Development and Qualification of Small Scale Test Technologies in Structural Engineering

 
Roadmap on the development and qualification of
Small Scale Test Technologies
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023
 
1
 
M. Serrano
1
, R. Hernández
1
, R. Gallego
2
, R. Palma
2
 
1 CIEMAT
, Materials of Energy Interest Division  CIEMAT, Avda. Complutense 40, 28040
Madrid
2 
 UGR
, E.T.S. de Ingeniería de Caminos, Canales y Puertos, Universidad de Granada, Campus
Universitario de Fuentenueva (Edificio Politécnico) 18071 Granada
 
IFMIF-DONES Users Workshop Granada,  19-20 de October 2023
Contents
 
Some  slides on introduction about small
specimens
Actions towards standarization
Fission
Fusion
Non nuclear actions
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023
 
2
Why we talk about SSTT
 
Materials used in engineering
applications as structural
components are subject to loads,
defined by the application
purpose.
The mechanical properties of
materials characterize the
response of a material to loading.
Mechanical properties are
determined 
following 
standards
,
which define testing machines,
specimen shapes and sizes
,
experimental procedures, and
data 
interpretations.
Consistent,
Uniform, and
Reproducible
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023
 
3
 
Mechanical properties 
are driven by the
microstructure
 and 
stress state 
and thus “relevant
volume” should be tested to determine properties
that are 
independent of the specimen size 
to be
transferred to engineering structures
Why we talk about SSTT in IFMIF/DONES
 
The verification of the structural
components of a fusion power reactor
requires design criteria developed
specifically for those components at the
unique conditions at which they are
operated
The RCC-MRx design and construction
code constitutes a single document that
covers in a consistent manner the design
and construction of mechanical
components for high temperature
reactors, research reactors and 
fusion
reactors
Need to acquiring and gathering the data
which describe the physical and
mechanical behaviour of the material,
necessary to apply the component design
rules available in the RCC-MRx code
Materials and Design rules have been
extended in order to be applicable for
nuclear components likely to operate:
in creep conditions (significant creep)
in irradiated conditions (significant irradiation)
Mechanical data at 
RELEVANT
 irradiation
conditions
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023
 
4
Why we talk about SSTT in IFMIF/DONES
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023
 
5
 
Neutron flux (n/cm2/s) distribution on the horizontal cut-plane
 
Qiu, Y. “IFMIF-DONES HFTM neutronics
modeling and nuclear response analyses”
Nuclear Materials and Energy Volume 15,
May 2018, Pages 185-189
Each capsule of
IFMIF/DONES offers
a cuboid volume 79
mm x 39 mm x 16.5
mm (54 cm³) for
specimens
A standard fracture
toughness specimen,
with a thickness of 16
mm to be
accommodated within
the capsule, has a
dimensions of  40 mm x
38.4 mm x 16 mm
 
Reduce the
dimensions of the
testing specimens
 
hardly
 two standard
specimens should be
irradiated within the
same capsule
Advantages of SSTT -> Small volume
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023
 
6
Challenges on the use of SSTT- > Lack of standards (for
some techniques)
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023
 
7
Actions towards standarization
 
Previous activities
Nuclear Fission
EURATOM funded Project FRACTESUS
Nuclear Fusion
EUROFUSION
IAEA Towards the Standardization of Small
Specimen Test Techniques for Fusion Applications
CRP II
Non Nuclear actions
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023
 
8
Previous activities
 
The lack of standardization, not only for
the specimen geometry but also for the
testing protocol and data uncertainty
analysis, is highlight in all the SSTT
activities since decades
Early effort for standardization 
on the
use of SSTT for fission and fusion
applications was launched by 
ASTM
 in
the 80’s and a task group was thus formed
under the auspices of ASTM
Subcommittee E10.02 on “
Behavior and
Use of Metallic Materials in Nuclear
Systems
” to consider whether a set of
recommended practices for individual
small-specimen techniques might be
useful and, if so, to write such practices.
They agree to organise a serie of
symposium on small-specimen testing
,
being the first held in 1983 in
Albuquerque, New Mexico, and focused
on test techniques for fusion reactors and
the last one was held in  2014 in Houston.
 
