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14IND03 Strength-ABLE

Grant Agreement number 14IND03

Project short name Strength-ABLE

Project full title Metrology for length-scale engineering of materials

Version numbers of latest contracted Annex 1 and Annex 2 against which the assessment will be made

Annex 1: V1.0

Annex 2: V1.0

Technical Report (Progress) 1st 2nd 3rd 4th

Period covered (dates) From 01/12/2016 To 31/08/2017

For JRPs:

Project start date and duration: 1st June 2015, 36 MonthsJRP-Coordinator: Mark Gee, NPL Tel + 44 20 8943 6374 E-mail [email protected] website address: http://empir.npl.co.uk/strength-able/

Internal Funded Partners:

1 NPL, UK

2 BAM, Germany

3 CMI, Czech Republic

4 DFM, Denmark

5 INRIM, Italy

External Funded Partners:

6 Adama, Ireland

7 QMUL, UK

8 TUCh, Germany

9 UCov, UK

10 UKAEA, UK

11 UoL, UK

Unfunded Partners:

12 APT, Switzerland

13 ATOTECH, Germany

14 E6, UK

15 EMPA, Switzerland

16 FhG, Germany

17 MML, UK

18 PTB, Germany

Report Status: CO Confidential, only for members of the consortium (including EURAMET and the European Commission Services)

Technical Report (Progress) 1 of 17Issued: August 2017

TECHNICAL REPORT (PROGRESS)

http://empir.npl.co.uk/strength-able/


TABLE OF CONTENTS

1 Summary...................................................................................................................................32 Overview of progress towards the objectives of the project.....................................................33 Explanation of the work carried out...........................................................................................64 Deviations from Annex 1 (tasks not fully implemented), the consequences and proposed

corrective actions......................................................................................................................75 Ethical Issues (if applicable).....................................................................................................7

Technical Report (Progress) 2 of 17 Issued: September 2017


1 SummaryThis report covers the 3rd 9 months of the project (01 December 2016 – 30 August 2017).

The project is proceeding well and predominantly to plan. There are no organisation difficulties and the JRP-Partners are working well together.

Main achievements for the JRP Partners during this reporting period:

Excellent progress has been made in developing numerical modelling methods to enable length scale engineering of materials.

A third generation of single crystal diamond AFM probes for nano-indentation was produced by Adama targeting oblique cone angle with sharp apex and high spring constant. These probes are more comparable with the geometries of indenters generally used in nano-indentations and the high spring constant will allow a higher indenter force. These third generation probes have been validated in instrument indentation experiments on test samples.

A traceable MEMS-based instrumented indentation system has been manufactured and validation experiments have been carried out with the test system, showing that the test system operates well within the operating envelope expected for the test system.

Characterisation of all the test materials being used in the project has been carried out.

A major testing exercise across all length scales has been carried out with the results and data being assembled into a matrix database for further analysis.

2 Overview of progress towards the objectives of the project2.1 ObjectivesThe project addresses the following scientific and technical objectives:

1. Develop validated design rules for combining different size effects to optimise strength and toughness of materials and components over a range of temperatures. Develop a plasticity size effect algorithm for processing small scale test data maps to obtain material-only properties. This algorithm will be incorporated into an analysis programme to support materials property mapping (by indentation) of surfaces and small volumes of materials. The project will enable simultaneous calculation of multiple length-scale effects reduce the uncertainty in property and performance prediction by an order of magnitude (from factors of 2 or more to tens of percent).

2. Improve nano- to micro-scale property measurements by developing a MEMS-based instrumented indentation (IIT) system to bridge the length and force-scale (<1µm to ~10 µm, 1 µN to ~few hundred µN) between AFM and nanoindentation; developing better-defined-shape probes with lower uncertainty contact sizes; and improving AFM-based property measurements. The project will develop tips down to less than 10 nm in size with ~1 nm precision, and/or with high aspect ratio, exact shape and high repeatability. These tips will also be stronger (up to 100 GPa), cheaper (~1/10th of cost), better-defined-shape that will reduce the key uncertainty of tip contact area from ~50 % to ~10 %



3. Develop methods and associated uncertainty budgets to determine the length-scale dependence of the strength and toughness of materials vs. temperature. The methods will have sufficient resolution to distinguish between model predictions and will use:

o Characterization methods, such as for dimension of a particle, structure or layer, grain size, crystal orientation and crystal rotation, residual stress.

o High-resolution indentation and compression (vs. temperature) of surfaces, micro /nanostructures.

o Systematic quantitative variation or estimation of dislocation density.

