8 0

-...J 0 0 0 0

00 0 0 0 0

< VI n 0 VI ;::;: < c CIJ -CIJ



Q. r::: ii1 r+ a· ::I -::r iri -

0

U1

...... 0

...... U1

N 0

N U1

w 0

w U1

0

I

...... 0 0 0 0

N 0 0 0 0

~ "---. r--

w 0 0 0 0

Viscosity (cP) ,J:. 0

8 0

U1 0

8 0

en 0

8 0

-...J 0 0 0 0

00 0 0 0 0


n d ..N ..m

I

:::0 w I

(/) CIJ

3 "'C -n:> N

Info

scite

x C

orpo

ratio

n Sh

elf S

tabl

e Ep

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ive

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93

F

INA

L R

EPO

RT

80000

70000

60000

50000 ~ u -> ·~ 40000 0 u Ill

> 30000

20000

10000

0

0 5

Viscosity Data - CT011211E-R4- Sample 1

I

I _/

10 15 20 25 30 35 40 45

duration (hrs}



Q. t:: iil r+ c;· ::I -::r ... In -

0

...... 0

N 0

w 0

+:> 0

U1 0

en 0

-...J 0

0

...... 0 0 0 0

\

N 0 0 0 0

w 0 0 0 0

Viscosity (cP) +:> 0

8 0

"---r------

U1 0

8 0

en 0 0 0 0

-...J 0 0 0 0

00 0 0 0 0


V') CIJ

3 "C -t1)

N



Q. c iii ~ s· ::I -:r .... ~

0

lJ1 0

...... 0 0

...... lJ1 0

N 0 0

N t.n 0

...... N w 0 0 0 0 0 0 0 0 0

0 0 0 0

I

Viscosity (cP) -"" lJ1 0) -...J 00 0 0 0 0 0 0 0

0 0 8 0

0 0 0

0 0 0 0 0

< iii' n 0 Ul ;:t.' < c Q,J ... Q,J

q 0 I-& N ~ I-& N O:J

en cu 3

"'C tD I-&



Q. s::: iil -

0

t-> 0

a· ~-" :::::1 <J1 -::r v: -

N 0

N 1.11

w 0

0

rJ

t-> 0

8 0

N 0

8 0

Viscosity (cP) w 0

8 0

~ 0 8 0

~ ~ ----

1.11 0

8 0

CJ)

0

8 0

-....1 0

8 0

~ 11'1 n 0 11'1 ;::;: < c cu .... cu

::0 c:: :::J w



Q. c iiJ ...

0

U'1

..... 0

a· ..... ::::1 lJ1

::::1" ... II) -

N 0

N lJ1

w 0

0

1-.

-

lJ1 0

8

\

..... 0

8 0

..... lJ1

8 0

Vis<:osity (cP) N 0

8 0

N lJ1 0 0 0

' r----

w 0 0 0 0

w lJ1 0 0 0

~ 0

8 0

~ U"1

8 0



Appendix 2B: Viscosity Data for Fenuron Based Samples

c. c: iii ,... a· ::J -:r .., Ill -

0

..... 0

..... U1

N 0

N U'1

w 0

w U'1

0

..... 0

8 0

~

N 0

8 0

w 0

8 0

I'-----~

Viscosity (cP) ~ 0

8 0

U'1 0 0 0 0

en 0

8 0

-....J 0

8 0

-

00 0

8 0

< II' n 0 II' ;:::; < c QJ ,.. QJ



Q. s::: iil -a· ::::J -:::r iil -

0

...... 0

~ U"1

N 0

N V1

w 0

w U"1

0

...... 0

8 0

N 0 8 0

w 0

8 0


1'--------

U'1 0 0 0 0

en 0 0 0 0

-....J 0

8 0

00 0

8 0

< II\ n 0 II\ ;:::;: < c QJ ... QJ

"TT t'D :::J c::: .., 0 :::J V) QJ

3 "'C t'D N



Q. s::: iil -a· ::::J -:::r iil -

0

...... 0

~ U"1

N 0

N V1

w 0

w U"1

0

...... 0

8 0

N 0 8 0

w 0

8 0


1'--------

V1 0 0 0 0

en 0 0 0 0

-....J 0

8 0

00 0

8 0

~ V) n 0 V)

;::;: < 0 1:1.1 .... 1:1.1



c.. r:: D1 ... o· ::::s -::r ... ~

0

N 0

~ 0

0'\ 0

00 0

...... 0 0

...... N 0

...... N w 0 0 0 0 0 8 0 0

0 0 0 0

Viscosity (cP) ~ U'1 0'\ -...J 00 0 0 0 0 0 0 0 0 8 0 0 0 0 0 0 0 0 0 0

< "" n 0 ~. r+ < c cu r+ cu

n ~ ... ... N N ... ... c:J

V) cu 3 '0 n> ...



c.. r:: Dl ... a· ::::J -::r .., ~

0

N 0

~ 0

0'\ 0

00 0

._. 0 0

._. N 0

._. N w 0 0 0 0 0 0 0 0 0

0 0 0 0

Viscosity (cP) ~ U'1 0'\ -...J 00 0 0 0 0 0 0 0 0 8 0 0 0 0 0 0 0 0 0 0

< "" n 0 ~. r+ < c ~ r+ ~

n ~ ... ... N N ... ... c:J

(,/) ~

3 '0 tO N



0.. c D1 ... c;· :::J -:::T .... "' -

0

U'1 0

...... 0 0

...... U'1 0

N 0 0

N V1 0

w 0 0

w V1 0

...... N w 0 0 0 0 0 8 0 0

0 0 0 0

1

Viscosity (cP) ~ U'1 en -...J 00 0 0 0 0 0 0 0 0 8 0 0 0 0 0 0 0 0 0 0

~ Ill n 0 Ill ;::;: < c cu rot> cu

n -1 ..-N ..-U) ..-..->

"" cu 3

"C ~ ..-



0

U'1 0

..... 0 0

..... c.. U'1 c 0

D1 ... c;· :::J -:::J' .... ~ N

0 0

N V1 0

w 0 0

w V1 0

0

;

r (

•

'

..... 0

8 0

N 0 8 0


U'1 0 0 0 0

0'\ 0 0 0 0

-...J 0

8 0

00 0

8 0

~ VI n 0 VI ;::;: < c cu rot> cu



D. c iil ,..

0

...... 0

N 0

o· w ::J 0 -::r ii1 -

U'1 0

en 0

0

...... 0

8 0

~

N 0 8 0


1'--------

U'1 0 0 0 0

en 0 0 0 0

-...J 0

8 0

00 0

8 0

s V\ n 0 ~. r+ < c G) r+ G)



c. c iil ... Ci' :::1 -::r .... ., -

0

.... 0 0

N 0 0

OJ 0 0

~ 0 0

V1 0 0

0'\ 0 0

0

Viscosity (cP) ...... N w .f::> 1.11 0'\ 0 0 0 0 0 0 0 0 0 8 0 0 0 0 0 0 0 0 0 0 0 0 0

T

< V\ n 0 V\ -· r+ < c ~ r+ ~

n ..... ... N w 0 .... .... "' V) ~

3 "C t» ....

~~----1--t---+--L_

Info

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7 F

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80000

70000

60000

50000 ~ u -> .~ 40000 1/1 0 u 1/1

> 30000

20000

10000

0

0 5 10

Viscosity Data - CT010512A- Sample 1

15 20 25

duration (hrs}

30 35

I

j I

/ 40 45 50



Q. s::: iil r+ a· ::I -:::r ~ -

0

U1

...... 0

...... U1

N 0

N U'1

...... 0

0

0 0 0

Viscosity (cP) N w ~ U'1 en -...J 00 0 0 0 0 0 0 0 0 8 0 0 0 8 0 0 0 0 0 0 0 0 0 0 0 0 0

~ "' n 0

"' ;::;: < c ll) ... ll)

n ~ 0 ~ N 0'\ ~ N )> ~

V) ll)

3 "C ro N

......___~----t--+--t-~k



0.. r:: iiJ ... o· :::J -::r ... ~

0

U'1 0

._. 0 0

._. U'1 0

N 0 0

N U'1 0

._. N w 0 0 0 0 0 0 0 0 0

0 0 0 0

Viscosity (cP) ~ U'1 0'\ -...J 00 0 0 0 0 0 0 0 0 8 0 0 0 0 0 0 0 0 0 0

s Ill n 0 Ill

~ < c Q) ... Q)

n ~ 0 ._. N en ._. N )> N

V) Q)

3 "C ro ._.



c. c iiJ ... 0 ::J -:r ... ~

0

N 0

+:> 0

0'\ 0

00 0

._. 0 0

._. N 0

._. 00 0

._. N w 0 0 0 0 0 0 0 0 0

0 0 0 0

Viscosity (cP) ~ U'1 0'\ -.J co 0 0 0 0 0 0 0 0 8 0 0 0 0 0 0 0 0 0 0

~ In n 0 In

~ < c Q) ~ Q)

n ~ 0 ..... N en ..... N )> w V) Q)

3 "C tD .....



D. s:::: iil r+ a· ::;, -::r .... Ill -

0

U1

~ 0

~ U1

N 0

N U1

w 0

w U1

0

~ 0

8 0

\

N 0 8 0

w 0

8 0

Viscos ity (cP) ~ 0 8 0

~ ..____ 1--.

U1 0 0 0 0

en 0 0 0 0

-....J 0

8 0

00 0

8 0

I -n -1 0 ...... ~ ,c::. ~ N ):>



Q. s:::: iil r+ a· ::;, -:::r iii -

0

U1

...... 0

....... U1

N 0

N (11

w 0

w U1

0

...... 0

8 0

N 0 8 0

w 0

8 0


~ .____ -

U'1 0 0 0 0

en 0 0 0 0

-....J 0

8 0

00 0

8 0



Q. c iil ... Ci' :::1 -::::r .... Ill -

0

(1'1

0

...... 0 0

...... U1 0

N 0 0

N (1'1

0

w 0 0

w (1'1

0

~ 0 0

(1'1

0 0

0

...... N w 0 0 0 0 0 8 0 0 0 0 0

' Viscos ity (cP)

~ U'1 en -....J 00 0 0 0 0 0 0 0 0 8 0 0 0 0 0 0 0 0 0 0

< II' n 0 II' ... < 0 CIJ ... CIJ

n ~ ...

I

0 0 ... w

I ... ... ...



Q. c iil ... Ci' :::1 -::::r .... "' -

0

(1'1

0

...... 0 0

...... V1 0

N 0 0

N (1'1

0

w 0 0

w (1'1

0

~ 0 0

(1'1

0 0

...... N 0 0 0 0 0 0

0 0 0

-....

~

Viscos ity (cP) w ~ U'1 en 0 0 0 0

8 0 0 0 0 0 0

0 0 0 0

-....J 00 0 0

8 0 0

0 0

< VI n 0 VI ... < c CJ ... CJ

n ~ ...

I

0 0 ... w

I ... ... N



0

...... 0 0

N 0 0

w c.. 0 c 0

D1 ... c;· :::J -;r .... ~ ~

0 0

U1 0 0

en 0 0

-....J 0 0

0

...... 0

8 0

" ~

J

•

t \

t

N 0 8 0

w 0

8 0


U1 0 0 0 0

en 0 0 0 0

-....J 0

8 0

00 0

8 0

< VI n 0 VI ..... < c CJ ..... CJ

n ~ ...

I

0 0 ... w

I ... ... V1

Info

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App

endi

x 3A

: DSC

Dat

a fo

r M

onur

on B

ased

Sam

ples

Neat Monuron

-.gJ ~ -~ 0 u: -ro OJ I

-2-

-4-

-6-

I ........

... . ~· ·----..·---·----·- ·--·--. 173. 76"C . ....._ . ........_

1 1391.Ug ·-......, .,

174.1s·c \

151.0J/g '