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop (on-line) 26-27 September 2022
 
9
 
Nuclear Fission - FRACTESUS
 
EURATOM funded Project FRACTESUS Fracture mechanics testing
of irradiated RPV steels by means of sub-sized specimens Euratom
work programme 2019-2020 GA 900014
The objective is the validation of the use of small CT specimen for the
determination of the T
0
 transition reference temperature –> Reactor
pressure vessel surveillance
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023
 
10
 
Li, M., Chaouadi, R., Uytdenhouwen, I., & Pardoen, T.
(2023). Engineering Fracture Mechanics, 290, 109486.
RPV surveillance tests
 
Nuclear Fusion - IAEA
 
IAEA Coordinated Research Project (CRP) 
Towards the Standardization of Small
Specimen Test Techniques for Fusion Applications (F13017)
 2017-2021
to provide a set of guidelines for SSTT based on common agreed best practices on
main test techniques (tensile, creep, low cycle fatigue, fracture toughness, fatigue
crack growth) valid for reference structural Fusion materials (RAFM steels)
to establish supporting experimental activities and
to elaborate datasets and elements needed for a full standardization of the SSTT by an
international authority like ASTM or ISO.
Note: the standardization process itself was not part of the CRP
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023
 
11
 
Shanghai Jiao Tong University  
  
China
KIT 
    
Germany
Osaka University  
   
Japan
QST 
    
Japan
NIFS 
    
Japan
CIEMAT 
    
Spain
UKAEA 
    
UK
 
IAEA  
Sehila M. Gonzalez de Vicente
Rapporteurs
Eberhard Diegele (independent expert)
Roland Heidinger (independent expert)
Nuclear Fusion - IAEA
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023
 
12
Tensile:  375 completed at
4 labs.
Creep: 20 tests
completed
LCF: 147 test completed
@RT, @550C
-
Master Curve: 34
completed
-
Brittle (local)
Approach: 43
completed
-
Ductile Approach: 96
completed
FCG: 8 completed at 2 labs, all @RT
 
Heavely affected by
COVID lockdown
 
The CRP includes an expert and in-depth literature review for the
tests selected that is unique in its scope addressing a wealth of
tests and types of specimen.
“Reference” guidelines have been established, following
international standards, for the five different test techniques.
Subsequently, they have been applied in the course of the CRP to
get immediate feedback in terms of applicability and verification.
“Round Robin”: Respective test matrices (selection of specimens,
materials and common “test conditions”, test methodologies)
were agreed
Nuclear Fusion - IAEA
 
IAEA Coordinated Research Project (CRP) 
Towards the Standardization of Small Specimen Test
Techniques for Fusion Applications 
PHASE II (2023-2026)
To provide the bases for the standardization of SSTT specimens making them available for their use in
Fusion material irradiation facilities. This includes:
(a) to provide a set of guidelines for SSTT based on common agreed best practices on main test techniques
(tensile, creep, low cycle fatigue, fracture toughness, fatigue crack growth) valid for reference structural Fusion
materials (RAFM steels);
(b) to establish supporting experimental activities and
(c) to elaborate datasets and elements needed for a full standardization of the SSTT by an international authority
like ASTM or ISO.
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023
 
13
1st Research Coordination Meeting
 30 January to 01 February 2023
IAEA Headquarters, VIC, Vienna, Austria
 
