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TECHNICAL REPORT

EUSTOMXRIC INSULATION FCR SOLID PROPELIANT

ROCKET MOTORS

By

D. H. Sale

" Departent of the Army Project No. IO124401A

AMC Code No.- 5025.11.8 4 2 03

Report No. 64-3158 Copy No. .

EL 1-9-100-2 Date 27 October 1964

DISTRIBUTED BY THE rHIS REPORT MAY BE DESTROYED WHEN

OFFICE OF TECHNICAL SERVICES NO LONGER REQUIRED FOR REFERENCE

U. S. DEPARTMENT OF COMMER(CE

WASHINGTON 25. D. C.

The findings in this report are not to be construted

as an official Departm-nt of the- Army poxsitIon.

"(kxpies Available at Office of Technical Ser' ices S . 75

Repcrt No, 64-3158

Copy No.

ELASTOMERIC INSULATION FOR SOLID PROPELLANTROCKET MOTORS

By

D. H. Sale

Apprcved by:

A. C. HANSONLaboratory Dlrector

27 October 1964

DA Projecý Nc. 1CO-24401-All0

AMC Code Nn. 5025 11.84203

Rock IslaDd ArsenalRock Islandd !lltnois

DDC AvaIlabilltv Notice:

Quailfied requesters may obtaincopies of this report from DDC.

ABSTRACT

The development of flexible, elastomeric-based,solid propellant rocket motor case insulation is discussed.The effect on insulation properties of type of asbestos,of liquid versus solid elastomers and of methods of dis-persing fibrous compounding ingredients, are reported.

Oxyacetylene torch and static motor firing test datafor some of the better insulation materials developed,as well as for souie commercial materials, are presented.The torch test, the principle screening tool used in thisstudy, conforms to the test currently being standardizedby the Flame Ablation Test Group of Section III-L of ASTMCommittee D-20.

A material with 40 percent elongation, 1.34 gm/ccdensity, performance ind3x of 95 cm2 sec/gm and erosionrate of 2.0 mils/sec was the most promising insulationdeveloped. The material is a 55/45 butadiene/acrylo-nitrile compound containing phenol furfural resin, asbestosand oxyazoline wetting agent. It has been satisfactorilybonded to aluminum and to steel by conventional bondingagent. The thermal properties of this vulcanizate arenot affected by oven aging for one week at 700 C.

1 64-3158

RECOMMENDAT IONS

It is recommended that this project be discontinued.It is believed that the insulation materials developedduring the course of this investigation represent anadvancement in the state of the art and that furtherinves t lgations under the approaches outlined in this and

earlier work would result in only marginal improvements.

I-- is recommended that the oxyacetylent torch testeqipment be retained in a usable condition, in order thatpromising new commercial insulation materials might beevaluated and that cooperative work to further improve*his screening test might be conducted, if necessary

64-3158 ii

ELASTOMERIC INSULATION FOR SOLID PROPELLANTROCKET MOTORS

CONTENTS

Page No.

Object I

Inttroduction 1

Procedure 2

Results ard Discussion 4

Literature References 14

Appendix I 16

Appendix II 17

Distribut icn 18

iii 64-3158

ELASTOERIC INSULATION FOR SOLID PROPELLANTROCKET MOTORS

OBJECT

To develop improved, flexible, thermal case insulation

for solid propellant rocket motors.

INTRODUCTION

The need for flexfýl rocket motor case insulation nasbeen well established, Elastomers have played animportant role in meeting this need, as evidenced by themany types of elastomeric-based insulations which have beendeveloped for use in solid propellant missiles. The widespectrum of commercially available insulation ranges fromlightly filled rubbers with excellent flexibility butminimal ablation resistance, to highly loaded compoundswith little Alexlbility but outstanding resistance to thehigh temperatures and erosive gases found within rocketmotors.