. 173.94"C 152.6J/g

175.14"C

11s.oa•c

174.91·c 20101021.()04 20101021 .005 20101021 .006

~~~-r~-.~--~.-.-~~-.-.-,~r-r-.-~~-r-.~~--~--~~~~

120 140 160 180 200 220 240 260

Exo Up Temperature (0 C)



CT121110E Graph

Heat FloW (Wig)

~ 3

"& ~ OJ g; c

ii -• 9

..... 8



CT122910A Graph

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CT123010B Graph

~

Ol

~ ~

~ .Q LL.

iii Q)

I

I~======~~------------------------~ 0.5-.--

0.0

-0.5

-1.0

-1 .5

nues CT123010B- 3 Thees CT123010B- 2 Thies CT123010B- 1

-2.0 +-~~---,.~~~-,--~~---,.~~~.--~~---,.~~~.--~~---r~~~.--~~--l 80 100 120 140 160 180 200 220 240 260

Temperature (·c)

Info

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CT123110A Graph o.51 I

167.38'C 167.36"C

0.0 107.0J/g . 100.6J/g

-0.5

~

"' 3 ~

~ -1 .0 .Q u.. iii Q)

I

-1 .5

169.08'C

168.93'C -2.0

168.82'C

20110209.003 20110209.()04 20110209.005

-2.5 +-~~ .......... ~~~--r~~~.--~~---.~~~-.-~~~.--~~---.---.-~~-.-~~-.--;

120 140 160 180 200 220 240 260 280 300

Temperall.lre ("C)



CT010511A Graph

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CT011211D Graph I~~~~~----------------------~ 0.5-r--

0.0

c; -0.5

~ ~

~ LJ...

iti Q) I -1.0

-1 .5

"""=\

CT011211D_Sample 1 CT0112110_Sample 2 CT0112110_Sample 3

~

-2.0 +-~-~~---.-~~~~.-~-~~-----~~~--.--~-~~---.-~~~---l 120 140 160 180 200 220 240

Temperature (°C)

Info

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orpo

ratio

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CT011411B Graph

~

~ ~ ~

:;: !2 LL.

iii Q)

I

I L======~~--------------------------~ 0.5-.--

0.0

-0.5

-1.0

-1 .5

Thies CT011411B Thtes CT01 1411B- : Thies CT01 1411B=1

-2.0 +-~~.---,,--.~~--,-~~~.-~~.---,,--.~~--,-~~~.-~~~.--.~~--.~~.,.....-j

120 140 160 180 200 220 240 260 280 300

Temperature (·c)

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CT011211E Repeat 1 Graph 0.0 ~==================~---------------------------------------.

-0.5

-.Q>

~ ~ -1.0-

u::: ...... co Q)

I

-1 .5

~

r: ====:j (

Sampte3 Sample 2 Sample 'I

-2 .0+-----.----.-----.-----.----.-----.-----.----.-----.----.-----.---~ 140 150 160

Exo Up

170

Temperature (0 C)

180 190 200 Universal V4.5A TA

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CT011211E Repeat 2 Graph 0.0 ...!;:::==========::::::!

-0.5

-.g> ~ -~ -1.0 u: -(I) Q)

I.

-1.5

Sample 4 Sample 3 Sample 2 Sample 1

-2.0+--------.-------.-------.--------.-------.-------.--------.------~ 150

ExoUp

160 170

Temperature (0 C)

180 190

Universal V4.5A TA 11

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CT011211E Repeat 3 under 63 Graph

~

~ ~ ~

0.5-F===========~------------------,

0.0

CT011211E.R3.underb3.S01 CT011211 E.R4.unde!1;3.S01 CT011211 E.R3.under63.SO CT011211E.R3.under63.SO

~ .Q -0.5 u.. iii Q)

I

-1 .0

-1 .5~~~~~~ 1~ v 140 160 180 200

Temperature (·c)

220 240 260

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CT011211E Repeat 3 63-106 um Graph

~

~ ~ ~

~ u.. iii Q)

I

o.5..:======== === :_--------------------,

0.0

-0.5

-1.0

-1 .5

011211Erepeat3 63-106 S01 CT011211E repea1 3_63-11l6.SO CT011211E repeat 3_63-106.50

-2.0 +-~~-.----,~~~~.-~~-.----,~~~~.-~-.--.----,~~~~-,-~-.--.--l 120 140 160 180 200

Temperature (·c)

220 240 260

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CT011211E Repeat 4 under 63 Graph

~

!!! ;: ~

~ .Q LL

iii Q)

I

0.5.!;===========~------------------,

0.0

-0.5

-1.0

-1 .5

CT011211E.RA undetb3.SO CT011211 E.R4.unde<b3.SO

-2.0 -1-~~~--"T~~~~.-~~~--"T-~~~.-~~~--"T-~...--.---.-~~~--t 120 140 160 180 200

Temperature (°C)

220 240 260

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CT011211E Repeat 4 63-106 um Graph

~

,!2' 3: -~

.Q ~

iii Q)

I

0.5 -F======= === ::::!_- -------- ------------,

0.0

-0.5

-1 .0

-1.5

CT0112t 1E.R4.63-106.SO CTO t 1211E.R4.63- 106.SO

-2.0 -1-~~~--,,...-~~~--,-~-,...-~.-~~~-.-~~~-..~-~~--.-~~--,r-; 120 140 160 180 200

Temperature (°C) 220 240 260

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CT012612B Graph

-C)

~ ~ .Q u. co Q)

I

~~ ======~~----------------------~ 0.0

-02

-0.4

-0.6

~.J \ I I Sample 3 Sample 2 Sample 1

-1.0

-12

-1 .4 +-----~----~------~-----r----~------~----~----~------~----~ 1~ 160 170 180 190 200

ElloUp Temperature rc) UniVersal V4.SA TA II

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CT012612C Graph 0.0 ~--------------------------------------------------------------~

-0.5

-C»

~ ~ -1.0 0 u: i J:

-1 .5

Sample3 Sample 2 Sample 1

-2.0 +---------r--------.----------r--------.---------,----------.---------,---------; 150

ExoUp

160 170

Temperature (0 C)

180 190 Universal V4.5A TA II

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IST Run #2 Graph 2~==========~----------------------------~--------~

0

Oi -2

~ ~

.Q LL -m I -4

-6

t72.8t~c t73.71•c 172.64°C 142. 1J/g 155.4J/g 179.5J/g

t74.ts•c

174.1o·c

174.so·c

20110128.001 20 110128.002 20110131 .001

-8 +-~--~~~--~~--~~~--~~--~~~--~~--~~~--~~~~~-4

120 140 160

Exo Up

180

Temperature rq 200 220 240

Universal V4.5A TA In

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IST Run #3 Graph 2 I I

0

Oi -2

~ ~ 0

u:::

m ~ -4

-6

-8 120

ExoUp

\.

140

17326"C J40.2J/g

I

160

173.13"C 173_11•c 144.0J/g 142.1J/g

\ r•

174_44•c

174.50"C

174.52"C

180

Temperature (•C)

20110202.002 20110202.003 201 10202.004

-

200 220 240

Umversal V4.5A TA h



IST Run #6 (washed) Graph

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IST Run #7 Graph

~

Ol

~ 3 .Q I.J..

iii Cl)

I

I I 2

0

) --2

-4 I -

-6 120

{\..__

140

Exo Up

167.66'C 200.3Jig

160

167.65oc 167.71'C 220.3Jig 141.1Jig ., ({ '

)

168.71"C

17UJ4'C

170.17"C

180

Temperature ("C)

2011 0303.()(}3 20110303.004 20110303.005

200 220 240 Universal V4.5A TA tr



IST Run #8 Graph

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App

endi

x 3B

: DSC

Dat

a fo

r Fe

nuro

n Ba

sed

Sam

ples

Neat Fenuron I I

0

......... -1 .!21 ~ -~

-2 j \ I Sample 6 u..

..... Sample 5 co Sample4 Q) I Sample3

Sample 2 Sample 1

-3

4+-------~------~------~------~------~~------~------~----~ 110 120

Exo,up

130

Temperature (°C)

140 150 Universal V4.5A TA

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CT112211B Graph

~

Ol

~ ~

~ .Q u.. iii Q)

I

o.o-)::.1 ====-~---------------,

-0.5

-1.0

-1 .5 CT1122118.capsules.S011 CT112211B.capsules.SO~ CT1122118.capsules.SOc

-2.0 +~~~.--.~~--.~~~.-~~~.--.~~--.~~~.-~~~,--..--.~--.~~.........-~

80 100 120 140 160 180 200 220 240 260

Temperature c·c)

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CT121911A Graph 0.5!;::::1 ===::::!....! _ _ _____ ______ ---,

0.0

Ol -0.5

~ ~

~ .Q LL.

iii Q) I -1.0

-1.5

1 I I I

CT121911A 501 CT121911A- S02 CT121911A: so3

·11 ~~~nd~

-2.0 +-~-~-.----,-~~~~.-~-~-.----,-~~~~.-~-~-.----,-~~~r--i

0 50 100 150

Temperature (·c )

200 250 300

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CT121911B Graph 0.5~1 ======~~--------.

0.0

- -0.5 .Q>

~ ~ u: _. <ll Q)

I -1 .0 I I ll I ll I Sample3 Sample2 Sample 1

-1.5

-2.0 -t-------,------,..----,,----.-------.---------,-------.-----i 110 120 140

ExoUp

130

Temperature (0 C)

150

Universal V4.5A TA l1



CT123011B Graph



CT010512A Graph



CT010512B Graph

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CT012612A1 Graph 0.0~' =========----' ------------,

-0.5

-J2> ~ -~ -1.0

IJ.._

(ij Q)

I

-1 .5

Sample 3 Sample2 Sample 1

-2.0+-------~------~--------~------~------~------~--------~----~ 110 120

ExoUp

130

Temperature (0 C}

140 150

Universal V4.5A TA

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CT012612A2 Graph 0.0~1 ===--I ------------,

-0.5

-.g>

~ ~ -1 .0 u: m 1 \\ II I Sample 3 I \\ N ~m~ 2

Sample 1

-1 .5

-2.0 +-----,------,------r-----.-------.-----,--------.-----l 110

ExoUp

120 130

Temperature (0 C)

140 150

Universal V4.5A T A It

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CT012612A3 Graph ~~ ~~~~------------------~ 0.0

.Ql ~ -

-0.5

~ -1.0

~ i ~ I I Sample 3 m ~m~2 J: Sample1

-1.5

-2.0 1)---.---------:;rr~---,----~--.-----~---,.----_j 110 120 130

Temperature (0 C)

140 150

Universal V4.5A TA ExoUp

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CT060512 Jar 1 Graph

-~ .......

~ lL -«< Q)

I

~1 ====~1 --------------~ 0.0

-0.2

-0.4

-0.6

1 \\ II Sample 3 Sample 2 Sample 1

-0.8

-1 .0

-1 .2 +-------~------~--------~------~------~------~--------~----~ 110 120 140

ExoUp

130

Temperature (0 C)

150 Universal V4.5A TA

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CT060512 Jar 2 Graph 0.0~' ================:::::=..._' ------------,

-0.2

-OA

-Ql ~

-0.6 -~

-O.J \ I I Sample3

u:: Sample2 - Sample 1 nJ Q)

I

-1.0

-1.2

-1 A -+-------r-------.----....-------r-------.-----.------.-------t 110 120 140

Exo Up

130

Temperature (0 C)

150

Universal V4.5A TA



CT022612B2 Graph



JCT071412A Graph

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JCT071412B Graph

..-.. Ql

~ ~ u:: .... (1) Q.l I

~I ====~~ --------------~ 0.0

-0.5

-1.0

-1.5

Sample 3 Sample 2 Sample 1

-2.0 +-----.-------.------r--------.------.------,----.---------1 110 120 140 150

ExoUp

130

Temperature (0 C) Universal V4.5A TA



JCT071412C Graph

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CT082612-1 Graph

~

Ol

~ ~

3 .Q u. iii Ill I

I I 0.0

-0.5

-1.0

-1 .5

-2.0 40

~

60 I

80

1 -V\ ~

CT082612-I - sample I CT082612-1 - sample 2 CT082612-1 -sample 3

I '· ! 180 200 100 120 140 160

Temperature (·c)

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CT082612-2 Graph

o; ~ ~

;: .Q u. iii Ql

I

1.o-f=l ====;::~:=!::~ ======::::::;-------~

0.5

0 .0

-0.5

-1 .0

CT082612-2 ·sample I CT082612-2 ·sample 2 CT082612-2 ·sample 3

-1.5 +-~~~...----,-~-~~---.-~~~-.--~~-~.-~-.--.---,-~~...--~--l 0 50 100 150

Temperature (·c)

200 250 30



CT082612-3 Graph

-

~

g

;ol 3 "0 co

~ ~ Q.) "" c: 0

(il ,.... () ~

~ .. 0

-

~~~ ~ &! ~ ~~ www ' ' '

Il l "' "' "' .., ,.... _

Heat Flow (W/g)

6 f.n

5

i_

;;:---

../

I

0 b

'---



CT1-0013-111 Graph



CT1-0013-112 Graph

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CT1-0013-113 Graph I I

0.0.-----------------------------------------------------------------.

-0.5

v -.g>

~ ~ -1.0

&

u:: -«S Q)

J:

1 \ II sample 3 sample2

I sample 1 If II\ -1.5 -l

-2.0 +-------.-------,-------.--------.--------.------.--------.-------.------,--------i 100 110 120 130 140

ExoUp Temperature (0 C)

150 Universal V4.5A TA



CT1-0013-114 Graph

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0-.----------------------,

-1

......_ Ql ~ -~ -2

u::: ..-ro (1)

I Sample 3 Sample 2

I \\ I Sample 1

-3

~+------.-----.------~-----.-----.~----.------.-----,,-----~----~ 100 110 120 130 140


150

Universal V4.5A TA

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0.0~--------------------------------------------------------------~

-0.5

-JJ)

~ -~ -1.0 u: -('0 a> I

~ Ill ll

Sample 4 sampte3 sample 2

-1.5 ... Sample 1

-2.0 -+-------.------,----,-----,----.-----.----,-----,-----,-----l 100 110 120 130 140


150

Universal V4.5A TA I

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CT1-0013-117 Graph

....... ~ ~ -~ u: -('0 Q)

