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Feb 20, 2023 143 likes •431 views

Research on radiation damage of fusion relevant materials carried out at Warsaw University of Technology . Ciupiski Warsaw University of Technology Workshop Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme , 14

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Research on radiation damage of fusion relevant materials carried out at Warsaw University of Technology

Ł. Ciupiński Warsaw University of Technology

Workshop „Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme”, 14 – 15.04.2016, Rzeszów, Poland

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SLIDE 2

Workshop „Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme”, 14 – 15.04.2016, Rzeszów, Poland

Outline

  • Part I: Transmission electron microscopy investigations of self-damaged

tungsten targets

  • Part II: Miniaturized sample testing at Faculty of Materials Science / WUT

(Z. Pakieła et al.)

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SLIDE 3

Workshop „Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme”, 14 – 15.04.2016, Rzeszów, Poland

Samples 2015

Sample number Implantation conditions

  • 1. A0780A

20 MeV W ions, 0.5 dpa, at 300K, no pre-annealing, exposed to D atoms at 450K

  • 2. A0781A

0.5 dpa, at 300K, annealed at 600K for 1h, exposed to D atoms at 450K

  • 3. A0782A

0.5 dpa, at 300K, annealed at 800K for 1h, exposed to D atoms at 450K

  • 4. A0783A

0.5 dpa, at 300K, annealed at 1000K for 1h, exposed to D atoms at 450K

  • 5. A0785A

0.5 dpa, at 300K, annealed at 1130K, exposed to D atoms at 450K

TEM on self-damaged W. Defect annealing. EUROfusion Task under: PFC.SP3.1 - Role of neutron damage on retention mechanism and strength in W / Be Partners: Institute of Plasma Physics, Garching, Germany Jožef Stefan Institute, Ljubljana, Slovenia Goal: Evaluate defects morphology and distribution as well as dislocation density in the damaged W targets

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SLIDE 4
  • 1. FIB milling – thickness 200-250 nm

Ga ions, 40 kV, HITACH NB5000

  • 2. Thinning (gentle milling) –

Ar ions, 1kV to 500 V

  • 0. Self-ion damaged W plate from IPP

W6+ ions, 3 MV

TEM on self-damaged W. Defect annealing.

Workshop „Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme”, 14 – 15.04.2016, Rzeszów, Poland

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TEM on self-damaged W. Defect annealing.

Tungsten protective layer Surface protection Peripheral milling Bottom cut-off Probe welding and micro-bridge separation Extraction Sample transfer Sample fixation Probe cut-off Sample thinning Micro-bridge Probe Probe Carrier – Cu grid

5 µm 10 µm 10 µm 50 µm 10 µm 10 µm 10 µm 10 µm 5 µm

Probe Carrier – Cu grid Sample

  • M. Rasiński - Doctoral thesis
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SLIDE 6

W lamella

TEM on self-damaged W. Defect annealing.

Workshop „Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme”, 14 – 15.04.2016, Rzeszów, Poland

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SLIDE 7

7

6.94nm 2.98nm 10.5nm

10kV 5kV 2kV

Damage layer thickness as a function of final polishing kV.

HITACHI Hi-Technologies Specimen: Si single crystal Remarks: 300kV TEM image

Ga+ ion beam FIB induced sidewall damage c.a. 15 nm

60 - 80 nm W lamella (side view)

TEM on self-damaged W. Defect annealing.

Workshop „Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme”, 14 – 15.04.2016, Rzeszów, Poland

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SLIDE 8

TEM on self-damaged W. Defect annealing.

Workshop „Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme”, 14 – 15.04.2016, Rzeszów, Poland

2.5 µm

1µm

2.8 µm

1µm

1*1019 W/m2 (3.18 dpa) 3.7*1018 W/m2 (1.17 dpa)

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SLIDE 9

TEM on self-damaged W. Defect annealing.