Comision Nacional de Energia Atomica 
 
Argentina
SCK CEN  
    
Belgium
Shanghai Jiao Tong University  
  
China
KIT 
    
Germany
Centre for Energy Research  
  
Hungary
Osaka University  
   
Japan
QST 
    
Japan
NIFS 
    
Japan
CIEMAT 
    
Spain
National Nuclear Laboratory  
  
UK
UKAEA 
    
UK
Oxford Sigma 
   
UK
University of California, Berkeley  
  
USA
 
IAEA  [
Sehila M. Gonzalez de Vicente]
Rapporteurs
Eberhard Diegele (independent expert)
Roland Heidinger (independent expert)
 
Nuclear Fusion - EUROFUSION
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023
 
14
 
H2020 EUROFUSION 2015-2020
 
HE EUROFUSION 2021-2024
 
transversal activity
between ENS / DONES
and MAT (DEMO: EDDI /
SDQ / HHFM / IRRAD;
TBM),
RAFM, CuCrZ, W
Tensile, LCF, FT
Roadmap for
standarization
Non-nuclear actions
 
Characterize additive manufactured materials,
especially for metal-based technologies. [J. Dzugan et
al mainly]
high costs (raw material),
high number of samples needed to fully characterize a batch
of material.
traceability at various locations and anisotropy
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023
 
15
 
Dzugan, J., Seifi, M., Prochazka, R., Rund, M., Podany, P., Konopik, P., & Lewandowski, J. J. (2018). Effects of thickness and orientation on the small scale fracture
behaviour of additively manufactured Ti-6Al-4V. 
Materials Characterization
143
, 94-109.
Li, Y., Krajňák, T., Podaný, P., Veselý, J., & Džugan, J. (2023). Thermal stability of dislocation structure and its effect on creep property in austenitic 316L stainless
steel manufactured by directed energy deposition. 
Materials Science and Engineering: A
873
, 144981.
ASTM WK83107
(see later)
Non-nuclear actions
 
Data-driven evaluation of mechanical properties - 
high-throughput materials
evaluation techniques
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023
 
16
 
Heckman, N. M., Ivanoff, T. A., Roach, A. M., Jared, B. H., Tung, D. J., Brown-Shaklee, H. J., ... & Boyce, B. L. (2020). Automated high-throughput tensile testing reveals
stochastic process parameter sensitivity. Materials Science and Engineering: A, 772, 138632.
Gianola, D. S., della Ventura, N. M., Balbus, G. H., Ziemke, P., Echlin, M. P., & Begley, M. R. (2023). Advances and opportunities in high-throughput small-scale
mechanical testing. 
Current Opinion in Solid State and Materials Science
27
(4), 101090.
Heckman, N. M
Daniel S. Gianola
MAT-T.01.03-T017 D001 Interaction with regulatory
body (URG/CIEMAT)
 
Roadmap under development within
EUROFUSION WPMAT-EDDI-SSTT
ASTM route was selected as some ongoing
activities on SSTT already exists
EUROFUSION PILOT RUN:
Objectives
Organization
Labs, Test method and protocol
Time table
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023
 
17
Standarization route
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop (on-line) 26-27 September 2022
 
18
 
ASTM 
New Standard Activity
Determine if new standard is needed
Identify key stakeholders
Identify Committee and Subcommittee
 
Committee E10 – Nuclear
Applications or Committee E08
Register a Work Item
 
www.astm.org
 
ASTM Stimulates 
participation
from outside of task group
Balloting
Final publication
Standarization route
 
ASTM Work Item
1. Scope
2. Referenced Documents
3. Terminology
o
3.1 Definitions
4. Significance and Use
5. Apparatus
6. Test Specimens
7. Procedure
8. Post-Test Examination
9. Report
10. Precision and Bias
(MANDATORY)
 
11. Keywords
 
 
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop (on-line) 26-27 September 2022
 