Present day elastcmeric insulations are not consideredadequate for future neeas. especially needs related to theuse of end burning grains. It is anticipated that longerburning times at higher temperatures will necessitate morethermally resistant insulations and that higher internalpressures will require higher degrees of flexibility. Acontinuing need exists frr lighter weight materials,

I-, appears that maximum flexibility and resistance tothe environments within rocket motors are mutuallyexclusive properties. insofar as rubber-based insulationsare concerned, since tmprcvements in one property areattainable only It the expense of the other. Earlier workat this Arsenal, -8,9) as well as more recent studies, hasled to the development of r-'bber-based insulations havinga compromise In these two properties, namely, the highestdegree of ablative resistance which could be attainedtogether with flexibility which, when measured in terms ofelongation, amounts to 20 to 50 percent. Results of thesestudies have led to the following conclusions:

1. By far the cost effective filler combination forimparting ablation resistance to rubber vulcanizates is acombination of a phenolic resin and long fiber asbestos.

2. This filler combination is most effective in ahigh nitrile content, butadiene/acrylonitrile elastomer.Of the more than 400 combinations of elastomers, fillers

64-3158 1

and other compounding ingredients tested, none has led toa material having a better compromise between flexibilityand abltion resistance than that exhibited by the nitrile-phenolic resin-asbestos fiber system.

3. The degree of ablation resistance of this, or anyother asbestos-containing rubber compound, is directlyrelated to the fiber length of the asbestos in the finishedproduct.

These findings largely influenced the direction ofeffort described in this report. Minimum effort has beendevoted to seeking more effective combinations of rubberand fillers. Major emphasis has been placed on developingmeans for incorporating long fiber asbestos into rubber-resin matrices without significantly reducing fiber length.

PROCEDURE

Insulation resistance was determined with an oxy-acetylene torch test (Figure 1) using the conditons citedin Table I. The equipment and procedures duplicate thoseof the test currently in the final stages of standardizationby the Flame Ablation Test Group of Section III-L of ASTMCommittee D-20.

The effectiveness of candidate insulation materialswas meawured by two test criteria; (1) the temperaturerise on the back side of the specimen while the frontside was exposed to the oxyacetylene torch flame and (2)the time required for the flame to burn through thespecimen. These criteria are reported as performanceindices and erosion rates, respectively. The index,referred to as P 2 0 0 , is computed by dividing the time(seconds) required for the specimen back side to reach2000 C. by the original specimen thickness (centimeters)and by the specimen specific gravity The erosion rate,E, is computed by dividing the original specimen thickness(mils) by the burn through time. It should be noted thathigh values of P 2 0 0 and low values for E are indicative ofgood insulation properties. Unless otherwise noted, theperformance indices and erosion rates reported are theaverage of four test results

Rock Island Arsenal Laboratory has been an activemember of the aforementioned ASTM Test Group. The torchtest facility at this Laboratory was among those utilizedin a recent round robin. The round robin results showedan average variance among laboratories of less than ±5% foreacn of the Iwo test criteria. The Rock Island Arsenaltest facility produced results well within this variance.

2 64-3158

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TORCH TEST OPERATING CONDITIONS

Oxygen flow rate, standard cubic feet/hour (SCFH) 123Acetylene flow rate, SCFH 102Volume ratio oxygen to acetylene 1 2Impingement angle between flame and specimen, degrees 90Specimen size, inches 4 X 4 X 1/4Distance from torch tip to specimen, inches 3/4Method of determining moment of burn through Visual

Several materials which exhibited excellent resistanceto the torch test were evaluated (see Table VII) In staticmotor firings conducted b,, the AtlantIc Research Corporationand the Allegheny Ballistics Laboratory at their respectivetest facilities.

The major compounding ingredients for each materialtested may be found in the tables pertaining to thematerial. Curing systems are given in Appendix I. Testspecimens were compression molded in a four cavity mold.The liquid polymer-based ccmpounds were mixed in a twobladed sigma type mixer (Figure 2), with mi.xing armsoperating at differential speeds. All solid polymer-based compounds were mixed on a two roll rubber mill.Stress-strain properties were determined in accordancewith applicable ASTM(lO) procedures