Workshop „Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme”, 14 – 15.04.2016, Rzeszów, Poland

O.V. Ogorodnikova et. al., 2013, IPP

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SLIDE 10

A0 780A No annealing A0 785A 1130 K A0 782A 800 K Implantation damage depth difference ~2.2 mm ~3.2 mm

Workshop „Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme”, 14 – 15.04.2016, Rzeszów, Poland

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SLIDE 11

D.M. Norfleet , Acta Materialia 56 (2008) 2988–3001

A0 780A no annealing A0 785A annealed at 1130K Larger dislocation loops + lower defect density

Research on radiation damage at WUT

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SLIDE 12

No annealing 600K 800K 1000K 1130K

Research on radiation damage at WUT

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“Dislocation density drops by 66 % for the highest annealing temperature compared to the unannealed sample. This is in good agreement with the total D concentration results

  • btained by NRA and TDS, where also 60 % decrease was observed.”

Anže Založnik, Sabina Markelj, Thomas Schwarz-Selinger, Łukasz Ciupiński, Justyna Grzonka, Primož Vavpetic, Primož Pelicon, The influence of the annealing temperature on deuterium retention in self-damaged tungsten, Phys. Scr. T167 (2016) 014031 (5pp)

Dislocation density D concentration

Data from JSI: A. Zaloznik, S. Markelj

Research on radiation damage at WUT

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SLIDE 14

Part II – Miniaturized sample testing

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SLIDE 15

Miniaturized sample testing at WUT

Workshop „Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme”, 14 – 15.04.2016, Rzeszów, Poland

Source: http://www.ifmif.org

Why we need small samples in IFMIF / DONES?

  • Limited space for specimens

in the irradiation capsule / limited HF volume

  • For reliable engineering data for DEMO

design many samples needed.

  • Handling of active samples is “easier”

when they are small

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Miniaturized sample testing at WUT

Workshop „Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme”, 14 – 15.04.2016, Rzeszów, Poland

Is IFMIF / DONES the only reason to develop miniaturized sample testing methods?

A B C

microstructure of mini specimens cut out from a welded plate A-Plate 316L, B-HAZ+ weld, C-Weld

100 mm

cutting out mini specimens from a homogenizer mill

Motivation to use miniaturized samples

  • Material / technology related: nanomaterials,

weld heat affected zones, layers and coatings, gradient materials

  • Design related: small cross section, complex

shape (e.g. gear parts)

  • Cost related: low invasiveness of the

inspection vs. repair costs

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Miniaturized sample testing at WUT

Workshop „Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme”, 14 – 15.04.2016, Rzeszów, Poland

Challenges

  • Technical issues
  • Samples preparation
  • Gripping
  • Strain measurement
  • Alignment
  • Loading stability
  • …………..
  • Size effect issues
  • Relative volume of “surface layer”
  • Microstructure elements / sample size

relation

  • Sample geometry
  • ……………

Standard and mini specimen for tensile test

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SLIDE 18

5 10 15 20 25 30 100 200 300 400 500 600 700

Naprężenie [MPa] Odkształcenie (DIC) [%]

Próbka standardowa (I) II III Minipróbka (IV) V

Próbki 13HMF - wpływ wielkości próbek

Strain (DIC) [%] Stress [MPa]

Miniaturized sample testing at WUT

Workshop „Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme”, 14 – 15.04.2016, Rzeszów, Poland

Types of tests carried out at small samples at WUT

  • Static Tensile Test
  • Mini Disc Bend Test (MDBT)
  • Fatigue Crack Growth (FCG)

Samples before and after the MDBT FCG test sample gripping system

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SLIDE 19

Miniaturized sample testing at WUT

Workshop „Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme”, 14 – 15.04.2016, Rzeszów, Poland Mini specimen (IV) Standard specimen (I)

II III V

Shape and dimensions of the mini specimen (IV)

Size of specimens for static tensile tests

5 10 15 20 25 30 100 200 300 400 500 600 700

Naprężenie [MPa] Odkształcenie (DIC) [%]

Próbka standardowa (I) II III Minipróbka (IV) V

Próbki 13HMF - wpływ wielkości próbek

Stress, MPa Strain, %

Standard II III IV V

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Miniaturized sample testing at WUT

Workshop „Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme”, 14 – 15.04.2016, Rzeszów, Poland

Reliable strain measurements – optical method

Stand for tensile tests Scheme of DIC stand

10 20 30 40 100 200 300 400 500 Naprężenie [MPa] Odkształcenie [%] Uchwyty Bezpośrednio na próbce 5 10 15 20 100 200 300 400

Naprężenie [MPa] Odkształcenie [%]