I

~~~~~~ --------------~ 0.0-r----

-0.5

-1.0

1 \ II sample 3 sample2

-1.5 ' . ' sample 1

-2.0 ~------~----~~----~------~------~------~----~------~------~----~ 1 00 11 0 120 130 140 150

ExoUp Temperature (0 C) Universal V4.5A TA

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CT1-0013-118 Graph

,-...

J2> ~ -~ u: -m Q)

I

~~ ~~~~ --------------~ 0.0

-0.5 ~ r ~

-1.0

] sample 3

I sample 2 Sample I

-1.5-l

-2.0 +---.----.--~--r---r--..------,---.---.-----r---r---.----r--~--r---r--..------,---.-----l 80 90 100 110 120 130 140 150 160 170 180

ExoUp Temperature (0 C} Universal V4.5A TA

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CT1-0013-119 Graph 0.0~' ============::::::....__' -------------,

-0.5

-..!2> ~ -~ -1.0

u::: .... ('0 Q)

I

-1.5

v-- \

~ ~

Sample 3 Sample 2 Sample I

-2.0 +----..r-----.--.-----.--,--,.-----r--r--.-----,--.-----,---.---,-----.--,--.------r--,------l 80 90 100 110 120 130 140 150 160 170 180

ExoUp Temperature (0 C} Universal V4.5A TA



Appendix 4A: Apparent Shear Strength of Single-Lap-Joint Adhesively Bonded Metal Specimens by Tension Loading

lntertek

fMt.flllE:t'"•C.:I P'{!Je:.:l NumbOI r:us1c:.mH A,il'C>"LOI' A,._al·>'~t

uale:

TK11D Adh~rJ•:e /'v~llCSI'IC. l ·nC"-"'16,S:::i.( 11;

A<Jhe~n.-: -y:)f.' ~111(\11.:'11(.; -h.ICKiU~.SS .; IJI ) M~lf-1 Pr~r.-.3r;;,tic_ .. , Bon.JU•g Gcnt.lt ous T.;;s.i SnF.o.=o.J1 SaJn;:rle Coud1t•e' 1!rtg T~!'i: !:n!'lr.it•nr ~

Sr1r··p1~ ~.a-:>-e

P H04,$L$.<l01.F P1404..SLS.OOl.F P1..0A.SLS.tJ0-:J F P1404.~t.S.OOU P1404.SLS.005.F f1404.SLS.OOG.F P1404.SL~.OOT.F P1~i.St.S;,008.F

PU04..St.S.OOi F

• Apparer:~t'Sheac Strec:agtl:l Of Single-Lap-....oinl Adl'ie:.&ively Bond'ed Metal S~cimens By Ti!n9ion lOading

• ~ .. S' M 0 I JI)~·~J,C ~2013<1~1.:·2

nfoS.:;,Tr.l< \.·:lr1J:Y3~ion C~1,rne-J).'ul • ·.::rreir;. :( C11rh:··

: O<:!cemtx~r4. 2C:~

• 8.-,selrne 1)'lki' ¢Wl'".

Q.:.l1 J (~WC'i!G:.:.:

~ .,.,, "'' """''" , ... , ... ....,....,.. .. ._

C.rtli:n•11 ·M;.d t:y ~uot; :~c:i ,·'il :;dherend bicllr~ss from OW:r.=!!llap joint lhic~ne?-5 .L.b . ml'ill""~ IJ.J!$:J . l'lkr-ov~.

J'\ktf:.:'IIH 0 (.1:; oim n U':IC~n..: Jii:.; .. ;,:o

· WC • 2"C /50'}> • 10% RH

Alifl<">le-11 O·.·o:-t.,~ lvl;))(.l,lll-._m ·Snea' l y':.~C>O' AIIIQu •~

foN::J ih L€'\qit· Lc-.ed S:Mn·;Jih fO'!ili, 'f.- ~f F;::; ~··e nn; :in) ( tli"l ;p$!~ (%)

'1 c~ C:,4 .;&1 12/'IJ r\<W~SII)Il :C> "'~:;) "~0 1 C{l C.:S I GDO 1350 ?.:j t;.gs!bn :t:· ; •· ;.?;a ' fiO ·lc;l f: 51 7tlB '''10 Ac:h~!'iinn : \.(lt'~~i'.·A ~SJ"~ :J sg ~;:,...:. .:,~.;; 1e~1J :\a f"\c-!or tQ •)le~l ' U(.I

!l,!'Ji.) C,t::.! 809 1t~(' A:.hc:i ·::11" lo !111:'-l.al · ao 1 Cl c ~..{ 72;) 1Y.C. A:t "'F.S nr io mel;, I . 00 J &g C 5S 910 1BJC ,.!.,~ -._eS .:w to metal ~oo

J !.i:J ~.t-2 ~UD '1;.1.40 fo,:J ·,~:~\::•· fo m~t.tl ! J(I

l Q9 t:&J ?G3 1.<13C• A:t>"I;>;S\:";1" io 'l"'(o'\;;1 ~:lo

A.\'UI¢1Y~ 776 145G ro.~1 "iwur- GG1 1.120. Max.·,,,\,fl• S18 ' 166~

tl\~t!l~k i'b>~iu ' !:;.h+:,I;;IW IAIJ:.;,I':Ii~t'tl ·~u.~rll ~'C-1\S.I,~ fo1 ~he·~::~:III~We \1:<:-UI l 'lt ~~~'lUI? ,.,.,~11'" thtf ~It YJI:<t~. ~:l..:jloU;;s!,o;;n, hJ.•oi itj:<J" \ II' (.'(I' ~,( !lo< lo• ~~~-1< r ll!<lii$ r,...•iii\> ... 'JI'!'<':;;;o.-.I!J ~!:) ''""'Ill' •>r,...•o•oit':t~ t>IH'I'~ -:<\ I'~JIJ'>,'j ~oil 'll .. ito:J io• "'jl ·~, ~~\~1>\Ji ... l '~J ;!JI\~ ~;!fl)' 11 '11, 1:; l'ljl , . , ... ,;•; , , ~..,· ~•·.,:•, ,'1·••:1!,, 1• ,,..- ,,.,·,. ~~,.,... l;<~h•:l, ""'""'' (''"'' ~~· l> """ )'"'I"' ' ' iL''~ -~ , .,.,,.,·- il!' ;.,.a;~~~~••!!. VI' II•" \f ol<lil ~ >·t>!'·•l~~ '" •il!'il"' ' ' "'"' ..,1, , f"~l .i:.l'> ,.. ,,,llf~i•~ Th. li«hlil )' ,r h •l!ot.,:.. Pl!f.<;i(l 1"~~· ·· •1:;~1'/ 1"1"'''"" ' '·,., .,,;,,, •t~!'"''l :o.u tr<i;.,., '""~"~I~~~ I~ !ilril"'' ~:; t·~i> ,, .~''" ' t:' f\'I'Lt1~1l>'Mif:r ,\;If! t,u;. otl' <H i/rf-< olrtl r:n · i.u lfljo il•!)' .'<l+.•S~:;o,;.o''l ..;.. ''"''-'olS~~.

'A 1>~·1 $1tel!.' . t~U<>'i.tlt), ~.t., (!1~,1)· Ph,.,!!~ wJ~4~m; '"'" i~?J~9

i ol Ill ;,v_,,.\~ •Plli-o<,<,o!l'



lntertek

l es: Mefhoo ProJe~ N..,tmof!f c u:st,m le-r .Atter.uon Ani:ilysl r)<l:e,

le$· 10 AtlhOSI'/U

Ac:h'*'i·•= Tl"-ickrf\SS (h j

AcheJF;"l(l Type Acll~r~:nfJ r:1ickr1c~s Hn; Me1a P~~mtior·

QQu"~..:.ng o.~.riJJ~o~~~ Tn: S·~Eed S,..mpiP. Cont:iti:>.""~~g

I e.s: COflCMIOrS

'Samol@ Nam~

P1404.SLS.001. 117 P1~.4.SLS.OQ2. 117 P1404.SLS_.Otl3.11~

Pl4<14.3L3.004:1 fr P1404.SlS,005.1H Pi<I04.SLS.00$.117 P140d SLS.007.111 P1·4U.1iSLS 008.,11 1'1404.SLS,OOD. 117

· A.PDI~nt Sh~ar Strength Ot Sln.gle-Lap.Jolot Mheslvelv Botfcled M9tal Specimens By Tension Loading ,e..STM DIO'C2-~r.

• ?20·I34sc2 : lnfo$ciTel\'Corp~ (;nidn

C.~rr•c-A1n Forroua :I Cerii!r: n~,"'I>er 4, ·Ul' .3

· aas,Une ; U·' k.IIOWP · o 011 (:=NeraAe)

Ocl<.;rm\l'lCd tly sUbhi.1ctipg a:Jfl i:!NJl !d lh.ir.:k,·lrJSS m:trr ~'.>•;c"r3J. 1av jbir·L t.hY; ku!J:iS

· Alu:nirJ.II"' ; .0.05-'3 · Ur1kno>Jm

Jnkr'IOwr·; : t •.Q5-in.:mh · V'\r.ontiitr.J;~o ; l3°C !: 2~C 150"h.!. 10% RH

Overlap Maxim till• Wdlh Le11gtr load

( fo} <in) i lbf.

P.S$ ·c.!·3 IQS•J 1.t•) C.&3 I•J3D 1 no n b5 ·) 1?(\ I,CO C.5:S iOt!O ),;;) C.51 998 ·J s~ .c.s~ SS2 {l.tf:} P.P~ f161J j%1 r;. -5~ 11r.0 a.s·:~ C.51 963

Average. 1040 M"'lilr•l\m e9z r;'i;}X(Il'IO.. rT'I 1160

- - -A:l"pa,r~nT

S1ear Type Of /\"'10\..0:-ShEngtf.- Failure oJ FaiJUre

(Jni!j ·:%:

2·J03 ~hC:sion lp mblal l((l

1950 Achesion to metal l(o:l ~~4o) Ache.sion to m~ta• 10~ 4!-:.14:,) 14,UhCSIU'I tO III'O:IUI II);)

19P.O A(;tle~ion ka metal 100 1640 AdheSIOn to metal 100 217.:1 Acl;lesion I\J rrlj.>ll:ll 10:0:1 ?·J~O A~llesiorr to tn<':ltal 100 ~ ~~ o Adh<:::SnJn IO lll¢1:11 100

tgao te4o 2HO

I'll;> .. ..,< " "ttlel' T~1~c-~· .111:0'n~:1il'> l"l:t"'l;,oitA i<<~.>tr...:u t'>r. ~o,c;~-.. 'i!-;,st: ,;f 11-ei.l<i!<•· ; t(!·.~1'D .,.. tt~:; II"( :d:lr~l!ll. ri" I::'.J~V.I r· ~~· lt!\11'" l:::t:Jt. ;)f ;l~ott!lt !~C~ "«l it> 1..-\l·•o:,;l(t~'V' l_i11Kl'MUI:Sf\:n:·!S ;7t:fll'ltt~ t"lMpl<t~ ~·~·~"·~;· ;1•.1!1\>)' 'l~~ I~Y!r :il',::l .• !.o:tt:e'' -~"!,! i.~;;o l_$·11fol,l~ ~I''',' to :~.c-~11!\ :n'c ~~·;:,J;, ~!-'\L:.b .c~ p·~~~~~ • .,~ ' A:.wt.:. -::.~II'II'CC-ll ~1/f\":-',~C ·.,,.\~ "'~ ' ' " .: .,,.,~">.~~,. ') i}'l11:~f.•::: ~ :1-e :1\Z ~~~} o-.;-,m•~l ·,of \o "l'll~;,· '"l'l:rtctl~lr. f.f!OU.~ : r ~l;t~li>O. hl'.li ~:.oi!h·o ~>' r.,o ,\'":l'k -".~I'U:i:: "R-.:1'!10'011)' .llll'VJ<' '.\"'"', ~..::•:11 f~~ t:. ~vi:~- r::n:h:lta }!Holl tl\' I:,, ;, ;:;J 1a ? < ,tft'O<J'It of ~'«ll:lt ~'" 1;;,!-.; It•· ·~ .. '• \l'l'olru :.11e nt lnU .. d~«r~ to··~~.,,!;"' ot .... ·.,~:~"'·

!otr!\e<~~•l <>• •..-~t. l'ln<·f ~l.1. fAA ;!lit: rf•o<""' ; .... l: .l'l')..Y.aJ ; ;u:. "'" :.tll9

hl!f<•',\ w\<tt .... ;'lfl ,,«~M



lntertek

l t:. ~l ),,.~lhUtl

Pu:· ?.c: Nu"""t:i<r C .... $tomcr ..S.t:f.'nlie::·, An::.t)":5; l:l~IC

Test tO t+.<.lhesi'..·F.: Ajl·:lsh•e -h.IC.<.hHS :iu:·

A\Jhe!r:~nd ·r ~·pe A:iJ'I?.rf!nd Thi:;:~ne!'.s (L-.) M~lall-':eoO'-' :iDn 3:.:r· :Jn;~ Cont1iliC.lsTe~tSr:~,:;d !:>:~r .. 1.1t~ Co:tj !Jon )•9 I Test C!>"'~ndirir.n~

$cW!f:>¢ N~ltlc

Pi4Q.{,$LS.Ol8 .f P1404.SLS.OZO.F-P1404,SLS.021.F P1 ~0A.SLS:.0"!2 ,S:.

P1404.SLS,02l.F P1404.SLS.02A.F P140oi.SLS.025.F

F1404-SLS.026,f P1 oo•.SLS,027 .F

AP,patant ShOaf StJ,ngtt'l Of Sitt\tlll:-Lap..Jornr .Adh~slvcly Bonded Metal Specimens By·Tension L-oading

i \S"fM D'C02-10 P23'3115.:'J2 t1f;'SciT~x Co·~(;:::~on = .. ~rie-Anr Fi:!r':c-ta 0 C::u;p._r u::ccr-rr~c .. 4-. 20'1\..\

Dry Extreme Tempe)".lfture - Hfg)\ l..,.n'·q lO'.'·'!'l J.c·.c •:a\•e;-;;9~:::•

~ ,.~ .. , ......... '" , .. ,_ ........ _.

De:e~mine::l By _suotro·~ n9 o:::l f".e:rend thit,k'l·~~ i'r<tn- crte(Ll! ~I> J<;irt.:h cKne~t:

A.! .l,ffl llj.l ll~ j Ct13-tn~1(1,\'0

Ln!<'llY•\'Il :1 f:-1j in/r · in l.I'1(;(111'J!.tC>!l00

1SO•f (82.<;1

'-"ii.i1t.

~· ... :·

O.Yf! u.~~ H"J!: 1.0C ogs v.~!J o.9a r.· ~~e

C .9~

.!.,'/!';':1:9 !'!

··~''' :u~m Ma:.-irn!.in;

r.:..•eJlaf: -..la:.:.i,r tJfli

1 e.n9th I (ia.J 1)1) ~ It I.:

I) ~>I I (If!·:; o .•• trs·a 0 5~ El::•J 0.54 !J(jU

0 . .51 973 0.5 1 742 6 . .51 87/,

0 51 eM;.<

o.•~ !J:i!j

919 742 >oao

A:..!>41'Cn! S -!l:ar T•t ,::e !":it Ar.t~uf'l : St·~..-,g:t .. F-.at!(.!fe Qf F;)ill.-re

~~$<) (:·~;

21::(1 Ar:hesion rn mf!t."il ftXl 1~:Q 1\d 1e-s1~ ·VC~hes (In 95 : ~ 197<! Ac:he~ir.n In mel;:ll 10~ 1G~O A!-l ll~\; 1~~-..'t>~~,~ Ul' \)1£ ,I s 19:1-) Art n F. ~i~i'.'f:!'YIP.$ \if' ri:'>i fj

14N P:;htJ::S-ot to m~1:011 1C:J 17~·) Ad"'(;!>i::;··iCt:o'il:!t: ·:>r. 9c: 5 16e ·~ Ach~!'iir.i"ll\1 met~l 100 162·J .C..CilC:SIO!l l{.f!nt l:ll 10~

1711~ 1A7fl :! t54l

1!1:~,-:o:)( l' ~tb ·~·".j!l"(()-~;;)' t.¥bol·~l>'lj:t·l:~r.~ ,:,·~ tl>WM fv th• e~. J 'si.<t ~~~ ci t,!'C,(I'!U t?w.nm t'l:'i ;u: ~j~rt,~ . \QqUC•:Utl:ll'~ (r~'-:lltj;q•t; ~ ~ 1!\" <•1 !I·~ !lll"''!"'k !'l'<).:io\ ,,.,~+m;f~~Jt ~:n, ,.;, .. ;,.._, .,,.,.,':' l> t•~•·•· ~l"'tll!».~hl ,.t "'>.fl'( .» 1 tJl•t;;o o(~.\' it• \._flli rtf, ~~~"''~"''''* '"'~!J"·~~\1\II!U'!\1 IOJ l.''" \ f "':if i. "'"'"''"'*\ 1•t · l.•1• ) •·· :tl<" " '-. :">1-::~.l 0:'>4~rio..,~~r '>-' ''!!fl!•*<'•·•l "'" •••• ""''"•)<joi~ r,.J;~IIl 'It' "I '"" t:\o;ol rl]"" ' ,,I_ ... ,(<>:J ;;!'~il!i\111• " l"''"'i" l.l. , , o;.t o: l~- 0::• 1'!'""'-.. l t,,. ti:~t;ili~-,· nl 't•·'t'' il!l! l>t.e:\il.Jo· "~'"'l•~'J!i)l ' "'·"''""d"'~ w i1h '"~''!:"l ':.> ~.,.,.;~!:') '"'""'"'"'-,. 1h:1!! I~ {iwil!c"ll ~~ t.t•~ ~"'' ~"l q l (llf~'($1'111 ''"l'""id t•v~ . .:!) ~.l'ro1rt><' ;j"d 'I~ I 11'/'li.d~ il 'l'o t·\llO"~'·~•\Iiill ( l ilfllii,H.