The project will establish a new NMI capability in high temperature indentation, at temperatures up to 400 °C in air and at least 500 °C in vacuo with a reduction of uncertainties to 10 % in high T indentation modulus and hardness. In addition, the project will establish a new capability for high temperature, high spatial resolution (lateral <10 µm, depth ~10 nm), indentation creep measurement.

4. Develop and evaluate new measurement methods to distinguish between the contribution(s) to the total test response from test-related size effects (i.e. Indentation Size Effect) and that from size-related strength or plastic deformation properties of a particle, volume, or structure. In addition to conduct a feasibility study to determine the capability of the measurement methods to characterise and map difficult to measure properties such as material dislocation density and mobility, stacking fault energy and plastic deformation zone size

5. Support the competitiveness of EU industry by engaging with industries using manufacturing technologies and process control and by supporting the development of new, innovative products. This includes conducting case studies to facilitate the uptake of the technology and measurement infrastructure developed by the project; and by contributing to standardisation bodies.



2.2 Deliverables status and progress towards objectivesRelevant objective

Related WP number

Del. No.

Deliverable description

Partners (Lead in bold)

Delivery date as per Annex 1

Actual Delivery date

Status:inactive,on schedule,delayed to..., or completed & submitted to EURAMET

Progress towards objectives(one paragraph includes all partners)(max 250 words per deliverable)

1 WP1 D1 Validated design rules for combining different size effects to predict the strength of materials at a given temperature in the range 20 ºC to 500 ºC

UoL, NPL, QMUL, UKAEA, UCov

Jan 2018 (M32)

On schedule

Existing state of the art models addressing the different aspects of the plasticity size effect was selected by UoL, NPL, QMUL, UKAEA and UCov. UKAEA is working on CPFEM UMAT code development for strain gradient crystal plasticity. Design rules have been proposed and initial validation looks promising. Validation and calibration of material strengthening mechanisms to continue.

1 WP1 D2 User acceptance report for the analysis programme for materials property mapping analysis by indentation

UoL, NPL, QMUL, UCov, UKAEA

Nov 2017 (M30)

On schedule

The physics-based hardness law for the effect of the materials size effect on hardness proposed by UoL, NPL, QMUL, UCov and UKAEA, has been implemented as an analysis algorithm. This will continue to be developed and refined as more data becomes available. User acceptance report is in preparation.

2 WP2 D3 Test report describing new diamond-based probes for AFM with tip sizes down to less than 10 nm achieved with ~1 nm precision that are stronger (up to 100 GPa), cheaper (~1/10th of cost), with a better-defined-shape and uncertainty of tip contact area ~10 %

Adama May 2017 (M24)

Delayed to M30

Adama contribution: 3rd generation of high stiffness diamond AFM probes, and fused silica testing thereof. Testing carried out by ADA and COV in April 2017.

CMI contribution: Using 2nd generation Adama probes, CMI have performed AFM indentations and scans on various materials, and tried to determine cantilever stiffness with a nanoindenter.

The delays have been caused by issues with the development of the processing route and its control. However, as stated above 2nd generation probes have already been tested and proved to be effective and testing with the 3rd final generation probes has now started. No

Technical Report (Progress) - 5 of 17 - Issued: September 2017


knock-on effects are expected.

2 WP2 D4 ISO14577-2 compatible calibration and verification report for the MEMS-based IIT system that will bridge the length and force-scale (<1 μm to ~10 μm, 1 μN to ~few hundred μN) between AFM and nanoindentation

Adama, NPL, DFM, TUCh, PTB

May 2017 (M24)

Delayed to M30

COV, DFM, and BMI have receivedj MEMS nanindentation system and have assembled working system. Mechanical testing is underway at BMI with DFM (Oct.) The expertise of NPL was used to advise in the assembly of the test systems.

