Small-Scale Mechanical Testing on Ion Beam and Neutron Irradiated - - PowerPoint PPT Presentation

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Small-Scale Mechanical Testing on Ion Beam and Neutron Irradiated - - PowerPoint PPT Presentation

Small-Scale Mechanical Testing on Ion Beam and Neutron Irradiated Engineering Materials Peter Hosemann ; D. Frazer, H. Vo, A. Reichardt University of California at Berkeley Nuclear Engineering 1 OUTLINE Introduction/Background Mechanical


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Small-Scale Mechanical Testing on Ion Beam and Neutron Irradiated Engineering Materials

Peter Hosemann;

  • D. Frazer, H. Vo, A. Reichardt

University of California at Berkeley Nuclear Engineering

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OUTLINE

Introduction/Background Mechanical property changes due to displacement damage Indentation Micro compression testing Micro tensile testing Micro bend testing Non ambient environment Summary

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Ion beam irradiations and implantation in nuclear engineering

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WHY SMALL SCALE MECHANICAL TESTING ?

Reactor, Fusion,BLIP and Spallation source irradiations Ion beam irradiations

  • Materials will be radioactive.
  • Time consuming, costly,
  • Available samples are often limited
  • Bulk sample irradiation
  • Material will not be radioactive.
  • Several dpa/day. àFast
  • Cost effective.
  • Fundamental studies are accessible
  • Limited penetration depth of ions in

matter. Small scale mechanical testing can be useful for both! Small scale mechanical testing:

  • Add more data points to decrease

uncertainty.

  • Local areas are accessible (welds)
  • Additional conditions can be tested
  • n the same sample (temp, env.,

etc.) Small scale mechanical testing:

  • Mechanical data can be gained from

ion beam irradiated materials.

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Micromechanical testing on an ion beam irradiated engineering alloy ION BEAM IRRADIATION OF 304SS

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MATERIAL STUDIED AND ION BEAM IRRADIATION

G.S.Was and Z. Jiao Univ. Michigan à 1dpa irradiation and 10 dpa irradiation à 2MeV protons at 360°C à Sample material 304SS 304SS is the material studied here Samples were provided by UM G.S.Was and Z. Jiao Univ. Michigan

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INDENTATION TESTING AT ROOM TEMPERATURE AND ELEVATED TEMPERATURE.

cBN Ion beam penetration depth

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CROSS SECTION MEASUREMENTS ON ION BEAM IRRADIATED MATERIALS.

Irradiated property Un-irradiated property

0.5 1 1.5 2 2.5 1000 2000 3000 4000 5000 Irradiated not irradiated not irradiated Nix&Gao fit irradiated Nix and Gao fit

Hardness [GPa] Indentation depth [nm] IR Depth

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1 2 3 4 5 6 7 5 10 15 20 25 30 35

Hardness (GPa) Distance from the surface (um)

Irradiated Control 1 2 3 4 5 6 7 5 10 15 20 25 30 35

Hardness (GPa) Distance from the sample surface (um)

EXAMPLE, CROSS SECTION INDENTATION ON 304 SS IRRADIATED AT UMIBL, QUANTITATIVE DATA

1E-22 1E-21 1E-20 1E-19 1E-18 5 10 15 20 25 1000 2000 3000 4000 5000 6000 7000 8000 9000 10000

dose rate [displacements/atom/ion]

Depth [um]

H content Atoms/cm3/ions/cm2]

H content displacemtn damage

  • A. Lupinacci; P. Hosemann. et al JNM, 2014

1dpa irradiated at 360C 304 SS (protons) 10dpa irradiated at 360C 304 SS (protons) At ion beam dose of 10dpa the beam profile cannot be detected any more. à Defect saturation SRIM calculations

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HIGH TEMPERATURE NANOINDENTATION ON ION BEAM IRRADIATED

  • MATERIALS. (304SS-10DPA)

Tracing the hardness of the irradiated and unirradiated material

  • ver

different temperatures using the Micromaterials Indenter.

  • H. Vo et al. JOM 2015

Control thermocouple Control thermocouple Resistance heater Cement Sample Pendulum assembly Water cooled heat shield AlN tile Insulating base Resistance heater

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INDENTATION SIZE EFFECT AND A POSSIBLE APPROACH TO EXTRACT BULK DATA

Indentation size effect is well known and can be fitted with the Nix and Gao model: H.. Hardness at depth H0.. hardness at infinite depth h… depth H*…characteristic depth Macro hardness Convert Berkovich Hardness to HV Hv=0.0947*Hnano Relate HV to YS σy = 2.5 (Hv – 68) Empirical equations. G.R.Odette et al. Step 1) Step 2) Step 3) The size effect over temperature is difficult to assess; Assumption: The relative difference between nanohardness and microhardness does not change with temperature.