W """"'' Sll(fl'l.> l'ltl<' !,\1:1, MA. :H::lOI l>l!~ll:>: :<11 ~! 411!!-·)')10 'IIK.41!1-JU!I

tnt.d.\"'""' ·~'I J'tll'i'l



lntertek

T e·st M e~ho'd ?rojt:c1 Nl ·~I C .tstomer Atten:ion An~lfst )a'i'!

Tasl IIJ l·.~l" ~Sl\'e A.dtesh.•e Th cll.ness i ir·)

A:h<nw:J TJ~~ ;..~'\P. ~.;o:r.:;l Tt'ti~kr<e5S ~ir'l) M~l91 1-'(c(J~!~ IIoh

~:-: "''!t l "'rJ .Cvnditio~~

I t:st Spc.t:<l 3:~-·r: ~ C~'ld.l ·:>nln£T~S:l ('.onii·ion~

SC'O'fpll:' Narne-

P1404.SLS.019.11 7 P1404.SLS.020.117 P1404.SLS.0!1 ,117 ~1 4o4.:U.G.o~z. t tr P1404.SlS.02:3.1 17 P1404.SlS.024.111 P1404,SLS.026.111 P·I404.SlS.02o.11T P1 40oLSLS.027 H?

Artp;mmt St'rcar Strength ot Siugi~.L<II)·:l<Sint A(11\c$iVoly Bonded Metal Specimens. By Tension Loading

: A.STM ::1C!l?. I(• . P2ti:'45:02· · l llfcSciT~>t Corr.,o~tr:v f!a~II~·AII'l fC ' IE:IJI:!

11 Carter· oe·~be1 1 ~!)1~

. lley Extrem~; Temoereture . High • Urv:.n·own • C C·l 0 ·: ~\'€-r£::;1€-)

Pvrc.1".se Oroer # · 13! 7 :-s

nf.-tEt.m~in~rl l"fS~•.I'J~;-J;n_g; .l)fiM'er d th't~ ":~~·t· f··~"' '{i·Jf:'Z :1):) Jel1t t•·i~kreS$ . A !.IIIIIII•.(III

• !'I 00:\ • lJriO:.IIOWil

• Lln<nqwn • ;,: ()~ ll't'111l • Gno:.)nJi:ione:J · j 8Q'F (82"C)

·.\'ict'l f.h:!

0.0~ O.'il!i ... ,o ,., _ar: 0.~~ o.~E 0.9'5 0'.9!.i ' 00

,.).•,_..:3gE" t.'in•rtl•.m M:il;<Jf:"Ufr"'

C.v~rap

l•ngtn ( \lj

0.52-0.5(• 0 !it) (J :; ~

().:;,~

0.5& V.5i3 0.54 (I ;, ~~

,\ppN.e:nt Ua~iru-· .S'le-ar Type Of A"!'lt:·Jn:

L<.l~d StrMgt'l F'a1 ... 1re 1fr£~il ,tre

ilt·l:· (psi)' :%;.

'440 292.0 .4,chcsio•llCcllesi~r. !J-J i• l '3G3 2~03 /4.chesion1Cof'l·esi::r 91 ! . , !<!(":/.) 2(1 t ;) Ach~;,io1t'Cr,h~$iOr ~O !' :l 1 57~ ?.f.l7:l A(;fl,..~i'<'''Con¢~·~,- so :' t :l 1SN J::IJ.U /\C tl6:iii~ ·'•.'GOi)('~•~r'· !J[I / ~ J 17~0 ~263 Achesb'iiCo;tes or 8Qi 2J 1730 3-153 Ach~t.ic1:cc -.es-or SO i IJ 16(!-:.) <! 150' Au l11:'sl:.: .,:::;u'l"s -;;r C0 / 20 I Sf.' ~~·al AchP~im!Or:'"'i~ or ~(I )' I ~

15>0 ~000

13>0 l~10 1000 1.280

lf~ll.n~l: Pl:r;::j:l l;::r"'"~Si' l..lb.,,l.~(>'l,f:~ "(p:l,r.~ ,)"( IUJXIfo• ~rc- tYO:,I!ISI\'(' ~< 01 t"':\ ~1;.-m t.lW"'~fl'l tlltj! .:It :.dn,ru·.<~d . "'q~O::tJ,IJI'S f'O., :tj:O.":~ ~ o.St~t :r.c lr-~trt<:l:( PI:UUG T«1ftt:)~ L~,l:t.lto1e,S "1,;1>1'1'! t:.p-.nn~t:l C;«!,ct ~ CI(I)'(Uit ~olt,):I\UC: \r Y,llt.1~· ~tl:o:trdtC~!)::H'I:tl1_1fP'+I; t:: l'l e ~~ul'l: ""~(.(:' .11\. p'O:lllr.::~ "~ ~t~.r.o:u,"' t-:n,--t r.~:n'n:l(J 4: $.1.1r.e•'<'d 01r.d art. 1\:.t _rccc~fltj '\:1!(:/J~e oft!'l:\ 'lJ..)Incs d:"'t;::~ . :1 ~lll'i!ilt 11".1!~,.,1\ p--oXI J:t Q.• ~"C.:SK'$'. tl'C ll;!bl!lt\1' lifJr:t:mk 1'1;&~:\U ~:l!r~l!~i Utlai~O"(S V.'llh ~S~I),.~ ~C :~_M:IS ~11«-tC,d :toll be- hlrll'!:l U t':l! :no.111~ ::;' !)):U'd~mr; Cl:t.d for ?J:I! :cr.l«S ;,r.d nt: II'C!U~.= lVOOIIS:~I:q\1-,l) d'ma~<f.

:;.) ~1'1 !.t'(.<~. ~'ltt:hrl~. M.'. -;.il:tt~ fii-Oilt: (4 1:1j ""~ •:n; 4;':1..u"J'

l'tr.p:I,V.\W•.Otl t.e?lll



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r:::-"''"'9 I 'j"'~lil M~:h.:C

Proie-::t N.Jm.-,P.-· CliSt::·...,·e~

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.t..dhes v.:. Thl::l~ne-s<> (i ;:•

,.40 •lC' c··;d 1 yp:.; Ac"'tr 'F. ·.:1 T-.ickn:!'il'i ( n~ Md•.g Prvpar<:,ltOr' R.-:.nrl ins C>:wdiiions .::stSm::vj

Sr;mp.e Conr.\ti.~•· ing los: Go11l tor·~

Sa~np!e- ~<Jme-

P1404.SLS.GlO,F P1444.SLS.Q l f .F P1404.SLS..012F FHc)4.$L.S,01~.r

P1~t4.SLS.Ol4.F P141~.SLS,Ol.6,F

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Appare,n,t 'Shear St~ngth Of Single-lap-Joint Adhe!iively Bonded Mct31 Spec linens 6y Tetlslon Lo~ding ASI V 010::1~· 1 3 P2'Q13/.002. ln .. oS.: l ex Coi)XIr ... tic1 Carr;!.-.4r·n Ft:>1!'eira

: i) Co1er : De;~rr.t:er '1, 2J13

- Otv Extreme T\:lmptrtJurc -Low Ur'~IIO\•w C>.OI ~ {av-?1'3ge:• OF.t~r,..ir-e.-: o·; $.Jt:tr.=tr.ring acl'lero71:i :h :{:~ne&s frnrn <WP.r:o.lll;;n jr, o: t"'ir:kf'tess'\rur-\n' "-''l" () (J:l_,;

Ul'k.lla\'JI' lJrkn.:h•:r C.~iS , .. ,:,·,·ur, Ur:-::::---::1 tone.;

. ~7·F t-so•c)

( .. ~;:,g •;:;-"11 O·l~i13:> t/t;;j!.-rnn' She:<Jr T'fOFc 0: f:(n· r-:t1n.r

\1\'!;;Ut I..ZI'~lti -·~:.1(1 StrCI1~lil ra,lu'C e>i :~1!h.: tC

j'\) ·: ~~~ Hbl:· ,(.:>si) (%~

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"'1.30 J .5;3 !:76 ' 2GC Ad.h·:.:~i'on !,~_; ; "::tel 103 <»~~ ~ ti4 ''~2 '11C Ao:lh;:ii•)f'l tG> ,··et,:;r 100 1.;.fr} :.t.~S ~Jt. 'l54t: ;\dll<:.:l)!Ofl ~c r·;·.;,;tc: 'ICV •).08 ) . €•) 74~- '•5~C A-Ph~oi·on :t: r'i~t<> 100 •JQT 3oe1~ ?.7(, ·s~c: AdJ'1~sion ·:: r·~·c; 1c-o iJ !j~ :) ~3 e.>€ ' ·if~l: t\ <lt;eSIOil {Qf"'Ot3 ·JC·J lJ.Ut~ J <':" - < !:24 ·soc ;;.,.:Jfl:!!:iiOII tU(f'CtC Ill-)

h~·.;;r;e.;;r.; 727 1500 t,!'\irim.lm 592 1110

'l"AtliW"''U"' 971 1830

!r~ertcl: 1'1~~~ ~~ ~:tn~l::$'1 u.a~r:.t~<!es f«':trn· ;II~·~' :J:l<.11<~• :l't. .. e;x:lli~M·u:c-oi ~!I ~ :1~-.tt t~ vi~:. II' •lle~· .~r·r ;ade7r.:" ... ~. ~l ·:ILO'I.w ~·n f-o~1 --.:·~~s 0" O.St'~.f :I'>: lr~trt>:k l'l~'n!a li'.t;'ln00l)' ~ll:·r:rto~..es 1~m.e ~pe,Jr.t't <!X~tCt x cQ~~t,.:t.llt,l:fl:.i:dlr. Yotlt ,,..!.l. ~tr~;:·ril:l~por:'l au,:tvo'ltf tt t••e ~~a'o: m:~t'r-.:1: . .)"''Jt.C'U o• crt«U~ to:n:-d. c~ '"I~ o· .1'J·r.t;W ;:'rf.l JIC' n:t rt«~~ll)' l!l ~leoJti•C of m: OJ~I!t~ 'CI~IIt"3' tt l!l"l:ltfT"oli!' '·4!S. ~J~ d' «'-'<'=\~. It(' h3b'1!tS> of lr·:trteill'l»:ll~ !e:l'l'(ll~t·t um·rw:trc, •••itt! :o:~~t:t :o str.lt~s '""l'i':: t<J !I:,• b~ !!'IT;~\' :I t;- ne ,df'lt"Jur: ~·: ,,,.n\.dt''<!r.i;;o· "'d (<fo ·>.l:.l• ~\'1\'~<1'"'<1 11~-: ,,.., • r"J~ ,.,,. :~it:n•:.:~ol .:,l l lll'l'lll{i!l .

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Adhesve .t..riM !'-'y'"?. Thi~l<.nes& ii·"r.•

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Oo:1d nc Condi:ions. -f!st S o::ej $3.1"01> e Conciti~rulg -.;;:;.,l G':n:J to'u:.;.

Sam·ol&-~·"j!TI<?.

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A'pparenl She.~tr $t~n9th Of Sin!!lf·lap-Jnint Adhe$ivtly Bonded M~tal Specimen$ B'y Tc.n-.s;iOn Loa<liclg .1\S I M 01QOZ·1~

P?C:·1~:)02

IIHOSO ~~ Corp:wath>·) (;1;rr ·~-Arn Ftr·~in;

u. t.::a·t~i' ' nr<~?.-t.~r 4, ?$1 s

Dry f)(tl'errle Tel'nP"GtatUre - LoW Url:.utro.vr1 c 01 ' :' ~ ·,:f!r:"'IJ~) Uctt• ·· ~u:<:c ~~ $ .. t .ii'aCltllQ ~ll!lt:'fC"'tl Ill ckn¢~S Hn t ow1aU l;}:l JiJ. Ill hJt.:kJ'>NJ:.;~ A umin .~c~rr l{-03,3 Ur1<..nowr U1·Knmw C.05 i··.::nin U• ··~~·"d t'(•ned

: ~7·F t-ss•c)

A~,:>:~·;,wt ()v~r ;:~p M\l)l.' 11111'n S tle;;r -y'Ji-l O: /\I""Ol. t'l\

\1\'idlh -~riJlh _:;Jl:J ~~~~IIQ.U I F'="iluno o l :.~11!J I P.

( t.'l ( n; ;'lt.;f, (J:~si:l (:.~:

() 96 (l ::(1 '?.9fl ;>.;.;~r. Atl f";e~ ~~· !i;. 'YIP-131 1t,(l O."tl9 ·:J.e1 edl> · ~tiC AJro·~ ~r· to •(Jr.: tc:ll 'I CO •l.9o :J.52· "2,~0 238C t..:Jt·cr: ·:>r io rne!al 1C•J , , ~h) :.. c;- ':!CO ·n -::n l·.rl~.r:~. :'II"' 1() Mr:1n ,l 1 (;·~

(J g~, :I!}S ' 13~ ?I)Q:) • .:..~'ie$-¢1• t9 rtle-~1 11;)

1.:.10 :,) 51 ' 15C 2~GU A:.l ' ll::::OX.:·'"'~ to lllC!cJI 10) 1.00 J,5 1 ·;,.;c 2" -'IC A:J1F.~ ::;\ ro mf<tAI 10) (! f.l7 'J ~'l 'HC, / ?$C ,.:..dne·s·Qt >0 met:.1l 10J 0.:.1/ IJ.!5:i'i '14!.: 2Ctit A.;:Jt· • .:::: ~r · !6 qlt:;t:ll 1&-)

/\\•er~{Je 1160 2250 Mirif11 Jm 8116 1690

'M ,)Xi '"'.ll"fl 1290 26~0

~·~t)!d: iole.~ti;> ~•.1.,-(I!'J!j)' lli~JI,O'!V'il'~ ·o:~'(lo ::.~·<' i,~,.,.J ru· '.!•< t »h>i•':l .... ~ ~·' J' '!ll' ' jo!<ll> l•.) ' .... )t'JIJ) ~!ot:,.\lll t -,..)\llt~. \u •:jlf~' ... li\fo') fUt«l/l>j:(o·~· •• '·' " " r l·" l"l!!.ll"k l'l~:;.,•t.o lot•vln<Jr l<"""'l•:ol• ~ir.o ·•~'"!' '1- ' ' 1 ,. ,.,,.,,.,~,,.·"" "'1''"'' 1 ~.of<'~:;ri•~~< lo• ,.,-ilj,-~J · ' "'·'l!' '"' '( i ; >oj:ll·', .,.(.lt ly l t<'ll, 1:1 f'lf> jl:l:'l.i)" " '"'""'"'' l'' ' t 1,., •~ ( I' \fO·;:o,.,,.- ,,.., .. l >o~<o··io•;.:l.,... ~V"''!-0!•1 o<•l! l"'" o roo 010olto.<.<o·il1 ·o:livll),,. l ol "'"' o:• o:Olil~ \ 1..,.., ~ ... tr flo) •ti M .,,,.,, ol,\1,. I"MI 1;,1> ('' 1" 1'~1'>1':":' Tl •t lio<l:<lil ·,. •.•I h· :l!•!~k f'l,.y,i;,~ -,.;,loo•o\~,,o;,;y l iihJo:o l•.l'it .l ~•itl) 11')\l ..... l ,o) l.~fVi~O!'I> ff:'Otl\<#•1\' ~~ i<l' I"P ll.,li1,o!';l ~·~ ·1'1,1 Joo>')\ 111!1 {lf (M ;.'(;;.>-"iui."' p:;iol l(., .$1 .:11 ~M.~tfo~ iiol"'l fit' II tlol11" ' '"' )\IJl•l'>!!•·f•\lfAI II ~(I•OI!Io'\,

'N ;"W.,I ~H>I>I,. (o!tt<' iOII:I, f,1,), :I I~'

fi~M>II: 14l l: ..V.~:/9Sa 'IIX: l..,~~l!i l'>tlp.:.\W••••.Iirli ~~~~



lntertek

T t=;S·1 Met'IIXl P ':!lj~ct I~ Urr' br::r .r.u~:O:rtl\'=!"r Alte:".t~r

kll:i~•st I)~ :,F.

Teo:i 10 ·"\cr.e&i\'e /'..r.;l•~sf··:~ 1 t·•~Jt;r·.{;.-s:s (n )

i\Ch~Tf;'Ol't T)•frR

Ach~rcnd 1 tucl<rc$:~ ::u'> MF.:~I P~p.;r.:ll ~r

U~001na C~1'd lOO~ T~.:S:J.f.~:1

~~nlp!o GundtiiC",ulg T ~·1 (';;,nd :~n.

SniT'ple Niirr fo:

P1404.SLS.Jl46.FE.N

P1404.SL$.047.FE.I'I P14.04.SLS.04B.Ff.N P1AOo'I.SL S.O~I!o.FriN Pl404.SI.S.OSO.FEN P'404.Sl$.051.FEN P·1404.SLS.052.FE.N P1404.SLS.OS3.FEN P1404;SL$.0M,FF..I<I

Appe~..-..nl Shear Strotngth Of Singi•Lap-Jo!nt AdhesivelY Bonded Metal Specimens. B~· Tension Loading ASTt/ 01(J:':Y · :1 -?201.:..:~:::~

: nfoS(, -:r.~ Coijj::lr.:~1j:-:-• C\loTie Arn rem;.iro

-=tar 11.- F~ ·t ,!i:!'l,L':lry 3;1, ;·1';'1 ..:1

High ._.umidlty ilc.clets~ed 4 glng J!\kn-;t\"r

• c.tJ10 {c:w .. 'l~fy~.;j OetP-r-,ir-?d ':J'f ·: :. t:·ra'"tin~ ad'"le·e -.:1 Ufc.r"'E-3;!:' h1'n· d'fF' 'l.

• ,o;.l,•:~in·.lil• ,(;.('63