19
An 
interlaboratory study (ILS) 
is
a multi lab study done for the specific purpose of
producing data that will be used to develop a
Precision & Bias statement and
Research Report in order to demonstrate the
expected variability of a test method.
ASTM E691 − 19 
An American National Standard
Standard Practice for Conducting an Interlaboratory
Study to Determine the Precision of a Test Method
Where numerical data have
been
generated to establish the
precision
and bias of a test method, a
research report 
is
required
13. 
Pilot Run
13.1 Before investing laboratory time in the full scale ILS,
it is usually wise to conduct a pilot run with only one, or
perhaps two, material(s) to determine whether the test
method as well as the protocol and all the ILS procedures
are clear, and to serve as a familiarization procedure for
those without sufficient experience with the method (see
9.3).
The results of this pilot run also give the task group an
indication of how well each laboratory will perform in
terms of promptness and following the protocol.
Laboratories with poor performance should be
encouraged and helped to take corrective action.
MAT-T.01.03-T017 D001 Interaction with regulatory
body (URG/CIEMAT)
 
ASTM ongoing activities on SSTT
Subcommittee E28.04.01 (Task Group on Small Specimens in E8/E8M) 
to publish an annex
providing guidelines to uniaxial tensile testing of subscale geometries WK83107
Additional efforts are underway through 
ASTM Subcommittee F42.01 
(New Test Method for
Additive Manufacturing – Test Artifacts – Miniature Tension Testing of Metallic Materials),
 
ASTM WK83107 . Rationale
There are situations where standard ASTM E8/E8M specimens are too large. These are often
because a particular part or component from which the test specimen is to be excised is small.
Excising miniature specimens is a logical conclusion, however there are some important
considerations that need to be addressed. Tensile test procedures and properties can be
dramatically affected by specimen size. 
This annex is intended to address the problems that can
arise from testing miniature tensile specimens.
ASTM Interlaboratory Study to Establish Precision
Statements for Tensile Testing of Miniature specimens using
ASTM E/E8M
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023
 
20
EXAMPLE OF AN EXISTING WK ON SSTT (TENSILE)
MAT-T.01.03-T017 D001 Interaction with regulatory body
(URG/CIEMAT)
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023
 
21
2023
2024
2025
Pilot run on tensile properties
ASTM Committe selection
ILS on tensile properties at
room temperature
Pilot run on high temperature
tensile
Tensile properties at room
temperature
First draft of the ASTM
WK including ILS
ILS results submitted to
the ASTM ILS section for
approval
Tensile properties at room
temperature
Draft standard in the
ASTM format
Ballotting of the draft
standard
Tensile properties draft (room
temperature)
Pilot run on fracture toughness
 
TO BE DISCUSSED at Next WPMAT-EDDI
SSTT meeting
MAT-T.01.03-T017 D001 Interaction with
regulatory body (URG/CIEMAT)
 
PLANNED ACTIVITIES in 2023: PILOT RUN
Send material to Labs (SCK-CEN)
Finish protocol and test method (Task Group)
Follow draft of AX1 for E8/E8M balloting
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023
 
22
MAT-T.01.03-T017 D001 Interaction with regulatory
body (URG/CIEMAT)
 
Pilot run on tensile properties at room temperature
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023
 
23
MAT-T.01.03-T017 D001 Interaction with regulatory
body (URG/CIEMAT)
 
Definition of tensile geometries
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023
 
24
EU FLAT
Modification of
“DONES” geometry to
fulfil Standard
requirements on
proportionality
SCKCEN ROUND
Same geometry used
for EUROFER97
irradiation campaigns
SS-J3
Extensilevly used, e.g.
IAEA CRP on SSTT
MAT-T.01.03-T017 D001 Interaction with regulatory
body (URG/CIEMAT)
 
Finish protocol and test method (Task Group)
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023
 
25
Summary
 
Different actions towards the standardization of small
specimens to determine mechanical properties are
presented (past and present)
Within nuclear fusion two main action are already run
in parallel and connected:
IAEA Coordinated Research Project (CRP) Towards the
Standardization of Small Specimen Test Techniques for
Fusion Applications
MAT-T.01.03-T017 D001 Interaction with regulatory body
(URG/CIEMAT)
First step for the standardization of SSTT has been
launched within EUROFUSION WPMAT-EDDI-SSTT
2023 Pilot run on tensile properties at room temperature
launched
 