Uchwyty Bezpośrednio na próbce

Strain Stress [MPa] Stress [MPa] Strain

Lens Source of light Digital camera Sample

standard

  • ptical

standard

  • ptical
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Miniaturized sample testing at WUT

Workshop „Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme”, 14 – 15.04.2016, Rzeszów, Poland

Optical method – Digital Image Correlation (DIC)

Optical extrensometer Strain field on the mini specimen surface Testing stand setup

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Miniaturized sample testing at WUT

Workshop „Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme”, 14 – 15.04.2016, Rzeszów, Poland

Miniaturized disc bend test MDBT stand at WUT The LN container Samples before and after the MDBT

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SLIDE 23

Miniaturized sample testing at WUT

Workshop „Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme”, 14 – 15.04.2016, Rzeszów, Poland

The deformation stages during MDBT

M.P. Manahan „A new postirradiation mechanical behavior test - the Miniaturized Disk Bend Test”, Nuclear Technlogy, Vol . 63, nov 1983

1 - elastic regime, 2 - elastoplastic regime, 3 - 4 – plastic deformation and strengthening 5 – crack initiation and propagation

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Miniaturized sample testing at WUT

Workshop „Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme”, 14 – 15.04.2016, Rzeszów, Poland

MDBT “applications”

  • Strength of the material – correlation with YS and UTS
  • Ductile to brittle transition temperature – correlation with Charpy

Impact Test

  • Crack resistance – correlation with KIC i JIC obtained in CT test

cylinder puncher shape sphere

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Miniaturized sample testing at WUT

Workshop „Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme”, 14 – 15.04.2016, Rzeszów, Poland

Set-up for FCG rate (dA / dN) testing Fatigue Crack Growth testing

  • T. Brynk et al., 2010
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SLIDE 26

Miniaturized sample testing at WUT

Workshop „Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme”, 14 – 15.04.2016, Rzeszów, Poland

Fatigue Crack Growth testing

Mini-samples testing with optical crack length measurements

 

f

M a Wt P K        

2 1 max

Manual crack tip tracking DIC and inverse method

                                      

4 3 2

39 , 30 72 , 21 55 , 10 231 , 12 , 1 W a W a W a W a M f

a – crack length, W - sample width, t - sample thickness, P – maximal force

26

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SLIDE 27

Miniaturized sample testing at WUT

Workshop „Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme”, 14 – 15.04.2016, Rzeszów, Poland

da/dN tests of ECAPed Al 5483

  • 1.5
  • 1
  • 0.5

0.5 1 1.5 2

  • 1.5
  • 1
  • 0.5

0.5 1 1.5 x [mm] y [mm]

  • 5.5
  • 5
  • 4.5
  • 4
  • 3.5
  • 3
  • 2.5
  • 2
  • 1.5
  • 1

x 10

  • 3
  • 1.5
  • 1
  • 0.5

0.5 1 1.5 2

  • 1.5
  • 1
  • 0.5

0.5 1 1.5 x [mm] y [mm]

  • 6
  • 5
  • 4
  • 3
  • 2
  • 1

x 10

  • 3
  • 1.5
  • 1
  • 0.5

0.5 1 1.5 2

  • 1.5
  • 1
  • 0.5

0.5 1 1.5 x [mm] y [mm] 0.022 0.024 0.026 0.028 0.03 0.032

  • 1.5
  • 1
  • 0.5

0.5 1 1.5 2

  • 1.5
  • 1
  • 0.5

0.5 1 1.5 x [mm] y [mm] 0.022 0.024 0.026 0.028 0.03 0.032 0.034

KI = 14.9 MPa*m^0.5; KII = 1.6 MPa*m^0.5; x0 =0,74 mm; y0 = 0,21 mm

DIC Model U V

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SLIDE 28

 Investigations of radiation damage in tungsten have been successfully carried out at WUT since 2011 in cooperation with foreign fusion laboratories.  The estimated dislocations densities correlate with the amount of deuterium trapped in the material.  Miniaturized samples testing is developed at WUT for more than 10 years.  Considerable experience and knowledge have been gathered for different type

  • f mechanical tests.

 The tests are used in practice to evaluate degradation of properties

  • f components being in service at industry.

Summary

Workshop „Town Meeting Workshop on IFMIF/ELAMAT Possible Scientific Programme”, 14 – 15.04.2016, Rzeszów, Poland