i.Jrkno·.·~r • Vtkn<::'l\,•r · f. Oil ir.''Yli1

• 30 t"layt: at 9011F, .9li% RH 23'0 d ' C I 5~11! ~ lOY., I<H

(N~.r~p IJ:;I'\1 ""'i(l "'l"'

'v'•'ldlh Lcr..g·:h -~a.::i ( nl .; n1 llbli

·J.a~ ::U:b (;_.')2

Bo l$> ·es·1 !.l.!J/ ~-~.6 o9/ ;).00" '·-~-1 <:a o~~, :1 f:f) 1'?7 0.93 3.~.5 ~·· .:J.!JU ;J;4ii ·<.4~

H~ ::1.5.6 ::!22 1 ~fl ~.54 ~18

J:.'Jerr.·;~e 182 M.inii\Utli &t 7 M~>:hiJl ~ .....

App:~rent

$1&-.'Ui Tyr,eeit SucnC\1 feu .J(~

(p?.i:l

' ll:l A.c'\tH>i::,"'' tO rrif.taJ ~uo r.c-1~i~1 t·:. i"llt:-~1 * i~ Au·tc.st:.:·-.· to •uet.ul 70~ !.<:h~s:ivn 10 'T'!>'lll:~-1.

· 1r:~ t..ch~~i,in I{Y m-etf!l "'OZ! 1\·~h·e·sion t<:t.tMtZII u~u :A.I.;I\'I,J~II.;.'IIl;J !rl~l;,l

''G ~·cht'!sk;o t:: m~.ut1 s~s /'.£h•;:sit:n t~ tn•::IOI

HOU loi 1 6>~

/','"1"t-J.n: ·ol Fail\o ll:l

; =:o:t;

10~

10~ i (o' 1C:'I. ·16J, 1G~ ·{co 10:t 10l

~\o!'<lHI'I:I>iiu 1(\l ·o';lllttt V·l;•:ol(f'·oa ~p:>~} l"'<!·h'I'.~"U•to o:~ .11;•t \l:t-·;f lheo:i~'r:110'''hO"'1~' :n: ;so:dte'~~:! . llo: :~....,U:io:r< ·;'1:>'"-'~oor.s , ,.,,,. ::' , . .., ' ~~••-<< 1'1~<~:•'< 1"- ·'"' ~' -t~tl,.:o:<> ":"·;,:., .,,.,,~ -"~·~'·,l(o··J oo>o,~l~~~ l'•i,..·,~f«Vl~-'.:'l.l\"'J i'o ••i·'~ir,; . • t~c•~ :o'!\1 ~nrt: o:~-.;,y :>"Itt:,: li·~· 'f~· •:;, , .·,..,.,,;.,, ,., ./:lo ,oA .,':- 1'' "'"''~ !oo\.f ... l ,.·_....,,.;,-.,.1 1;• ... , .... , .. _,,.,t "'"' "'" ,.,., '\~:-.M" 'i io oiO>~o;~ :;: : lo;o 'l'l<l!;• io•-o i::o ... k\11 •r ')i.-, <1~..-,,t~· ~f· M·':l·.r•: .u •'"' .. u;1o:, n·...,l;~•. ,i:.>· J•' J•"•t•~"" "'""' '" -,. .,,,.,~,sr ·~· ·~o:~ .... ; ... · ... : •· ... 1 ... ••; ~,. .. ,,.., .. ., .~, ... .,.., 'f''"'l "~ t,,.,,~\· w \•·~ ·~··r;~o•·t ~·' (1\MI:IIIII ;:If..rl :'>1o·:l '!\1 "·'f~ t<N«-J ~1'11 111; : -:o·r • ..-.l!t--;l~'~'lmoq•.•r,ll~l /J ~Yo~A:..

;r, -;.;..,.,1 $l ~~t. f'iU•~i~~l II A•)' i0'1 "'"'""· ;41'\j .. 'liJ.IJ{!(I.; ..... J'l'l.Jl~':l

l :lo1f1•'""<"Jiii."''"



lntertek

·<~:;ot r~:l~U·:Jc

Projr;cl N .. mtiP.I' t:ustu-·'mii"'

AttenMn ·.41'-'!ly~l Om F.

Te1;1 fC li.C'ii)3Ne Ad'\E6W TI!J':.:t;u~ss- (ir )

:- Apparenl Slie»r Stre_oyih Of Siugte·Lap-Jotnt Adhesiye!y: Bonded Metal Spcdmcus By TcrlSI()fl Loading

, AS I f~1 ;::1CJJ2-10 • P?C124f>) ? . hlfl:Scr f 't:J. C(n;O:r -a',L·:.:r· . (:;:; rr.~·.~!j rP.r~(7 r:;

, H:au<. ~bi' : ,,;nuar,• :loJ,"'c· .:

Hlwll Huflt!\l!ty AJ;ctert~f~ At:~ hi!;! . un~nC'\vn . 0 C1 ' \,:1 \IGi e>.g~~ D~;le~·ini!d b·~ subrr;;:-:t'os :-;rlb~rer-d thk b f.:\'i : •fmm (h'?.r:;!I IAr: 1oint lh r.!lnes€>·

.~Uh~! ;; .. · ,~ Typ<.:~ . A liU'fll.lm

;,c.,e-•ert:;J Thiclwess (Hft · Q 05:3-M~;" ~repgrelou

Bond o~ (>:'11"1 ;ti:lon.o; ·.::est S.c·eed

' U!i,<.II0\\'11 • L·n!<.nown · u •;.S il:/"tlh' . 20 d AJ'S 3l90"1V Ss:'lt P.loi Se<IH~'C CV;fu\l..~)'!I IG

"'"?.sr C::t l_;j iions : n •c:t ~"c 161)% :t ,0% RH

(}i,•t;I I-Cij.: ~.1Cixir';;ut•·

VVit t h l •ngt~ I (l~;J SaUIPI!::" "'eu liE~ (It•) (•'1) ilb~

P1404.SL.S.04.6. 117 o ~r.. 0 ~~ ~or. P1404.SL$ .. 0<7. 117 o ~e ·:.! 52 i ll9 P1.W4.SLS.048.117 iJ.i!& IJ.5~ lOtiO J>14()4 $1 $ .(1.49 117 •• .:;IP.. ·:I G' ~~?

P1404.SLS.050,117 O.!J.O 0.52. 55~ P 1404.SLS.OSf . 117 . )0 0,56 :119 P1404.SL$.O~:i.117 M 9 {) ~!> 84C P1464.SLS.OS3.117 "'.00 0.56 ~ma

P1404.S~S.OS4, 11? 0 9~ •:l!;i?. R31

iw~;;,'ge 1)9 Mirim.Jm soo ··.t;;t;.;imw ··· 1000

A~parem s:w,; _,, 1 )·;::~ 81 .Am:::J(t~!l

$ tteSlQ.\J' F.)ill; re tA f".;!ih ·t~ i~.$1) ~%;.

~S1 Ac'l'le~io:. t(l meg;l 10.1 15 1J /lr.heSiQrr tc meH'II 100 19~l Adn~::;i ~·n I<J rii!:'IOJI 1({1 17?;.1 Ar-h.;osil"'n ~., m~t.;~l 11)1

11t.'J M llos1on to n1~t~l 1(.\:,)

11':l. Ache!'\ion t:'l met~l ·tO~ 154-3 / '-Qhe$iQn to 1he't-::~l 103 13&3 )..(;hesitm to metal ICO 16:1.) Ac he~ion t(l mat~J 10.1

1410 98•1 ,;so

'!k ~:c fl:~~ro tectf'l::leo; ~:•:ltoru ~11s ;,-.: ~~~J:ltlto• :re cx-:! J~I\'1: ~~c ~~1h::c er.~ tO •,,tf3tr~t'Y.y :~•-:-:d~1:'ssce. r_tQ<.U~t~~o'l:. 'r.:lm •e'o'lt :r AI: c;t·'l~ "'<rte9'1~tte !'Sc"'roiO:" -~~~~·•:~to<;cs 11:1111~ e w..-.~:~~ ex.:::Ft~s e~s;•( :.·.lt'llr..?!3 IIIW' :lrq . ..ctt~ l ~o r:~:~ :rw•,. ; r !\• :c ~~~ ~'< lit ">~1~1!;,1).. :tl'?liv:tt ~:-~n::.t-:1~::1, o::JW'l .'ltd Cl" >'.or-~'Cd :trd :~te rot n~:r.:~_rltt ... ~~:~ye.~ ' :tc.:~\4l'~lu l:er-~•ul o• H';l 41 "!17.0::1., : . ~;;~~;~~.~ .. ~~ ... ~:~·;!·~·~,:;.~ ... ~~.f .. ~~~~ l',l.~::.~r~~~~~:;~•):'i~!:;":~ w-:~ r~m-:1 t ; "'...,.;:.~ re1,:1tri· 'i :'!ill 111: lt•lllkd ~c \te :t<nt:\M ~

5) l>-;o;lrl$1'~@1. l"itb"l~l:l U~<) l)~ ! 1'1:.(•'~"' 1111 ): .t~4:'~1 -=om .s'l'l·"J~O

l ., ll $'!'•'"~,·~.;;.~ · .• " ''-'



lntertek

---=s~ t/c:t-:c r· ... ,je<:t N ,m~e · C .Jtil:.!'"'i:;V

G.n~n~i·:.o And·t:.l nat~

Teet r: A:h..:.=,·c ;,~'",6:5 v.;l Th ::kn~~s :'il·:·

,\~,.e ·et~ Ty~~ ;..:J·T:wj 'I h:;!w,.sS 1)'1) M?.t:-11 l"'rP.:·o:; '·F. !ion ll~'"~ 1g Conod!li01S T-:~:~t !::i~eetJ SR ··r. o; t::'lrl t,;n nr, I •)Sl COI' <ii)Oil$'

~·~f,)r:'IP Nom.;

P .. 41)4.~LS.0~7 .FEN P1404.S~S.0311.FEN P14Clof.SLS.03S.FEN

• Apparent $he-..~r ~trength Of ·Sinsle'-Lap.Joinl Adhe-5"i\'ely Sonded M~:~t<~.l Sp..,citnans By Tem;;ion Loi:idhly

· ,o\.STV C1032···:. :mao ii~c .. u .... ,l:erof spec'f""f~!\) P~C1.3-£-i>O;> Pt• ·~tlace Ort.Je· ii '3·· /;1€-

: ln'oSc·TcJ: Co•f:W:>rali:::··, • C~rre A.rn rf.'rreire

rvt B·;,d•/ ; G. ~i111r.

f·,l~ff:l · ~ I , ?.:l ' 4

• .Ar;celamte-d Aging . U!:kuowu

C C.Jf.. ~-w~rooe.•

~ ...,.., -.c .. ,. ... , , ..... -.--

Ll'.)lcl '' ' illt'!.! ·:;t-~- L-:riJ~tintJ .o~Ui ft:IO.:''U th :;~rfc~s tlt.:: '!t :;·\,e!ii.ll. ~<:~;,j-on·: t 1,h::k ·,~ • :\ t•••·inJn:

C CO'II ' Un.,n·ow.n • IJili<OO\\:.h : ecs if·/·•lir • "90 days at 120"F / SOY• RH

23•c. < 2'C.I SO% • '10'.& RH

c ·.,.·c)· t~r.· ~.' ~xi"ttu "'", \'·.'ir:h I ~ngrh I :a~;, ~l'"'j i-1,1 ,l~f;

' , ;.,('; (J.!i2 7i~ ... ~~ (J ~.6 ~?:-: ,:,1;. (\ >• :9::

A\'F. ~i'lqF.- fii(1 lt(n m1.. .nl 59& fl;1~;(iJI' I il " ijolo'

AJ:j:j3'-='r.t S·l(:llr 'l!r:¢ 01 r\ m.:iv"'l

SlrP.nf:h Fn lw~ ·:f f;: l!r~

(;>Sil ~:·

' :'4:1 A~lh~r-ipn ·:'!-. .. ~·~ I•::.C: < 1V~l .C.!:iJ\e.s"~~~ ~6 -e:" K•C " 'IO:J l·:.lll'.::.;tun {:,; ···:.::c: 1-;.)()

11511 ,,on "4~

"\"• • -~N~~~'" t•"' ''"''".ll' ,,.,,,,.,.,, .. -:-' , ... ,,,,~ ..... ;.,,,,.,, r .. .- ~,..,,,,,,._,,_,,rv ... :I•~··! ' ~" ..... ~~~ .. ·J·o:>· ....... ,,,..~,~·· ~~'"''"''"''"···'····., .,.,,.,. ~ •'•f• o<J> 1'/ l?o- o',l"ll~ .. f'lol;(l','< n>.' 'll'(••"tt)' ,.,,,,..,.,,,.-,., "~"'";.. ' "''._.,,;o:t>r. t>,<:t'l'' ~">1.:\f~dl "+i+I"V"~"'" ·,..,.,.,;, ''lJ· I .. 1•~1, ,.,•, 1 'O:I)'f.• .,?\f\1_:,' •\'1., tl'; f!l~ ~~"-t:lh .,.,.,.,.(iH, :'oM•I•.tl~ (I( I"'"'""'>'~.,..,,,.,,, ,.,. • .,;.,.o;~ oo'• , ,io ,,._, • ..,, ilo).l ,.,,. ' ' '' ,.,.,,.~~,,;~ i•o:ti, .. !i, .. "' l•o,- ')-••Iii'.., ' '""'""' '" ,;., ii,Ot ..,-.. uo/ o\,1\, t'>KI:i+•P' ;or f'I'I'Y.('<~f'C, ~ 1',11'>.01?.<11 '11,1>11,:0< f.!,:l;;!n TMI'11<\IMIJ l.;i'~:II:.'M(i;< .. 111'" ~Cfltfl ;(. <•f'•lft><. ~N..:-·•~1 <l '.f h;. ·;,.;,.,.;~I !'II""' .:.1~•.11'' ~.! o»MI~ti.::ICI"' :Ill>.'! ':r SIICI'!(I"'~olr.:l r« :rr:•Jltl ~nlo'. :!:r~C:,Q._;.."It l cl3m3t;C~ .

[?~~~~(4~:t~~a~cl~x~i~'~·, 'ft'tVJ, ............ ·.~tll,.-~111



lntertel<

l :::S: f••lC :I'<:.~ ProjectN .!m :>e' ,"';u~r:-: .,.. P. '

/\ll(.:•~;,-:.n

• .:..n<'(l.:;st (iz,te

;;~_t IC

·"'(lne$ ve

• Apparont Sh&ar Str\lngth 01 Sing!O·Lap.J.Oillt.Adn~i'tiCiy BOn elect Met<tl Sf\et;iin ens By Tension Lo$ditl9 t,STV D'I(.':J::..' ;J fm0aifi~ 1Uf'T'!b;!r r,f ~~~,..p:J~·,

: P2C•l Y ·6C:L Pu·:.:Has~ Ord(; ' ll . l:':l 71~

• ln"oS.::TF.-':1( c;,,lft-~ri'ilic 'l : Con· ev/\nn I en pi~ : M 8-'3d1 : G. Sime

: Maret"· 31 . 2j ' 4

• Aec~Jcmted A9,h1y • U ' i(OQ\\'1'

• c.o:.:;J :.~·.··(.•l <~y<>:• r:>~Mr""'in~c -:1•1 ~. Jt:lr."r:ling t~r:h·ere"li'l ~h-i:":knP.~!'> fm~ t:\·~mllt.;n ioin~ th!<;~ 'f'IF.-M;

t\01'1!-'e ,')~ l )'l>e • AiU{'"IIl,ll''

Ath1e ·an:J n'i~.:l<.q:.;i:: ( ·•.l • c.-:•34: \.1?.:~ Prep~r?-~ -J;n

Ocnd 19 Cordi:ir.>1S T =:Sl :5~x:c:J

: Ur .,.no\\•n • Ur lmown

c.os ir\f1uir S-a'n~ ~ .C.ont:l iti:-~.~ lng :iii~ ::;;;:··,:J ~ou::.

90 daytnu'120"F J-50"/.. RH . u~c ±. rc 1 tSO% t 10% RH

O~~t~lhtp M:ix•··,.,.ra 'A'id lh L~r;;~ th L:::a:J

S~mi.lle• ~~.a.me O'i P"(: !Jllfi

P1404.S.l.S.Ol ? .1 1 i 0'.:;17 :H,; "8C P1A04.SL,S.03B 1, 7 . 31 :·. ~'.) ?77 P1404,$LS.Ol9.117 • . JG IJ.-55 e62

A·.:~:-n;ge 740 t_..inim·. m sao M3Zit '·~,,.... 563

AC;'13..:e1! Bhp:r Type 0 1 ::.rnour-1

St.~no;t,h F:;•ILn: c:"F,; !Ui i!

(~S~I :,%)

' 13C A.11"Rsior :c: ,...P.:F.: ~'fit! ' O:.'H; t\<ll•·ee.or :o- ,-.. ~:a· ' :JC ~ G7C" ;.:dt-P.sior ·c:· •• P.:;;: · ~c

13'7:0 1 130 1!\70

f ~t~ei: ='l~rt.a ~liiQ'Oi~''-:ll:«,ll:,tl:tHMr.tf);',Uil il$1;~11 ' :lf1+1}t iotll <li11:\'>,l~:t·(lt :t;ll tllt.nt~;~H'•Il(.n:t~y~~ <!t:tl~\,11:1, t;.~ !!l .irl,~ :fu~;I,,/J'I !(pcl~ "' J~·ot tile !-.t..-:;:.:k -~~o:su:s Tc:tn:s:r;•t ~l:")r.rt :u~r.-Jrr,< l~·!llliM!tto.'deHtO: .)~C?t,tt'Aiy .ll. :l'«<t>.'d n · ... -1~111~. L~<n.~:l r;~rrs :.;:,:1\•"0nl!<_tcJI>c -;:~~!fie M:11<rl:l:. ~r:dJ~ tt p~o:::-;s'e~ te~co, ~)~minco~' ~ll~'>'('ittl.::ntl :..oe "': n:~~~"ly lr~:!•<c o1 : lie q:~a!!rl ::::. tlll!'l:l:;~l « $·m·•;r ~tcr .:. ~. ~r ~co,;c:~ ~·r ~./):eliSe~. !~1: t~llit-t d ll!t:\1:tk f'!:l:t'c:: Tcdn :!07t ~:IQcrJI:n !::l t~lt!l ~~~<C't to kr.~oes ttn:l:'~ ~)$! .:!! !ri~ll tt·tlle :i'll ~~r:- 0'1 ftr~•ll<l:l\0'1 i:lli \1 f ty ~~~VI s~!:oi's :n~ fVJt 11;l~e<' ~r·y t~OJ<:IIthi'Ul:ll"~q'='>