The final test system has been tested. Only the final verification of the system is now required. No knock-on effects are expected.

3 WP3 D5 User acceptance report containing ISO14577-2 compatible calibration and indirect verification for the high temperature IIT system at temperatures up to 400 °C in air and at least 500 °C in vacuo with a reduction of uncertainties to 10 % in high T indentation modulus and hardness. In addition, demonstrating capability for high temperature, high spatial resolution (lateral <10 μm, depth ~10 nm), indentation creep measurement.

NPL, UCov, BAM, MML, APT, EMPA

Nov 2017 (M30)

On schedule

NPL has purchased a new instrumented nano-indentation tester that is capable of testing at temperature above 700°C in vacuo. The system is currently being installed by MML and the deliverable completed on time.

EMPA has installed a new in situ nano-indentation test system running up to 700 °C and has demonstrated its capability with key tests.

Partners UCov, BAM, APT, MML and EMPA are supporting these activities through supply of their expertise.

3 WP3 D6 Documented contents BAM, all Jan 2018 On schedule BAM with support from all partners created a data matrix



and structure of the data matrix of material response as a function of length-scale and temperature

partners (M32) which incorporated their data in a logical and simple way; the next step will be to incorporate data from other partners into this data matrix.

4 WP4 D7 New test methods for indentation stress-strain curves and property mapping

QMUL, NPL, UCov, CMI, PTB, EMPA

Feb 2018 (M33)

On schedule

QMUL arranged a student taking an industrial replacement with UKAEA for one year (Oct2015-Aug2016). Indentation were carried out on single crystal and initial indentation stress-strain results were obtained using spherical indenters with different radii.

A second industrial placement student from QMUL has started at UKAEA. This student’s project is focused on the measurement and characterisation of pile-up surrounding the indenter tip as a function of strain and tip size. The data generated at UKAEA will feed into task WP1.1. UKAEA is working with NPL and UCov on the spherical indenter area function calibration, which is a key input for the data analysis of indenter stress-strain curves.

A methodology for separating test size-dependent properties from materials size-dependent properties (WP4.2) has been developed and is currently being evaluate.

Partners CMI, PTB and EMPA haven’t participated in this deliverable yet. Their role will become active at the next stages of the research.

5 WP5 D8 Report on industrial impact case studies

NPL, all partners

May 2018 (M36) On schedule

Progress is being made in several of the industrial case studies.

5 WP5 D9 Evidence of contributions to new or improved international standards; specifically focussing on the following standards

NPL, all partners

May 2018 (M36)

On schedule BAM, UCov attended the ISOTC164 annual meeting held in Tokyo September 2017. The preparation for the working item “ISO 14577 – Part 7: Instrumented indentation test at elevated temperature” is still on going. NPL and UCov also attended the CCM-WGH meeting held in conjunction with the ISO TC164 annual meetingOther partners have fed information into the standardisation



and committees: ISO14577, ISO\TR29381, ISO/TC164, VAMAS TWA22, CCM-WGH, and examples of early uptake of project outputs by end-users

process through discussion at project and other meetings to develop a common approach to standardisation..

n/a WP6 D10 Delivery of all technical and financial reporting documents as required by EURAMET

NPL, all partners

May 2018 (M36) + 60 days

On schedule

The publishable summary was submitted by NPL with support from all partners. The progress report and impact report were submitted together with this report.



2.3 Summary of exploitable results and an explanation about how they can/will be exploited

There are many benefits from this project which are expected to lead to strong impact in the next five years. These include:

The provision of new materials modelling capability to achieve the benefits inherent through length scale engineering to enable better products to be designed more cost effectively.

The abiltiy to validate the improved performance of materials through length scale engineering by use of new measurement analysis methods which separate machine affects from true material responses.

The development of a new MEMS based meso-scale mechanical testing system filling in a market gap between AFM based machanical testing and nanoindentation.

The ability of research institute partners to provide better measurements to their customer base who in turn will gain new confidence in the performance of their products.

The ability of the two instrument manufacturers in the consortium to provide improved test systems to their customers.

Case studies within the project on real production materials will demonstrate these benefits in real terms to these partners and their customers.