05/04/2024
 
M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023
 
26
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Small Scale Test Technologies (SSTT) play a crucial role in determining the mechanical properties of materials used in engineering applications. This roadmap focuses on the importance of testing relevant volumes to ensure transferability to real-world structures. It discusses the need for consistent, uniform, and reproducible testing methods, especially in the context of fusion power reactors. The aim is to acquire data to accurately design and construct mechanical components for high-temperature and nuclear reactors.


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  1. Roadmap on the development and qualification of Small Scale Test Technologies M. Serrano1, R. Hern ndez1, R. Gallego2, R. Palma2 1 CIEMAT, Materials of Energy Interest Division CIEMAT, Avda. Complutense 40, 28040 Madrid 2 UGR, E.T.S. de Ingenier a de Caminos, Canales y Puertos, Universidad de Granada, Campus Universitario de Fuentenueva (Edificio Polit cnico) 18071 Granada IFMIF-DONES Users Workshop Granada, 19-20 de October 2023 05/04/2024 M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023 1

  2. Contents Some slides on introduction about small specimens Actions towards standarization Fission Fusion Non nuclear actions 05/04/2024 M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023 2

  3. Why we talk about SSTT Mechanical properties are driven by the microstructure and stress state and thus relevant volume should be tested to determine properties that are independent of the specimen size to be transferred to engineering structures Transferability Materials used in engineering applications as structural components are subject to loads, defined by the application purpose. The mechanical properties of materials characterize the response of a material to loading. Mechanical properties are determined following standards, which define testing machines, specimen shapes and sizes, experimental procedures, and data interpretations. Consistent, Uniform, and Reproducible 05/04/2024 M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023 3

  4. Why we talk about SSTT in IFMIF/DONES The verification of the structural components of a fusion power reactor requires design criteria developed specifically for those components at the unique conditions at which they are operated The RCC-MRx design and construction code constitutes a single document that covers in a consistent manner the design and construction of mechanical components for high temperature reactors, research reactors and fusion reactors Need to acquiring and gathering the data which describe the physical and mechanical behaviour of the material, necessary to apply the component design rules available in the RCC-MRx code Materials and Design rules have been extended in order to be applicable for nuclear components likely to operate: in creep conditions (significant creep) in irradiated conditions (significant irradiation) Mechanical data at RELEVANT irradiation conditions Key challenge for fusion reactor > main reason why IFMIF/DONES is required 05/04/2024 M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023 4

  5. Why we talk about SSTT in IFMIF/DONES A standard fracture toughness specimen, with a thickness of 16 mm to be accommodated within the capsule, has a dimensions of 40 mm x 38.4 mm x 16 mm Each capsule of IFMIF/DONES offers a cuboid volume 79 mm x 39 mm x 16.5 mm (54 cm ) for specimens Reduce the dimensions of the testing specimens hardly two standard specimens should be irradiated within the same capsule Neutron flux (n/cm2/s) distribution on the horizontal cut-plane Qiu, Y. IFMIF-DONES HFTM neutronics modeling and nuclear response analyses Nuclear Materials and Energy Volume 15, May 2018, Pages 185-189 05/04/2024 M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023 5

  6. Advantages of SSTT -> Small volume 05/04/2024 M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023 6

  7. Challenges on the use of SSTT- > Lack of standards (for some techniques) 05/04/2024 M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023 7

  8. Actions towards standarization Previous activities Nuclear Fission EURATOM funded Project FRACTESUS Nuclear Fusion EUROFUSION IAEA Towards the Standardization of Small Specimen Test Techniques for Fusion Applications CRP II Non Nuclear actions 05/04/2024 M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023 8