~~~ ~l.ti. ~~l:d. ~-:uf·e'd. \IA IJ! l:ll ·1'1?1>~: (.ilJ) IIU O!IU ~ .);tH~S

11\t):• .... ,Nw.p:h.lt' ...



lntertek

,---- --- - - - --- - - - -Teslns

Tesi Melho:J P.·c.ect t·w-.ber C1,!>IOm~r

i\r:entic"1 Anc f;:li: no..,

lc;tiO A.dhqsi-:1:' A,(.lh~!'>i\'F.- f"'it:k'l~!'IS (1n:

A\Jh<:!f'l1-11' J 1' '/~"' AdllEo~f~llct l h,CV,IldS :ttlj fvlet)l P•ept'lr::~tion 8-:.mdi119 C..:•uJ ib~ir·~

Te~t·Sr.eec

S<..lmole Go~'<il:ir,.ni"a T ~sf C.•.mc'il!:.:~ts-

S O,r." l}c(! 1\>D~.re

PlAOA,$l$,llAO,FEN P1404,SL$,041.Ftl'l P14Dil.SLS.042.FEN P1 40ii.St..S.M!.FEN P1A04.SlS.044.FEN P 1404..SlS,045.FEN

Apparent S.hea("Strength Of Single4Lap-JointAdhesivet~ Be:nded Metal Specimens ay1cnsion Loading ,4Slr>.•1 0' 0'02-10. • Pl? :l'34~02 l r\1-:.:S::iTe:< 8:.:·poJ;;l.tm C:wie 1\n.· r.ar·e ";:; M. S:r~:Jy t G Si-e Mflr<:h ~1 ?014

Aecoteratcd Agbrg UuiW:.:'l/') o :l ~n (.>t'.'F. '~gF.}

• ........... -......

U:::t~'lll • 'k'-1 L:y -Su -..ba:Gt ·1y~di'CI~n1 lf\il','(,'IG'!St. 1!~Ml O••t ··fJ1 ~p . .01r1t lti ~t~ll~·SS AII.. O'!i"'ltm 0.061. Unk '"lOWO t,l llk'l;.Yoon 0 r.5 ·n..·r.;n 90 llay.$-at120"F /60'Yt RH 1BO'F (B2•C)

O·,·~rl(;p M<:u<lm.un ··,Vf:1·t- I F.Of:h lo<:!d

:u') :: ... ·:· ( bf;

1 ott 0.52 scs t: ~·S C· 5f:. 771 r. £·fl C<;s- SF,1 i O':l. C<.!.S 74.~

flGg (/,f,f: 7iG t:.$1 ... C·.~~ -545

Av "o:1i!yC 691 Mnir--,u~ • .a M<1XIJn~m eo a

~op;;~n:

Sl'oa I J·p~'Or /v·r~ .. m Stn; r;f1:t F:'lil:Jmi of F.aiLm,.

::r-s ; ·:*; I.&DO J.r..c:hf}sion. t: f'Jl.?t31 lC.j H &:l A(:·h~!'k,n lc. m~t31 103 •103-J Actie.sion tc m~t::tl •100 1JS•J .i•J:I IC.IoOit.~!ll") J"nQI;.,I 100 131(1 A<;hef.ion l:l' o;~rs 1(1(! l {)!.i:J /\•~1\QS;INl to n~et;:,. l(i!)

1290 16l0 1550

ln<:lr:tk I' .Uti~ !7:>:'11'"<)1:1~\' ,;1to.•.:.:tfl!::~ ~tS:O~~Mt l;,i5LCCi i : ll!I,C ~u:'•;t: liS~ ;,f 1ted,lt~ :.S ';Ot,1-C.'!I lh:oj ;If ( ;,,c'41CSSC:II. llt• C'~IO(~·if>lllli~)IU C( ll~!of~loc ll!t'!,-;ck P(:r:$1.ts lcct.'I~IC!G'tl.olb.or~:t+'!~fl~ls ~ertrll't~ '!~pt.n ~•et:llf~'-'*-o't.!:II1W~:!rq . .'tt'kf~ :1,~ ~~~fU.:IN:>'Il!Tir ~qthe .fJI!:: :!fc cr:~t-;..·tll.llo ~~~Jt'\~ 0:1 .)l~tc~:o<t ~en:.:c., ~:O:tm!,r~t -:, :~r~,c.ll :nu G.!e'l\0,1 ~~.S:I! v 1rC~I~!" ~; :tc ~""l lt\t~ lllltl':tul o• J""'~' .'tl:r.!:• •~~ pttO.r.u· t l · "~1~:.<1. l n.c: l~:r.tilltt t<i lnte."':rk "'·: nt:.s fep!!O.o;b' <-al:o:-~~Hcts "'~tl: 1:1pec ~~r-:~ rt:dc•~ .!'1,~11 ht lr?!Mel :e ~~c ~"1!:~1"11 .of ~l~~:.:r:ft~" ~"<'io: fu-: ,. ~:·• ~,..,..iu:s ~~~~: ·rtt ;,, ~I~Oe ~'J ~u·~~oeq~c•· :(11l uW<•, n.

~h••l $1J~tol "<t;~r~~~ MAl)' >01 t> ·,.J•·e: ~i·H) <~!I!I.OOe3 f.w <~!1_9.:>.3*

l•\t1:;;·,·,.,.,.,Afll1;.\..,.,



lntertek

T E:>st Mel_hq:t

P•st-ect t\Ul""''.~er C\ksloruel

AtH•tiC1 A:1oly•.:: 1)\;te

festiD A~U~~~i\·t:-A...1.h~~i·,.F. Tl'li;:«-nP.~~ ( in}

M herenc T .,:oe .A~Il~ICilc_ rll'~<ll~ ;Ul) f<•lo:,tAI P~~p::tr,1tir,:-o

Bowj n;g Gonu l{ • .WS T~tSpE;-~C S;:.m):lle Coi;di:loriil'~ lcY:.I Com;i,li~nli

fi~r- pi~ f\;~ T P..

P U04.SL<;.04&.1 17 Pj4&4.SLS.~41, 117 P14&4..SLS.OG.117 Pt.UW Sl ~ OA.1. 4'\7 PI<W4.SLS,<.'14. 117 PU04,SLS,045.117

AI)J)4'1fe!ll Shea( SttCI1{jth Of -$ii\QfC·l<:~fHOiill A(IMSivCI¥ B'CHit'JC:'rl Metal Spetimens By Tension Loading A~TM 0 "C02-1C P:?:r34~(12 P~l~";osc :::-jer#. '131 /li~ hi·:JS::iTex 8[:; por;::t.on ~t'l r'•e:·M•r r er·e ·a 1J. Bra:J.)' : G Sh 1e

1J oroh 31 ?.014

Ac&elerated Agfng U•ll<;lp·.·;u (1:1':) (.~·;'F.-';<!Qf! i

lX:tcrm !l~:t 1.; ~• .sl.J:)((St;.~·ry -~jh~!(;ftd Uut:l<, "'t:SS !low OV\.:'( ;lj ap JUI" I .~It l:::kflti!I>.O

Alt mi"'um o::Je"'

• llnk,r:;w'i

Uukr ::.'l/'1 O.fk} n.'mln 90 diiyS-t'l120"F I.SOo/.. RM

• f BO•F (B2"C)

0 'JtHI!lp Mal<im.Jm 1/./{.1'.)• l..:•'l~ l."'' L(\<JC

.:tn:. ~in ; .: tr)

1 03 c.r>:l 'e' :-: £•:J C S:-! 1/71) 'IOJ c .. ?£ 9:;!4 I O!l n.=.;; '-'!'i\1

[1 99 r. [>3 13~0 :.J ~~ l:.t-t ·Jt·~O

,.:.,'vCfagc 1060

fl!li "'ir:u.-· 1~1 'l tlx mum •mo

A:>pzren: She3r Type<)! i\1'"rvl.IU

s t·crg:t; t=-ajli;•(.~ 01 Faih..!t>

:ps ; (~- ~~-/ N,

15!!0 Adhesin'l t\'l mer,11 ".10 ?/~0 AJ":hF.;.i::>'l t9 met~! ·rll) 'I FJ•] /\Cil.:OS•C·' I 1(1 1.-u~l!ll 9C 17>1•1 4o l l\~,.,i:~\ r., m~~>~.:.~l <lr. ?65(J Ad 1ni:; 1 to m~Sl'll ~0 'W'IU /\t.: ' IL'.$1:.;·~· to IIIC I.>!I 90

199(t

1>60 2650

h+l'-'' lt' .. ;>,j , li<'> r~:".ai·U'-:11JY <lll lo'J'1 '·V<'i'-'P t'llifh 4t " i,~,t:\' !vr lilio io•f'•,o;;,·.~ "'"' :::( !.14-t'i~~>7> ly•~I ·>J11 11 ..... / ,..-., ~(J>Io~i,:.ol. I~J'"'~o;)l~ .. lif;o.•'l) ~•-'•IT 1¥\l't,< d ij V o•l ~ ~- lfU,:.· ;~r~ f'l;,<~loc To>tl\'oitiM.JI l.ol)'ot~l.llti~ , ,...,~.;\ p~tll~!ll.;o.:IA>I'Ptll ol~ ~ii'!'<'•W)' ;~~o!h()( ,a:l ill , ,.;-;;,-!1· ~~" ""'~ ~'It\ tl>.,lll'tl.ol(.P) f':r ~' 1() :t c )fl'-'iil '. "'i'h•:i<!l>. I~IYI ,nl• , ,. ·"('"-~'<>-• '"•Ill'~. ~~ ~,,.;,.l!li o;1 ••••"'!"1,:.~: t<~N ~~ ... ul)l ·~li:<l$f· :.' ;, tll· ... ~i\"" r: 1 •,!•~ <J• • .ol'! h< l lfi~ltlito\1 >'If ;,' (loltoo "(l~ll>ti;i\<., 1"1~,11,1} l;t (ll~(-~. Tit" 11 ~1)\llt~ t>! ll!l'-'''~1: :>~11(<. r,...,'l"ll()f•\W . olllf) '.l; v,l\i:; •N \ 1'> f""to;." H) 'II'IV! Pi" M'l~l>t .. :J iflllll :1* lrMII~tl Ul fltl> -'lfl'lt.J,•" Qf oc4'c:irlc'r;rt'.~tn l).l)t 11>1 s....:·'l ~e.-.!UlS :.nd l'l:ll lntlu.~ .n/ 'l»-r..:q~lll':l~l Mr\\~1'-

SO Peall S1Jet:t. Plt:~k>~ I~AO,lGI i'~er.c". ·;L13) 4!1' 00&3 F3>c 459 2»9

t~s::llwwYA¢!1.<ioim



Appendix 4B: Strength Properties of Double Lap Shear Adhesive Joints

\

lntertek

'Test '•,1etho:t Po;:fet~ Nu'Tll":i!r Ct..,itOmer A1!~·1t1011 AMPjSi

Dot•

it<SlU .Sp,e\.:ufll.m 'I yp:.; A:Jb:!~i\1t.> Su;:.st·:t:e ·3;; ·di..,!J CondifiO'"I!'o Snt"''fle ~~11t<Jn·rls_ Tf:':;l G~(!dMOil$

C;;::~>si·~&:J Sp~cl..:

$in··ifir.~,c.F.-

s~nlpte: \ I<:! Ill(;)

P·1A04.0LS.001 .FEI'I P1404.0lS.002.FEN P14Goi.OlS.003.FEN" P14G4.0lS.004.FE~

P1404.0lS.OOS.FEI'I P1:404 .0tS.OOS.FE~' P1404.0lS.007 .FEN. P1<104.0l S.OOM.FEN: P14DA.OlS.OGS.FE!i

f11l~~inh.:.m (1,1 ni .... ,U""' AV(;f~lg(;

Sid. ();:-:,· 'C.O V (#.;

SltC' I!:II~ ' !-l((l(X:I ~OS ;_: i UC:Uble. l 'ill}tjh'Ctlr tl),j')C~ :.,:e , l),!llS·b::· I CMOr' Lo~e1ng ASTM 0 '352S-,9a • .. RaapiLW;.!:J ~~iOO: _,,013.4!i{)2 nfoSciT &X C<~rr-·c~f!:ion

(;;lr'lC"·A "'ll F CIT<::trtl :; (~1t1r

~~t:F.'Yibe( ~. ?t l~

6~etii1 GJ [\

Uulu·:.:vn :41i •• miiU'YI Sr,:."l(j~c: ~'/ (: Jsr:-:r· ?!r Nor-e zrt: ± 2101..:,' 5o·;i ± 1C.% .:q +J. JC· n /111 f1