The participants in the case studies receive immediate benefit from the characterisation of their products. In addition the partners are working with a company to develop a new high pressure automotive manifold using additive manufacturing methods to obtain a controlled microstructure whose performance will be tested using the methods developed in the project. The benefits will be to reduce the number of components used to make the manifold to a single piece, reducing complexity and risk of failure; reducing weight, with comperable strength, and by using a metal rather than an alloy, increasing the recyclability of the component at end of life. This manufacturing process will have benefits beyond the automotive industry.

The successful development of new MEMS based indenter has been taken forward by the University of Chemnitz. Adama are developing improved diamond AFM tips to support this instrument which will be more resistant to damage and allow increased loading. Adama will benefit from increased sales and AFM users from benefit from a reduction in the main uncertainty in AFM indentation (tip shape and contact size) and significantly increase the maximum hardness of materials that can be tested.

The development of new high temperature nanoindenter test procedures at NPL will open a new area of research to the indentation world and provide data to materials developers for high temperature processes. Standards for the characterisation of materials at high temperature by nanoindentation will be developed in follow on work.

A workshop is planned was held in the third quarter of 2017 to provide more opportunity to work with industry.

The standardisation work will be continued

Technical Report (Progress) 9 of 17 Issued: August 2017


3 Explanation of the work carried outTask number & title

Task end date as per Annex 1

Actual task completion date

Status:inactive,on schedule,delayed to..., or completed

Explanation of the work carried out in each task

Summarise the highlights and progress towards completing each task

Explain any issues affecting the completion of the tasks (eg describe the cause of delays / deviations etc. and any knock-on effects)(max 300 words per task)

Task 1.1: Validated design rules for combining size effects

M32Jan-18

on schedule UKAEA is working on discrete dislocation plasticity code development:A new algorithm has been developed to calculate the displacement field of a 3D dislocation network based on the Barnett solution. This work is ongoing as an additional validation route for the design rules. Design rules have been proposed and a number of validation exercises using experimental data have been completed. The work is on schedule with only final validation against additional data from WP3 remaining.

The discrete dislocation plasticity code development is progressing slower than anticipated as the researcher has obtained independent funding with a research fellowship. The work is still ongoing however, and some results will be obtained. This aspect of the work is not vital to the completion of the task or the related deliverables.

Task 1.2: Length scale enabled plasticity models able to support property/stress mapping

M30Nov-17

on schedule UKAEA has provided UoL with a CPFEM UMAT code development for strain gradient crystal plasticity. UoL is continuing the work on crystal plasticity based finite element size effect model and simulations have been carried out for indentation contact with different contact geometries. A PhD student has implemented the complex codes and validated the results. Further sensitivity analysis of the length-scale enabled plasticity constitutive laws on the interpretation of hardness tests at different length scales will continue.

Task 2.1: Develop stronger,

M24May-17

completed A 3rd generation of single crystal diamond AFM probes for nano-indentation was produced by Adama targeting oblique cone angle with sharp apex and high spring constant. Tip shape was characterized by

Technical Report (Progress) - 10 of 17 - Issued: Month Year


stiffer AFM and IIT probes with highly repeatable, better defined tip shape

SEM and an AFM tip-checker sample before and after, verifying excellent stability, and reduced non-linear effects due to high spring constant.

UCov have received Adama cantilevers, which are compatible with the UCov Park NX20 AFM and have worked with Adama to advise on the use of reference materials and to design suitable experiments for testing the cantilever and tip performance. Testing is ongoing.

DFM have carried out measurements with Adama probes on various materials and characterized the tip shape after these measurements to check tip durability.

Task 2.2: Develop a MEMS-based IIT system with traceable force and displacement

M24May-17

completed TUCh finished the MEMS preparation and mount some samples on PCB, now PTB has to test the samples of functionality and calibrate the MEMS based system. PTB have carried out testing which has demonstrated the functionality and utility of the MEMS based measurement system which has traceable force and displacement measurement.

UCov have collaborated with NPL PTB ADAMA DFM and TUC to ensure that the MEMS device version 2 has suitable cantilever mounting capabilities for clamping an AFM tip in place without the requirement for gluing.