  9. Previous activities The lack of standardization, not only for the specimen geometry but also for the testing protocol and data uncertainty analysis, is highlight in all the SSTT activities since decades Early effort for standardization on the use of SSTT for fission and fusion applications was launched by ASTM in the 80 s and a task group was thus formed under the auspices of ASTM Subcommittee E10.02 on Behavior and Use of Metallic Materials in Nuclear Systems to consider whether a set of recommended practices for individual small-specimen techniques might be useful and, if so, to write such practices. They agree to organise a serie of symposium on small-specimen testing, being the first held in 1983 in Albuquerque, New Mexico, and focused on test techniques for fusion reactors and the last one was held in 2014 in Houston. 05/04/2024 M. Serrano IFMIF-DONES Users Workshop (on-line) 26-27 September 2022 9

  10. Nuclear Fission - FRACTESUS EURATOM funded Project FRACTESUS Fracture mechanics testing of irradiated RPV steels by means of sub-sized specimens Euratom work programme 2019-2020 GA 900014 The objective is the validation of the use of small CT specimen for the determination of the T0 transition reference temperature > Reactor pressure vessel surveillance Li, M., Chaouadi, R., Uytdenhouwen, I., & Pardoen, T. (2023). Engineering Fracture Mechanics, 290, 109486. RPV surveillance tests 05/04/2024 M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023 10

  11. Nuclear Fusion - IAEA IAEA Coordinated Research Project (CRP) Towards the Standardization of Small Specimen Test Techniques for Fusion Applications (F13017) 2017-2021 to provide a set of guidelines for SSTT based on common agreed best practices on main test techniques (tensile, creep, low cycle fatigue, fracture toughness, fatigue crack growth) valid for reference structural Fusion materials (RAFM steels) to establish supporting experimental activities and to elaborate datasets and elements needed for a full standardization of the SSTT by an international authority like ASTM or ISO. Note: the standardization process itself was not part of the CRP IAEA Sehila M. Gonzalez de Vicente Rapporteurs Eberhard Diegele (independent expert) Roland Heidinger (independent expert) Shanghai Jiao Tong University KIT Osaka University QST NIFS CIEMAT UKAEA China Germany Japan Japan Japan Spain UK 05/04/2024 M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023 11

  12. Nuclear Fusion - IAEA The CRP includes an expert and in-depth literature review for the tests selected that is unique in its scope addressing a wealth of tests and types of specimen. Reference guidelines have been established, following international standards, for the five different test techniques. Subsequently, they have been applied in the course of the CRP to get immediate feedback in terms of applicability and verification. Round Robin : Respective test matrices (selection of specimens, materials and common test conditions , test methodologies) were agreed Heavely affected by COVID lockdown Tensile: 375 completed at 4 labs. Creep: 20 tests completed - Master Curve: 34 completed Brittle (local) Approach: 43 completed Ductile Approach: 96 completed LCF: 147 test completed @RT, @550C - - FCG: 8 completed at 2 labs, all @RT 05/04/2024 M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023 12

  13. Nuclear Fusion - IAEA IAEA Coordinated Research Project (CRP) Towards the Standardization of Small Specimen Test Techniques for Fusion Applications PHASE II (2023-2026) To provide the bases for the standardization of SSTT specimens making them available for their use in Fusion material irradiation facilities. This includes: (a) to provide a set of guidelines for SSTT based on common agreed best practices on main test techniques (tensile, creep, low cycle fatigue, fracture toughness, fatigue crack growth) valid for reference structural Fusion materials (RAFM steels); (b) to establish supporting experimental activities and (c) to elaborate datasets and elements needed for a full standardization of the SSTT by an international authority like ASTM or ISO. IAEA [Sehila M. Gonzalez de Vicente] Rapporteurs Eberhard Diegele (independent expert) Roland Heidinger (independent expert) Comision Nacional de Energia Atomica SCK CEN Shanghai Jiao Tong University KIT Centre for Energy Research Osaka University QST NIFS CIEMAT National Nuclear Laboratory UKAEA Oxford Sigma University of California, Berkeley Argentina Belgium China Germany Hungary Japan Japan Japan Spain UK UK UK USA 1st Research Coordination Meeting 30 January to 01 February 2023 IAEA Headquarters, VIC, Vienna, Austria 05/04/2024 M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023 13