.4Sn.ll O~!i/.ft ;o;r.~d'i~;o. tr r~ ; r:IJ"" P.l"!;o.,ir,ns l:';e ...,e;..~sJ. r£-j td th\? n~:m:!,t .::1:0 ' In• :;nd t!f~1 1Ql=l~ -3.11\1 ~~fF.:=~ b~ Mr.~rF.<'I t.,., ~ !'.if:tt!k~m ii~ ,,~~

Towl A\•e:roge /¢hCSI'Ie' Soecunen I$OOC Maldn~um Uttuuate fyoeOf I!IC·<III:!i>s '••\'c<.llh OvGr~p Log~,; SL· fl ' IQ!I' 1-- ~llu •·c

(i-(1 ('lj (f'l) : t') (PSI:·

"J t~S: :Hi& Q.:4 2029 ~ 9' C Achc.sic1 to merol ~ 'CO~·~ o.~1e :l'*'' _, Q;54 ·22:60 22.SC ,4chcsi'-''.l. to m~l.al ( 'lC!J1~ j,~2t; l 07 3.53 Z51V 244C AullcSiO'llQ JII..;k!l l 1CoJ1:S ~ C1fr ~07 :).5:) 2J.l0 220C A~hCS•V'llo mclal l ,PO% j.~21 3 oa 3.5:i 26l0 2:54C Au:lu~siv·llo .l'llelc!l l 1CoJ% J&2C 3_ 02 J.S>S 2'.30 210C /\CilC:)Il.''l iO IIIP;UJI : i t,;r)';')

J.C21 JC9& J.54 27130 256C A6 hcil1V'llo mClcll r '10(1% :l..C2-t 3 98 ·J.M 2050 ' DIIC Adhesiti'l to m~tal l HiU'i} ':l:C1(! 1.98 1.5•1 3&::lC• ~3'"C Adhe'sic-1 to meta,l ( ~OU%

, f.:>A 1 9< 3G5 ~Sfh1 3.3 13 J C1~ (1.9'2 J.>l 2020 1~1J M20 0,91i 0,54 2470 2lBO 0 C0::l :t.C2 J.c· .t.6S ~2

9 2 ·o 1e

!nt :>-;tl( "'-an;.::: ~1roo~ ,:;t<Q·,, tr.ll!i;rt:r.Q~~.~~r.l'-secr. ·« I !It :,o:~ve 11~r. ~f"lr!C ~ltr:s tc•,,til)-n t-.~ :~·~.J"Ojr~c·c. tioQnhto-.sfttl!""r:::~~rb :r J~~of tllt l'll~ck "i''~(ln leth,,l:qJ ~bo·~ttfi::!-n:,rv.. ls cc<mltt-::d !.:c«ie¢.n ~~~ri•:.:'!Jii»ll!~ IIIW'n lrSJ. ~"' :.'lc rca~.1·wrr ct";V to11;.e ~~~~:de rn;rt-:-.·l~l'i. crcidJ:C « oro:~u :e...,ec, :u~riret ~~ s~r.~r.·o ;,,~_ ;u-:- ro: -,~::o:s:rf 'J irdl::.tl·.~ e.' :1:<:· ."!'-=" :!c·~ !c<ril!CJI 'Or ~·,11:.4 'I):IICII:Ib, cr:c .... ~ ::r :lu:e:cs. I 'It h~ollll't ~ !fltY:ck ".:rt!::l f«'Ofloo;b' ~:l:o·.:~a-lc~ 'N~I: r~ t -:1 ~.,.<·~ ,,~-.~~fr!.:c:l s:~all ~c ll'l!lt«<11) :~;: .:l~rW'lt oi (Cr-,l~r:rto., ~~~to· ~'-<1 s~ 'V!~S :.no IY.It 1!1(111~ ~·rr, oo~~chl~l ~'"l)~u.

::.1) ~:.11 ~-ue~ l',t",sf~!d. 1/AO':il.ll l' ,~r('( .;.qS) 4~!HiS'!;.;; 1•:10: <1\1\h~JP.

ht~:·lv<\w ... VL!!.to"'



lntertek

I~Lr· .. lr.:thod Pn;-:c. 1\un t:ot Gu.tomer At:.;ruif>rr A.n·~ •i31

o~•~

16sl d Sp~imen Tyf:~Adt\eS.i\•P. Subs.trmE: O:.rn.ia r1~ Coudlhl:'\s Si:lr:;ple C:.:r :n on ng Test Condi;ions Cr:.::osl-?.~:1 So~d SirJr ifi:;;;"'r.o:

.So'i"ip'e Nc)lll<:'

P1M!4.0LS.001.1 17 P1404.DLS.Q02.117 P140d.,OLS.003.117 P1404.DLs·.oo•.1 17 P1404.0LS.OOS. 117 p,~04.DLS.OIJ~.117 p,JJ)4.DLS.007 .117 P1404.DLS.OO.H •17 P1404iDLS.GO!l 1 17

Ml:llo:mt.m M t~ir-w··

Av.e.~ne Std. r:ev

C,O,V f t :

She"'~ it Pr~tJE'rlte~ ;1~ De Jb~- Lap She:ar-. .;,:hE::: '~)~ :1:> nts t:~· T\"\n ':' -nr 1 o~r:inr,-

t\STM D352.i3 9S .:Reappro· ... -e~ :?308:: r 2'JIJlSCZ ufoScile-1< Coro::·3:ion C~r·fP.·A ... ~n Ferr~ira

Pu,~hase Orc:r #. "" S17 .. -5

l C5rtF.' 1~r:f.-!TII~r -{>, 20' :l

A ~J"'kl"\~'1/'";

. .:..lu'Ylii"u .... 3t" ldCU ';)y c•.tSklltl~f

No:Jtl~ za··c :t 2"G ' 5C·~::: :t 1c~v, ~H U.~G "'im n ;..s:-M O:l!i?S ~·r.e::i·l"f.-;o. 1r :~ r :iin::r5i~'ls t:e 'l'le-,'l~t. r.:..i t,; the 'lf.,:u~M S.:t'- .n 3.1'1+7 t~'1:.1: INIC -~nl<l s.t·e·ss- be re~oned to 3 siQOiir.-3ol: tig.:retr.

Tr;.t,,l A•JF.' Rfi!'.

/~c ... es•·te Soeci"'(iM ~OM f\11SX'irrtJm Ultimate T·ipeOf I I IICk·l~& ','1/h.:l•t U1Je1lup LOOC SL•:::t' f:l !h !--el MO

;,il') (nj (I ... ) ( "'! (PSI:

3 0?1 ·J.9G a. 54 25'0 2~80 .4c:n~;o.i::: -. to metal/ ' !!0"/ \) (!2~ ·J.9B ·:),~4 ;-ago znn AM~;o.ir:·· to mE:otal : · f:O~i 0.02~ .;).;)7 3.54 37.SO 3590 Ac hesio P, to metal : · 0~·%.

(I 02'7 ().9'1 o1.5~, 2050 2770 Ache;o,ic .. to me-tal : • 00% .;) 0?1 ·194 ·:l. !'i~ ::'3:)0 n ,.n Al'iht;;o,i::p to !Yit":t.al : 201• (! ~2Q ·3.~& 0 ~4 3o)3() 2~6C h ! I'IF;:OiC1 to MF.:.tll•' ' 0()% ·3.~21 ~.06 •J.S2 2.'1(.\ :::r ;.: AfJriCSIC''\ 10 met.aJ l ,.-UO'Y: 3.:1~5 ).97 •J.52 21'52(+ ~~oc AUJtt::>SI:.!'' to ~~~~lei) / ~110'>! J ::l~f: ::).~5 ·:l G~ 2};,12(• ~-s · t: . .;i!h"'r>i:n to .mf:ta) I \ OOo/

'!) :)2'7 :19f; {tii4 375\J ~~~1 3 :l:>f: () f:IJ {) !'t? nne! 1-X!~ 0.02;5 M1 Q.S3 <.860 ~780 :.u::o3· "o· ( 1,;)' 3'9:.i 34~

' I "' •• n

lr\,cr:d: ".::(i'.s t:,·ro~·;y l;;b:lf~~oiu11:~r.s -:<\"-ll>W'!C~~·· t!•"" ~>1:1 Jif"ll ~--:~ e-' tnrclo:rils t.:~ ·..:h:.m t·lr(~l! «<:lie~~ r,oQI/n:t.,flSfr«"" •'"'IIIJi'b ...- '-'>"'o r •J·~ \"'·"'·•!o:., Pi.:'\o ;,_, l~oJ··o:;li."::J t<1V11-6'~'"'h .,,..,.~ • 1-'<:f•rf;t,..:.l l!.l.t<:\ll<" ,•rr,..>ol;o -:o.t~•\;l•t.W 0') "'''''''.J· ''tlt·~ 11\!•.lf\"Vo:o'h"<~fl.\1)~ (~ ·'1 1<1 ' ' "' .,.,,..,:r • . ... .,lt<'' .;l\o , ~·· ·J .... T,, •,. :;;u .:o·o!)...- lhl-:\l ('>..;•f"\•~1 ~,...,.,. .. ,,.,~IJ ., •• .-!"I'", l,ol l•io: o!-~1 ~ ··'!lj;;~ .,,.. (>! 11- ,,, .., ''"' 11fH•I ,.,, \1) ,.;.-.;,;•~·· ,.,.Ill'"'''"'" ,:.1)/'J·''"~ M i""'"''""· n,. .. ""''"i• ~ .,! ~,, .,. , : .. •. N~' '" .,..~ ,.,,,.l(fo;~· , ...... .-: .. -;,.. w J , '"''\1,., "·' ,, P ... ;. .,. II',.'"~' ""'' ,_. . .,,, •~oo ~; ... .,. ... , ••· 11 .. "'" ... ((11 '-'' 10'\;'Wf~\!ln ~lOr~:!> ~M.!fC.~ 11r1l 'I~J IMII ..:J) ~)'a"oM;Io.1!.(r.lfo)l l) ~'l'lo)(lo>;.

'iO 'Nioll "''"'"'· "'11<11~1:1,. ~~~ )l1f..! Nlllh.>: :•tll;tl.i(I~OORl .:ilf..A:I!I .JU'l

~pci.\•,w-..._,(lt!. ,oo'¥'1



lntertek

T~st Me:hvd ProjF.~NLmP.P.r C.J·~·:lJ1·~r

AltE!n;ion 1\n~ly!.t uato

-~st ID S!X:OIIl'Cr r9P·o. /1Q"'CS.v6 SliOl>UiHC Bc\i:.J uy (;ondi~h.': l:;

S2 ..... 1=e Cc ... .,c-·b::!n ns --~s: -~:-~r,iti1iPns

'~rcss1ea" Sp~c Sl!}lllt(;<:)II(;C

Sq.n1p1e "l,:nue

P1 .. 04.0LS.010.rEN-Pi404.DLS.011.FEN P1404.DLS.01UEN P1<1H.DlS.on.FEN P1404.DLS.014.FEN F 1 '10<\.Dl.S.O'I:O.FE~ P1404.DLS.Ot6.FEN P1404.DLS.017.FErl P14o •. Dl.S.01G.FEN

r ... Jaxirn Jrn ~.' in' •·•\Um A·;e~.:t!1:'!

St<l De\· c.::rv. <-~;

.St!engl.h Pr.ope.riieo& of DoUble Up Shea( Ad,hesive Joint-51\y le.nsion Loading AS-r,.1 03529-~!l- .( .R.ec:ppr~-\·ed 23C.S) f"20 1 3;4 502 !nfoS..-:iT E-ll' C::.r::~::-• li :i~n

C:~rit:··A ' " :=~rreir-~ F·~r·l-: rc)· Jan.1~'Y ~~ ;w14

:W da9'& a't 90"F 95''.~ fUI {\

,J..h1k<"'t(;'li""l t \ll.lll,I"11J'11

13VIICY:(: :J'j C.liil;.ir~·- .:1

N~IH! 7.~''\. t,1"C.: flO~( i' ·1t·~i: R -1 O.J~ tr;!m n '"'$ 1M U:J52~ ~jX:C1 '1CS TB:-d ll"'jt'St61$ b.O. · f1~1$U';.;(.:. 10 l 'lOOC<:tfO!.I 0 .:.'11 ll .and t;,ot lo;:~d .:~wJ stu~ss b;o I'E?POltl:d to 3 .si;pi:icau: liiJ'.I..res.

l ot.:~) "~~: .. er~9e Aolli';S.I·Je S:oecm..;n Oono M3l(llll .,Jiil Uttlflla.le J•,·pcOI 'Jruc<oe3;s V/IC; lil .Cv'<; il<ljl) LOOO St·et'g'.n 1 o tur~

(10) !r•l (1",) i o0 ( ->~IJ

J .C22 J.Q· •:Y.ri(Y 1·73C· 1 5~~ Adii.ES1:lr" io 'YIE':if..l f' VJN;,

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J.CZC J.O!' 3.54 t710 'G~O NJ·I~•::w to ' HOk.ii / 1-JC% ·:,) 1.:21 3.90 J.Sl'' i620 'ilOO l':o,.!.I'ICS.t(lr !0 '\ JC!.:"'ll / 1 JC% :.JX2t: :.U.J8 ~.53 2'f.IC• 21'(! Ad'lCSI~I' :0 ... 1<.'tt1l / 1-;)1,;·;4

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n 'j '10 c ·' ,,

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SO ~'rl Sl.<o:t~. l'il!~li"'li tf.'\ \1~)1) 1 ~lrY<o':': i'll )l·W.I~)S.3.) ~~.,. <i99·H3l'

l •l~l:<l·'"''' .. ' ;ol ~ ..........



lntertek

r ~LI11Klll'o:1 P1:;j:~;t;t Nur l::(:>!

Cu~tomer Attec"ttisr ,f.\ne~y$~

Date

'TIF.;tiD S:"'if'\C m~n Tfp~· Adh~siw~·

tl .IOO!i"tllC Bondiq~ Conc~t'J'r•,SS.,molr;- C:,ir.di:\t·n,ij"g T e:;.t Conciti~ '"'S Crossl'le~d $pee~l

:Sgn ICll/'Oe

$al""ple NOs 1 \ 1~

PI404,0L$,010,117 P1404,0L3.011,11V P1404,DLS.D11... 11V P,404,DL$.013, 1 1:: P1404.01.$.0t4.1 l'1 r 1-to'i,tii.&.OfO,I lT P1404,DL3.016,117 P1404.0LS.011.117 PI004,0I.SMB.117

\~.;xi-u-.

r ... lirim.lrn Aver·;;.~e-S':d. De•J cov :'%;

$trength Propenies of'Double.Lap Shear AdhesiV~ Joint$ hY lenslof! t.o~dlng AS;~ M U3t-28-~ tR6.:l0~'9V00 29U8:• F2C1~6.02' ln~oR..-Ti'!-.: r.orr:,,mri:-:,. Ca.me-...v ... r e·reJroF•~ul :t ~w .Jonuauy :?9. 2·cv

JO <IA)i.$.1J~O·r.- llSo/. RH A UnkOo)'\~li A u'fr' lfl ,il l'!