RESULTS AND DISCUSSION

Previous evalua.cn( 9 ' of several types of inorganicand organic fibers had shown that asbestc3 was the mosteffective for imparting thermal resistance tc rubbervulcanizates Curren, studies were made to determine theeffect of the type cf asbestcs on the properties ofinsulation materials Amosile, crocadolite and chrysotileasbestos of approximately equal fiber length "major con-centration of fiber lengths. 3/4 to 1 inch long) wereevaluated in a nitrile r.ibber..phenol.c resin based compcuindChrysotile samples from three different suppllers wereincluded The results in Table II show that the threechrysotile-based vulcanizates differ from one anotherconsiderably, but that all three are superior to eitherthe amosite or crocidolite-based insulations. The supe-riority of chrysotile is attributed to its flexibility(both amosite and crocidolite are brittle and tend tosuffer fiber breakdown during compounding), higher specificheat and fusion temperature, lower density and higherpercent of bound water- Hereinafter, the word "Asbestos"

4 64-3158

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The problem of obtaining a uniform dispersion of longasbestos fibers in a rubber matrix while et the same time *

minimizing the reduction in fiber length was attacked *through the use of the following classes of materials:(1P wetting agents, to wet the asbestos fiber and thusfacilitate fiber dispersion; (2) plasticizers, to soften C+the rubber matrix; (3) liquid polymers, to reduce shearing 0forces which prevail when solid polymers are mixed; (4) 0

s lvents, to dissolve the unvulcanized rubber prior to the 0 soasbestos addition.

Evaluationsof wetting agents were made as shown in ( 0

Table 1I1. The wetting agents were added to the mixture Cjus# prior to the asbestos. Although most of the wetting W

agents tested were useful in dispersing the asbestos,not all improved insulation properties. However, oxyazoline#1. a heterocyclic cationic wetting agent, produced vul-canizates with excellent thermal properties. A compoundccntairning 30 PHR of this wetting agent produced a 25 percent

improvement In thermal properties and a 100 percent increasein elongation over the control material containing nowetting agent.

Oxyazoline #1 at 30 PHR concentration showed no evidence 2of migration after aging for 7 days in an air oven at 700 C. C,1Aged specimens when evaluated in the oxyacetylene torch 0."est. exhibited thermal properties equivalent to unagedcontrols. Insulation containing oxyazoline #1 has beenbonded to both aluminum and steel using a two part, roomtemperature curing, general purpose epoxy adhesive. Bondstrengths (tensile shear on one inch lap joints) greaterthan the tensile strength (1730 psi) of the insulationwere achieved.

Data for plasticized solid elastomer-resin-asbestosccmpounds and unplasticized control compounds are presentedin Table IV. Small amounts (5 and 15 PHR) of phosphateesters served to increase elongation but larger amountsdecreased elongation. None of the vulcanizates hadimproved thermal properties over the controls.

Liquid irgredients offer a means of compounding withIcv shear forces. Data for liquid elastomer-asbestosvl;canizates, as well as the appropriate controls basedon solid polymers, are given in Table V. The data revealedthe following results: vulcanizates based on liquidelastomers have better thermal properties, greater tensilestrength but shorter ultimate elongation than the controlsbased on solid polymers. The liquid elastomers consistedcf low molecular weight, short chain molecules which required

64-3158 7

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| polymers.

Further evaluation of liquid elastomers included the

addition of thermosetting resins (liquid and solid) asfillers. The resins used in this stuoy were all polarand enhanced the erosion resistance of NBR-based compounds,but they were too incompatible with the less-polar SBRto be effective. Because of the lack of non-polar resinsand the low elongations obtained with the liquid elastomers,work with SBR and NBR liquid elastomers was di3continuedo

The two carboxy modified polymers listed in Table Vwere vulcanized using an epoxy resin at a concentration of13 PHR as a curative. The low elongations obtained fromthese two compounds eliminated the need for investigatingthe effect of adding more resin.

The method of incorporating asbestos by adding it toa methyl ethyl ketone solution of the polymer and othercompounding ingredients proved unsuccessful. The asbestosin the resultant vulcanizates was non-uniformly dispersedin the rubber matrix after air and vacuum evaporation of thesolvent. These vulcanizates had properties inferior to theproperties of vulcanizates prepared by conventional millingprocedures.