  14. Nuclear Fusion - EUROFUSION HE EUROFUSION 2021-2024 H2020 EUROFUSION 2015-2020 transversal activity between ENS / DONES and MAT (DEMO: EDDI / SDQ / HHFM / IRRAD; TBM), RAFM, CuCrZ, W Tensile, LCF, FT Roadmap for standarization 05/04/2024 M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023 14

  15. Non-nuclear actions Characterize additive manufactured materials, especially for metal-based technologies. [J. Dzugan et al mainly] high costs (raw material), high number of samples needed to fully characterize a batch of material. traceability at various locations and anisotropy ASTM WK83107 (see later) Dzugan, J., Seifi, M., Prochazka, R., Rund, M., Podany, P., Konopik, P., & Lewandowski, J. J. (2018). Effects of thickness and orientation on the small scale fracture behaviour of additively manufactured Ti-6Al-4V. Materials Characterization,143, 94-109. Li, Y., Kraj k, T., Podan , P., Vesel , J., & D ugan, J. (2023). Thermal stability of dislocation structure and its effect on creep property in austenitic 316L stainless steel manufactured by directed energy deposition. Materials Science and Engineering: A, 873, 144981. 05/04/2024 M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023 15

  16. Non-nuclear actions Data-driven evaluation of mechanical properties - high-throughput materials evaluation techniques Heckman, N. M Daniel S. Gianola Heckman, N. M., Ivanoff, T. A., Roach, A. M., Jared, B. H., Tung, D. J., Brown-Shaklee, H. J., ... & Boyce, B. L. (2020). Automated high-throughput tensile testing reveals stochastic process parameter sensitivity. Materials Science and Engineering: A, 772, 138632. Gianola, D. S., della Ventura, N. M., Balbus, G. H., Ziemke, P., Echlin, M. P., & Begley, M. R. (2023). Advances and opportunities in high-throughput small-scale mechanical testing. Current Opinion in Solid State and Materials Science,27(4), 101090. 05/04/2024 M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023 16

  17. MAT-T.01.03-T017 D001 Interaction with regulatory body (URG/CIEMAT) Roadmap under development within EUROFUSION WPMAT-EDDI-SSTT ASTM route was selected as some ongoing activities on SSTT already exists EUROFUSION PILOT RUN: Objectives Organization Labs, Test method and protocol Time table 05/04/2024 M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023 17

  18. Standarization route www.astm.org ASTM New Standard Activity Determine if new standard is needed Identify key stakeholders Committee E10 Nuclear Applications or Committee E08 Identify Committee and Subcommittee ASTM Stimulates participation from outside of task group Register a Work Item Balloting Final publication 05/04/2024 M. Serrano IFMIF-DONES Users Workshop (on-line) 26-27 September 2022 18

  19. Standarization route An interlaboratory interlaboratory study (ILS) a multi lab study done for the specific purpose of producing data that will be used to develop a Precision & Bias statement and Research Report in order to demonstrate the expected variability of a test method. ASTM E691 19 An American National Standard Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method study (ILS) is Where numerical data have been generated to establish the precision and bias of a test method, a research report research report is required ASTM Work Item 1. Scope 2. Referenced Documents 3. Terminology 3.1 Definitions 4. Significance and Use 5. Apparatus 6. Test Specimens 7. Procedure 8. Post-Test Examination 9. Report 10. Precision and Bias (MANDATORY) 11. Keywords o 13. Pilot Run 13.1 Before investing laboratory time in the full scale ILS, it is usually wise to conduct a pilot run with only one, or perhaps two, material(s) to determine whether the test method as well as the protocol and all the ILS procedures are clear, and to serve as a familiarization procedure for those without sufficient experience with the method (see 9.3). The results of this pilot run also give the task group an indication of how well each laboratory will perform in terms of promptness and following the protocol. Laboratories with poor performance should be encouraged and helped to take corrective action. 05/04/2024 M. Serrano IFMIF-DONES Users Workshop (on-line) 26-27 September 2022 19