Task 2.3: Incorporation of optimised diamond probes into MEMS-based IIT system

M24May-17

Delayed until M30 Now-fabricated (Nov. 2016) MEMS chips are to be shipped to Adama for

fitting and adjustment.

UCov PTB NPL and Adama have developed a revised work plan to enable direct comparison of measurements between AFM, IIT and MEMS devices at UCov and PTB.

An important contribution from DFM to the project will be that a DFM scientist will be guest worker at PTB for four weeks, to develop the MEM-based IIT system. This guest worker assignment is preliminary agreed with PTB to take place in the first half of 2017.

Delays in this milestone were due to problems in the supply and optimisation of the diamond probes. However the whole process has now been demonstrated leaving verification tests to be completed. No knock on effects are expected from this delay.



Task 3.1: Materials procurement and sample generation

M15Aug-16

M15Aug-16

completed A list of materials were identified and obtained for the use of the project including Cu, CuCrZr, Ni and Cr coating, 80Au20Sn, CuSn3. In addition, UCov has obtained samples (repurposed from other projects) of single crystal Fe, single crystal W and polycrystalline NiMoNic 75 Nb and 304 stainless steel. UKAEA has been working with Eric Schmid Institute (Leoben, Austria) to produce CuCrZr samples through a high strain process combining compression and torsion to produce highly worked alloy and small grain size material.

Task 3.2: Sample characterisation using current state of the art methods

M18Nov-16

Completed All materials characterisation work has now been completed.The techniques that were utilised were SEM, EBSD TKD and TEM analysis



Task 3.3: Mechanical testing as a function of length-scale

M22Mar-17

completed Indentation tests were performed on selected samples (Cu and CuCrZr) as a function of indentation size, including data obtained using nano-indentation, micro-indentation and macro-indentation. The influence of indenter curvature was observed and the understanding of indenter geometry influence on the measurement results was developed.

All indentation testing has now been carried out on the CuCrZr using tips of various sizes from R=2um to R=1250um. Additionally identical testing has been carried out for all cold worked copper samples. Some modelling work was carried out to interpret and understand results. UKAEA has devloped coding for a standard user friendly data analysis tool, instrument calibration, independent tip measurement and verification, and AFM measurement and analysis of indentation pile-up.

Uniaxial tests were also performed on selected samples (Cu and CuCrZr) as a function of length-scales from micro-pillar compression (micro-meter range), to miniaturised ETMT testing (millimetre range), and macro testing (centimetre range). The macro data were obtained using the “stress-strain” device has been specifically designed and realized by INRIM.

Task 3.4: Thermal stability of length-scale-enabled strength

M32Jan-18

Delayed to Mar 18

NPL has purchased a new instrumented nano-indentation tester that is capable of testing at temperature above 700°C in vacuo. The system was delivered in Feb 2017. However, other laboratory moves now mean that the system will not be installed and validated until November 2017.

EMPA is in the progress has installed a new nano-indentation tester running up to 700 °C and has demonstrated its functionality with a series of measurement.

Further delays have occurred with the installation and validation of the new test system due to laboratory moves. However, installation and commissioning will now take place in early November. There will be no effects due to this delay on other tasks in the project.

Task 4.1 Extracting the material size-enabled performance

M32Jan-18

on schedule Work started on the data obtained under Task 3.3 to identify the key lengths involved: i.e. a comparison of the different Indentation Size Effect functions is being made by UCov on indentation data obtained from single crystals of Cu, Fe, and W and from polycrystalline W, NiMoNic 75, Nb and 304 stainless steel. Analysis is ongoing to determine, and feed back to



from the indentation size affected test response

WP3, the optimum indentation cycle to use for future data generation.

Task 4.2 Indentation property mapping (stress vs. strain, residual stress)

M33Feb-18

on schedule QMUL arranged a student taking an industrial replacement with UKAEA for one year (Oct2015-Aug2016). Indentation were carried out on single crystal and initial indentation stress-strain results were obtained using spherical indenters with different radii.

A second industrial placement student from QMUL has started at UKAEA. This student’s project is focused on the measurement and characterisation of pile up surrounding the indenter tip as a function of strain and tip size.