Bon.:.JE:\1 t-·~· :;ust~Jrne• None "2~C -?'C/;)rJ%-13% Rta c ()5 il'/ """lil' t .. t 1 \1 D:3t:20 toetf~s IMt orme.ns,ons be fll~;}s,1reo {0 \he neo:ve.s: :.l 01 in 3 'V.I ·.rttll IC~t:J ;!nO S'IC.SS ~(: '0.('-C"LO::,j tC 2. ~ 911 1l fM~11 hQU'CS,

To:a AV<"!r~ge

i\<il'es;ve S!>e·cir:'er. 1301.' (1 ~axr""\um Ujj"'!a:e- lypeO' il'";;;kn:~:i 1.:.f.d\ll OV~Z·· laO j_{ljij SbCI'1eL·'1 ::a~qw

(in ~ i jn) <in: !'ib.t: \PSI)

f. l)?Ei c '-)g f:.£),:1 ~~!:1 :.·M6 ...:..~1'1-esivn ~~meta } 1W% P01~ C\1? I}' ~ ?£73 ?~0 -A\Jh.esio.lll:.: 11~et3 111Xl'}<,. t ·.01·1 o~-g C.b~ l9~3 18-10 AdJ';esJcm t:: m~tal l 1lXI% C·.~·ns: f)J.•Ji c &1 31~~ 3"10 A.d)1esicm t:: metal I IC\J% t:.Ut-1 C97 C.£)(. 2.'163 2~0 'MJ;esi<1n t.c met.:&,! I ICQ% C':· (J' I ()·~.·l'i C: \(14 ?'(15:1 Z;1.:1\", .:....th~l'iiuu ~(.; ll l<"li~J \' IC\1.,Ji,

r.m~ C §S c >2 2533 1480 .fl.\lhe.sion to metal i 1C~% t.O~~ C.9~ c.~:s ~t.O:J 2·3'10 A'.lll.::.s:,on lt~ nwtal ' 16:.1% C.023 C.'t-U C.63 26 ' J 2610 Adll~S!Oil I::: mCI~l ,• 1(iJ'·~:il

M28 C,Q9 Ck..L 3193 ;;nc 0019 C.9!i (i 52 '93~ iR4C 0.024 O.S8 · O.S~ 2S10 2420 0 (IC3 C•,01 C· •:•1 3:'JQ ~'e

•13 1 ? 13 14

U:;'\d 2.fC.a C9'>StJI~\lCI' :r~:Y.liJ Oil ::IGSI r:.f'Oil' !l1f.:la$.1! C.'Inl')~) !. C·I IX:r·:J Ui,mel\~10'11$.

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.9'.1 ~·! Slo·o:~~. tllb'\~11!, ~.1,\ ~IIJC ~ N•)•·l~: W):· d~'""',IO} r.,, .. f!l'l·1l3' ..... a,,,., ...... , •• Jl!ffi



Appendix 4C: Climbing Drum Peel for Adhesives

lntertek

T-es:iq : Climbing Oruro PHI t"ot Adh_esive~

Tes: f••l.ef">Qr: PI OJc-:;t N ~fll :)C' :":!ll>::;'"'"tF..' AUef! l'Oil Ar;'>! '!'!'>t

· t-.s-!,•1 01781 · M -:·R~31'flf•"'':ed '-'C1~) M~t;.IIJ!IIJ ~jJI....:IhlvlllvH{cllh !111/j ~>'Vvl <.li!S..iol.IIC'J.

. P2oJ1345C2 •nk1S.::iTF.X \.<'lro:::·a;ic;n .~ .. rc.~~'="~ Q!ri~r tt ·1317'16

J C"'te

: l:ar'iCMAf'•ll '-CIICirfl

: .J M'd~e~ :' <. Sci:Um~f1 · r:-e~C1"ll)er~3 201 :;.

I /161&'e/ <:1 Des~fi~Mr • ,;lwnil·up'f

Sampta-Oir-~ni::I"',S (ir) : 3 -l$ •J.5 .x 1' :nom,..,. ) OO'ld'OS Con<fi:ionS" ~(lt.S.uol>!ie;;l I f\~ l l~H)1Q I i"'o1Ck.f'¢SS ( "!) , 0.'):::_

So1lp!: P·cp:~r<:~lic•l . Ren::~d .ol n·-)jchru:•g pcrltw··.r:c 'j'f nte1tiH -:)TL

I Con<!i:ionira · U·r~enC t~nec -ast r.,.la:c ... in':! T:t'PE:' : l n~l·:.:r· .5G85 Br?.F.d Ct Te:.t:r:-r: ' Q in/;-in l 'tl! '·t~e ~'lCI Ius {•iJ · ?,!l l D•u·11 K:rt1US' ~ Ju; . ~.01

Cali:,.e.t ::r· \1o::>tho:J : A:J"!_c·cw:J -{lr\111~ Gr: ..... r.ens;:,ti!"J" :rt.:t; · 3R 1 Pu::l~•d .: (1;· .I : e.;:; 1 I T~s; c~"'l:ti ;jons : ?3"C:t·2 .. r. J 5C»· :! ! :)% RH

Sample 10

P14o.t.CDP.OO 1.FEN P1404.COP.002..FE/II F1404,COP.00l.FEN P14Q4.CDP.OOA.FE~

P1<04.CDP.OOS.fEN P1404.CDP.OOO.FEN P1404.CDP.007.FEN P14M.CDP.OOB.FEN P1404.COP.C09,FEN ti

AverorJP. Puc( Le-ad iiVf)

7() ~

i::iS.1 l3~.'6 n~ ij0,3 86.3 8~.:1 S9J /2.4

M"XIT!li,...

POOl _:;:aj

!:llif;

Ft"f> /" Uti.:> n . t, ' •105 !32.2.. 12G tt: ~ ~~})

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~? 0 i'51~ 5"7 .~

61 ~~ .'3 f 57 4 7<. 2 ~: 62 0

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3 (J

J .O 2..•J ~(J

3-.0 5.Q 3oJ ~.0 3.0

Average-Pee' Torque

(irt·lbfiin) of specimen

width

5S4 4.~0.

ll.oJC· ~ 7& 6.8S 4.(5·1 717 .~.4 1. !-J3C

~;30

i .2' ·

~ailure

T•t'pe

I ;1 ,. 1.4

•

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: lntertek

lc.Si tt~ T~;:.t Melh,Oj

P·;;Jer.:t 1\ LJrr iJ~..>! r-:u~tomer A~t-1liCA

A_,·a,}·~

0~<1e

S;,mple I 'J_

P140..COP.01i1.117 P1.404.COP..OOZ.., 17 PfdQ.l.COP .OD3., 11

Pr.el Rt':S,slar;ce Re-oc' l ? acF. 2 of ~

Climbing Orum E'eel for Ad.hasive& ASTM Q ~7Sl • 9fl (R~;:;pp(c,•e:1 2012:1 • tvhXJII!;J:l S~IC!rT121' ~r·;~;h , !)3~1 d!EIC!'\~ and no.mbst ot spe-:.inlell~ P~3'34502

l .,f~S.ciTe)( ~-:::•porntnn Co·nc-t\nr. 1 ~:'(C ·o D. ·._~kJ~e:b: : K Sc-.u·n ao

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1 &?.:i :2 ::;.t .:_!

3 55 c.

r ... l~-~i.ml:,m

1-'&i!l W:.a;l (lot:•

• fl2 tt6.U 7 1.2"

't = (;ui 'C$r,•c la!h .• rc 'I; lr•iu tho ~JhL'.Siv·u 2=- Ad'lesio-- to 1h e 'sc "9 l- Aoi"lF,Si::•· to t1F. r.r,•f: 4- r .6rl ... rc ··•·ll'l•r rr;:;:-s;~-o

AvEcage Peel Mn!n·uw TatQIJO

I-' CCI .;)j.ll>:,;llll~l l ~ in-lbf(in~

'-""' Vt!i~:l" of spe-cimen (I of) ( ll,: width

>W.:J ,~ 3.S'! 5'5 3.3 2.5.5 5' .-1 :..!1 2.713

i\vom~.-.; 3 .13 .s:c. De•l. ;)('.;

F.aii Jre Type

'.4 ' 1,~

-..

r>Wrtck l'ln-:lt~ !t:tt"n,l : t>: ub~1:rto1u -..:p)r:~.:. -c ''""'~*" tli( -I!»:·J.';Jfl! ~ost: ~~ ~ der:~ to ·.~~o'!l tm-J:Jfi: Jc!d~~eli. tle,c·~·~;·om •Cp?r:~ -t•· \t~ ·;; •toe r":~·~" l'lf>1!Q leo!>!lt~O.:O:Ii~1~YJt:<~<Jti,;:·~ "''fle \ p\''nr•tld i:~n tJII:.I~~I)'41.11~'J' z~::l i'IW' : or!( • • etku, ·t:l 1-:I'J::'rl: llj:O':f 'J '!h' :~o~lhe ~, .. , ,,;, ,.,~:.o!• ...:,, :.o·to:Jy~:, .,. ''";··~~ ·~~~\ ~,~,.;r"'-1 ~~ ,_.,.,,...,..:.;. •"\' ~~· ~ r ul 'it''.~,,;y -;....,ty~;.,.~ :.:+ l l•e <l"""ti~ i\le•dt'' v ~"'· 11r .-,Ye• .o ~ :,oio.,,h.l\l• I)• 1\o«@\>'""- n . ., /i,.l.~li•.,- follr .;.o!tk f'~t);., -'l'l.'li'V~.J!W loW'"'·U"it> .,..;•J· •~f~; W ..er~·~,o:~ ' "'0\lto.,.:l >'''" :.0~ " till!•; I I) II"~ ,.,..,,,, .• "I

.!-<l,llli:IO:Of.ttll\f•!olHIIC\1 .; ~tJ:: ~$1~((~ .:OI'Il t'ltl io•I!•..CI,o ll•'o1 ,.,-..,....:,o.'<'\li~ll.'.;rvt ..,)li o

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1\:• (>llf\~o•o oiA~)IoO,fn'YI



lntertek

1c~1ng Clln1bing Of"U1n PC,~} I (Or AdhO$ivct T E;it MethC",:1 P'CJeCt N.ll.lf'ter C!J$\orner A!tenrb;

ABTM 0 ( 781 • 98 (R~;;ppuwe:1 201~j • Mr.diti~ ~':im~l! t<'!lfQth 1l1'1111l~l :irMrmr.F.--1-'::.Kl ' ~,4~(12

A13 \1$: Dole.

1 ·\I":.:S~i~~ Ct:·J.:o•o.Lo'n Carrie·Anr F-:rr.: ra. M flrody r K Scl·un$'1' ' Jai"UClly, 20 2J~-4

•• ~ .. dhi=!rt:mc- O?!~c(p:io~;~ AI•. 1m .,um Adll~rene··hlc-<.ne-ss ·:tn} ~ t:2 .Sam:>l!". J·m~nsions (•,) 3 :< 0 5 >: 11 (""':Joinal! Bonding Cc1d.t<1ns .N-~$.tpolied

Sa111:JI,; PH:!Pi:<1=:b9•! • F',::nC(fi <>l ·n~•.;hJr·in~ IJ~ir:.;·ule'J 1.: ~· l ·,h:fk·~> P'TL CMJ'I .t,::.n on~ · JO days: @ 90"f /96% RH 1 e~t Macll11e r;o1;e 1'1&tro1 598~ S:>ltetJ Of ''=li~i1·g • 1.1: f:·.:·nar. Fl~n!Je Rttoill.$ ·;ini ? !i'l D•• •. m Hedi•.!S Jll~ 2.t:1 (';;; (t:r.;Jiic:"' MF.-11-~() · Ar.heril";n<:

1 or~ ~..c C.ompersa:ion (lj!j 3.8.1 r r l'l!pac. ~11-,f;. 60 (j 1.cst Conoaoors. 2~rc.!. ;t·c : t~O%.!. '10% !~ 1·1

A·lOfil~ :.:. Mc$(•fii L. I)I Mlnirl~.w-. Avera_go Peel

lotque i"c=!~i Pee Per;

Samplo;:ID NUil i o·er LMC LOOO P~l Sr.e~im~r:

looo '/+ildth 11•-lilflltl)

of sp e-cimen Fon.1r~ -,,pe

( b'') (' of) (!;,f) (ll} Wi(i111

1'14(14:COP.O:!ItF-f:N 1 4C,:: 41 :J "3!.UJ ~.c C.25C• P1.41fl.t.C:ITP.n:t9.ff' N 2 ~1 : 42 !1 &!8 3.:l C: 3Ql)

P140A,G'DP .QJO,FE.H ,; .;g,.[) 4C3 39 g ~.3 c -~Q·

P14a..t:O~ Jl31.FE."' 4 ~a.5 4Q . .1 36:~ 1.0 c : 3(o P to!l04..CO~ .031.FEN 5 ~.7.0 :!-13:::1 34.B 3.0 -0'. l~C P 1.W4.COF .on,Ft;N 6 :ltd nch(S<iCH ln.li ~J)flciiTe;l P•~~~c.:J ir o~&~ to obtair di:I<C: P1404.C·OP.O.lO,FEN s~.ti :).7.6 :'JS.S 3.0 -J.340 Pi~.COP.!US.fEN s ~9 3 ~S.5 35.1 3.0 -:l f:7!:' P1404.COP .O.lS.FE:N 9 3S Z 39 s ;jf:3 ~~.;; .:, cue·

;..v""rao~ 0.039 S:d. Ut:v c 2.36

lnt~~t~;>I;)~>:S l<'~ti\C<O>;I';'~l~tfut~lk$ l ~c:t~rtl ,:lr.:-'n :JM lo! :ho~C,X :It.~M:•ux ¢'1 "1\;r.c,m"kl · ... fi:'\M h.~{"iii:'UI~Iil:So>f; kt>'t ·•!'\I:OT f">'\~ lr:!i! INI:'\111 :1 ~~~·ottile 11tert:l·""'.:rto:s-:t':rro!, ll\• .:~tcrm?'r e~ I!Jtrr. U"e>!-'rn!l:to e~:tat :.1 t~otu•, ~ Jt,~rill\ll lr w1111r;g. ~..en~"'llflr. rr.t~utr.;\'rw;; !.rovi., :t (' s:l!:lfe.lll:rtcllals,· &:r:e>J:t t:: ~A:st~ t :1:t:t. urt~!~d·o: ur.1:~oed a'r,-3 :,l't Mt r.ttcmm, ,;,lr;l\'•;t ot ttr. !!·~ :1c~ lr.<"'l'lt'ul ;I• :l'l'!lo,t.· 'l'l~c·rl:~l\. cr~co.~s ;,r .,.,:t.t:es. 1"~~ l>!',·rlrt<t ' f -.tert~<. Pl~·rna INtf'l,lew. t..:l>:f1:1to•e~ wllf:l r'tl,t::t tt \~"JI:::$ r~11ec1en ~1'::111 tc llmlt.:d TQ :l'c :.11•r .... w of ~~Ytii:<l'flllO'o P:litJII.)·l\<11'1 .:-vi: otf<l'rJ rQI 'Y.! J~i' .,.,. :;;utllv~·rt« ·:1~/lll:llie\.

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2

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lntertek

Climbing Drum Peel for Adl'\e-sives Test 1G T~tMalht;'J

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Appendix 5: List of Scientific/Technical Publications

1. C.-A.M. Ferreira, M.M. Reed, J.W. Belcher, M. Cushman (2012, March). Shelf-Stable Epoxy Resin Adhesive. Paper presented at SAMPE Tech 2012, North Charleston, SC.

Documents

FINAL REPORT - DTIC · 2015. 11. 5. · FINAL REPORT Shelf Stable Epoxy Repair Adhesive SERDP Project WP-1763 FEBRUARY 2015 . Michael Cushman . Infoscitex Corporation . Distribution