Torch test data for several commercial insulationmaterials tested are presented in Appendix II. Of thesen-aterlals, one has properties comparable to the best

Rock Island Arsenal insulation, as shown in Table VI,

The work discussed he...in and work previously reported(8,9)has resulted in several excellent thermal insulation materials.The nine best of these, along with five poorer materialsand two commercial products, were evaluated in static motorfirings by Atlantic Research Corporation. Erosion rates,densities, elongations and major constituents for each arepresented in Table VII. The erosion rates from the staticfiring tests correlate reasonably well with the torchtest erosion rates, at least for the best five or six andthe poorest compounds. The erosion rates from the statictests cover a range of only 2.4 units, as compared to 10.4units for the torch test.

Unfortunately the insulation containing oxyazoline #1wetting agent was not included with the above materials.

64-3158 11

TABLE V I

EVALUATION DATA FOR THE BEST ROCK ISLAND ARSENALAND COMMERCIAL INSULATIONS

Property Measured Rcck Island Arsenal Commercial #I

P200- Cm2 sec/gm 95 79Time to backside 127 101

temperature of 2000C.for 1/4" specimen, sec.

E, mils/sec 2.0 2.0

Elongaticn, % 40 50Density, gm/cc 1.34 1.28

Major constituents Rubber, Resin, Rubber.Asbestos, Oxyazoline #1 Resin, Asbestos

However, this material was submitted to Allegheny BallisticsLaboratory for evaluation in their test facilities Theirdata indicates that it compares favorably yh materialsthey class as "current better materials."(11 t

12 64-3158

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LITERATURE REFERENCES

1. Batchelor, J. D. and Vasileff, N., "Solid PropellantRocket Motor Insulation," Conference on Behavior ofPlastics in Advanced Flight Vehicle Environments,WADD Technical Report 60-101, September 1960.

2. Dervy, A. J., "Reinforced Plastics of High Strength/Weight Ratio for Space Applications," Society of thePlastics Industry, Inc., 17th Anrual Techn.Lcal andManagement Conference, Reinforced Plastics Division,Chicago, Illinois; 6,7,8 February 1962.

3. Epstein, G., Cecka, A. M. and Robbins, D. L., "Plasticsin Rocket Nozzle Environments," Conference on Behaviorof Plastics in Advanced Flight Vehicle Env:!ronments,WADD Technical Report 60-101, September 1960.

4. Epstein, G. and Jaffe, E. H., "Materials for InternalTnermal Protection of Rocket Motor Cases. A State-of-the Art Survey," Society of the Plastics Industry, Inc.,17th Annual Technical and Management Conference,Reinforced Plastics Division, Chicago, Ill; 6,7,8February 1962.

5. Hazelrigg, W. K., "Design Criteria for InsulationMaterials " a paper presented to the Refractory MaterialWorking 6i-iup, Aerojet-General Corporation, Sacramento,Califcrnia, 14 July 1960.

6. Headrick, R. E., "Ablative Elastomeric InsulationMaterials," Directorate of Materials and Processes,Wright-Patterson Air Force Base, ASD-TDR-62-400,August 1962.

7. Sewell. J. J. and Kuno, J. K., "Aerospace Use of PlasticHardware and Thermal Insulation," Society of the PlasticsIndustry, Inc., 17th Annual Technical and ManagementConference, Reinforced Plastics Division, Chicago,Illinois; 6,7,8 February 1962.

8. Rack Island Arsenal Laboratory Report No. 61-2315,2 August 1961. "Evaluation of Flexible Insulation forSolid Propellant Rocket Motor Cases."

9. Rock Island Arsenal Laboratory Report No. 62-2366,6 July 1962, "Development of Flexible Insulation forSolid Propellant Rocket Motor Cases."

14 64-3158

10. American Society for Testing Materials, October 1961."*ASTM Standards on Rubber Products," 1916 Race Street,

Philadelphia, Pa.

il. Confidential Communication, Allegheny Ball.isticsLaboratory to Rock Island Arsenal, Subject:'Evaluation of Car didate Insulation Material"(U),25 June 1964.

64-3158 15

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24 64-3158

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