A methodology for separating test size-dependent properties from materials size-dependent properties has been developed by QMUL in association with UCov and UKAEA and is currently being evaluate.

The data generated at UKAEA will feed into task 4.1 and WP1. UCoV has generated data on a range of materials with different material properties to assess the effects of residual stress on measurements of elastic modulus as part of task 4.1. QMUL and APT have identified materials suitable for mapping mechanical properties and obtained preliminary data for task 4.2. Partners NPL, CMI, PTB and EMPA haven’t participated in this deliverable yet. Their role will become active at the next stages of the research.

Task 4.3 Feasibility of Indentation mapping of novel material properties

M33Feb-18

inactive This task has not started.

Task 5.1 M36 on schedule CS1: UCov has obtained under non-disclosure, access to the structural



Direct impact industrial case studies

May-18 design for a commercial high pressure automotive fuel rail. Burst test data has been obtained for the body of the design. A similar sized body structure that was constructed by 2D electro-deposition, using a mid-length-scale material, was burst tested in Q1 2017 but was found to be weaker than the original fuel manifold. The reason was felt to be the larger than expected grain size in the new electrodeposited sample. Plans are being made to optimise this structure with the aim of reaching the strength goals for the new technology.

CS3: Discussions have been held between NPL and E6 about this case study. It has been decided that in situ indentation of binder phase rgions in both WC/Co and polycrystalline diamond materials will be carried out to examine the link between the mechanical properties of these regions and their size.

Task 5.2 Knowledge Transfer

M36May-18

on schedule The JRP website has been regularly updated.

A major input was made to the ECI nanomechanics conference in October 2017 with 4 oral presentations and 4 poster presentations.

Papers and conference presentations are listed in the impact report.

UCov led the UK delegation to ISO/TC 164/SC3 Mechanical testing of Metals – indentation testing. Here it was agreed to work with SC3 and its working group WG4 to develop further instrumented indentationtesting methods for creep properties, elevated temperature testing and discussed adoption of project outputs.

Task 5.3 Training

M36May-18

on schedule Further training activity is planned for the last period of the project

Task 5.4 Uptake and Exploitation

M36May-18

on schedule Work is ongoing with uptake and exploitation expected in the final 9 months of the project.

Task 6.1: Project management

M36May-18

on schedule The JRP-Partners are working well together.

The partners are very motivated participating the activities of this project



and attending the project meetings.

Task 6.2: Project meetings

M36May-18

on schedule A successful kick off meeting was held at NPL on the 30th June and 1st July 2015. The 9 month meeting was held at BAM on the 14th and 15th March 2016. The 18 month meeting was held on the 16-18 January 2017 at CMI, Brno and the 27 month project meeting was held on the 18-20th September 2017 in Chemnitz University.

Task 6.3: Project reporting

M36May-18

on schedule The publishable summary was updated.

Consortium performance

EITHER provide a statement confirming that all partners have contributed satisfactorily to the activities specified in Annex 1 for this reporting period OR list any exceptions to this by naming the defaulting partner(s) and the activities that they were required to do

All partners have contributed satisfactorily to the activities specified in Annex 1 for this reporting period



4 Deviations from Annex 1 (tasks not fully implemented), the consequences and proposed corrective actions

- Annex: - Section: - Task:

Summary of proposed corrective action

Reason for deviation from Annex 1

5 Ethical Issues

Ethical issues associated with this project (as specified in Annex 1)

Third countries Yes

Data protection Yes

Dual use Yes

Environmental and health and safety / Health and safety Not applicable

Fair benefit-sharing Not applicable

Export controls / Export issues Not applicable

Use of humans/animals in research Not applicable

Requirement to complete an Ethics report during the project Not applicable

Overall Conformity with ethical requirements

The coordinator confirms that this project has conformed with all of the necessary ethical requirements specified in the Annex 1 to the Grant Agreement. /

Technical Report (Progress) - 17 of 17 - Issued: Month Year

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EMRP-template (document)empir.npl.co.uk/.../5/2019/03/14IND03-Technical-Report_… · Web viewTechnical Report (Progress) 1 of 17. Issued: August 2017. Technical Report (Progress)