  20. MAT-T.01.03-T017 D001 Interaction with regulatory body (URG/CIEMAT) EXAMPLE OF AN EXISTING WK ON SSTT (TENSILE) ASTM ongoing activities on SSTT Subcommittee E28.04.01 (Task Group on Small Specimens in E8/E8M) to publish an annex providing guidelines to uniaxial tensile testing of subscale geometries WK83107 Additional efforts are underway through ASTM Subcommittee F42.01 (New Test Method for Additive Manufacturing Test Artifacts Miniature Tension Testing of Metallic Materials), STILL NOT APPROVED ASTM WK83107 . Rationale There are situations where standard ASTM E8/E8M specimens are too large. These are often because a particular part or component from which the test specimen is to be excised is small. Excising miniature specimens is a logical conclusion, however there are some important considerations that need to be addressed. Tensile test procedures and properties can be dramatically affected by specimen size. This annex is intended to address the problems that can arise from testing miniature tensile specimens. ASTM Interlaboratory Study to Establish Precision Statements for Tensile Testing of Miniature specimens using ASTM E/E8M 05/04/2024 M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023 20

  21. MAT-T.01.03-T017 D001 Interaction with regulatory body (URG/CIEMAT) TO BE DISCUSSED at Next WPMAT-EDDI SSTT meeting 2023 Pilot run on tensile properties Tensile properties at room temperature First draft of the ASTM WK including ILS ILS results submitted to the ASTM ILS section for approval ASTM Committe selection ILS on tensile properties at room temperature Pilot run on high temperature tensile 2024 Tensile properties draft (room temperature) Pilot run on fracture toughness Tensile properties at room temperature Draft standard in the ASTM format Ballotting of the draft standard 2025 05/04/2024 M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023 21

  22. MAT-T.01.03-T017 D001 Interaction with regulatory body (URG/CIEMAT) PLANNED ACTIVITIES in 2023: PILOT RUN Send material to Labs (SCK-CEN) Finish protocol and test method (Task Group) Follow draft of AX1 for E8/E8M balloting 05/04/2024 M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023 22

  23. MAT-T.01.03-T017 D001 Interaction with regulatory body (URG/CIEMAT) Pilot run on tensile properties at room temperature 05/04/2024 M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023 23

  24. MAT-T.01.03-T017 D001 Interaction with regulatory body (URG/CIEMAT) Definition of tensile geometries EU FLAT Modification of DONES geometry to fulfil Standard requirements on proportionality SCKCEN ROUND Same geometry used for EUROFER97 irradiation campaigns SS-J3 Extensilevly used, e.g. IAEA CRP on SSTT 05/04/2024 M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023 24

  25. MAT-T.01.03-T017 D001 Interaction with regulatory body (URG/CIEMAT) Finish protocol and test method (Task Group) 05/04/2024 M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023 25

  26. Summary Different actions towards the standardization of small specimens to determine mechanical properties are presented (past and present) Within nuclear fusion two main action are already run in parallel and connected: IAEA Coordinated Research Project (CRP) Towards the Standardization of Small Specimen Test Techniques for Fusion Applications MAT-T.01.03-T017 D001 Interaction with regulatory body (URG/CIEMAT) First step for the standardization of SSTT has been launched within EUROFUSION WPMAT-EDDI-SSTT 2023 Pilot run on tensile properties at room temperature launched 05/04/2024 M. Serrano IFMIF-DONES Users Workshop Granada 19-20 October 2023 26

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