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100 200 300 400 500 600 700 800 100 200 300 400

STRESS [MPa] Temperature (C)

UTS- Tensile YS-Tensile NI-YS Method 1

Neutron irradiated and tensile tests vs. Nanoindentation RT measurements

CORRELATING THE NANOINDENTATION TO YS MEASURED BY TENSILE TESTING

0.0 100.0 200.0 300.0 400.0 500.0 600.0 700.0 100 200 300 h* Temperature (°C)

800H Control RT: h* vs. Temperature

Grain 1 Grain 2

Size effect is less pronounced at higher temperature à Underestimation of YS at higher temeprature

500 1000 1500 2000 Yield, Flow [MPa]

Correlation Comparison for Irradiated Alloys

Calculated vs. Measured Stress

s_Busby_H1000 s_Busby_H0 s_Milot_H1000 s_Milot_H0 s_y s_flow

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MICRO COMPRESSION TESTING ON ION BEAM IRRADIATED 304SS

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20 µm Grain size typically ~20µm to ~200µm

3 different sets of pillars are manufactured in the same grain and tested using the Hysitron PI85 in-situ indenter

SAMPLING DIFFERENT AREAS OF THE DOSE PROFILE

  • A. Reichardt et al JNM 2017

Penetration depth

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Unirradiated Pillars Irradiated Pillars Irradiated Stopping Point Pillars

COMPRESSION TEST RESULTS

  • A. Reichardt et al JNM 2017
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3 µm

Not irradiated

Many small slip events occurred.

10dpa region Stopping peak region

Very few but large slip events occur

POST TESTING SEM IMAGES OF THE PILLARS

  • A. Reichardt JNM 2017
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LOAD DROPS ANALYSIS

  • A. Reichardt et al JNM 2017

Peierls stress: 𝑋 = 𝜐$%&%'() ∗ 𝑐 ∗ 𝑚 ∗ 𝑢𝑚 + 𝛿 ∗ 𝑐 ∗ 𝑚 Energy to move a dislocation through the pillar: Surface energy Energy to move the dislocation through the pillar 𝜐$%&%'() = 2𝐻 1 − 𝜉 ∗ ex p( −2𝜌 𝑒 1 − 𝜉 𝑐) b=burgers vector, G=shear modulus, γ=surface energy, ν=poison ratio, l=pillar width, tl=length of the slip plane # 𝑒𝑗𝑡𝑚𝑝𝑑𝑏𝑢𝑗𝑝𝑜𝑡 = 𝐹𝑜𝑓𝑠𝑕𝑧 𝑠𝑓𝑚𝑓𝑏𝑡𝑓𝑒 𝑒𝑣𝑠𝑗𝑜𝑕 𝑏 𝑚𝑝𝑏𝑒 𝑒𝑠𝑝𝑞 𝐹𝑜𝑓𝑠𝑕𝑧 𝑢𝑝 𝑒𝑠𝑗𝑤𝑓 𝑝𝑜𝑓 𝑒𝑗𝑡𝑚𝑝𝑑𝑏𝑢𝑗𝑝𝑜 𝒕𝒎𝒋𝒒 𝒕𝒖𝒇𝒒 𝒊𝒇𝒋𝒉𝒊𝒖 =# dislocations* burgers vector Force Displacement Energy for a load drop

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COMPARISON IRRADIATED VS. UNIRRADIATED

Not irradiated material: ~200 - 500 dislocations pass through the pillar/slip event à50-120 nm slip step height Irradiated material: ~3500 dislocations pass through the pillar/slip event à868 nm slip step height

3 µm 3 µm

  • K. Farrel et al. 316L

0.78dpa ORNL 2002 TEM 304 10dpa pillar test

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FIB trench

COMPRESSION TESTING TO EVALUATE FRICTION PARAMETERS IN SiC/SiC COMPOSITES

3µm

Matrix Fiber Interphase

  • J. Kabel et all Composites B 2017
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Pillar testing: HNLS control Pillar testing: HNLS 11.8dpa HFIR samples IN SITU TESTING OF FIBER/MATRIX INTERFACES

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𝑄

U'%VW ∗ 𝑡𝑗𝑜θ

𝐵 = 𝑄

U'%VW ∗ 𝑑𝑝𝑡θ

𝐵 ∗ 𝜈 + τ\%U]^\

𝝊𝒆𝒇𝒄𝒑𝒐𝒆 µ

EVALUATING THE FRICTION PARAMETERS

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MICRO TENSILE TESTING ON IRRADIATED MATERIALS

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MICRO TENSILE TESTING ON 10DPA 304SS

200 400 600 800 1000 1200 1400 1600 1800 2000 0.05 0.1 0.15 0.2 0.25

Stress [MPa] Strain [-]

Load cycle one Load cycle two Yield: 1544MPa Uniform elongation 4% Total elongation 8 % PTP device testing

  • P. Hosemann MRS JMR 2015
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MICRO TENSILE TESTING ON ION BEAM IRRADIATED 304SS

200 400 600 800 1000 1200 1400 0.1 0.2 0.3 0.4 0.5 0.6

Engineering Stress, σ [MPa]

Engineering Strain, ε

Irr P3 G2 Irr P2, G1 Irr P1, G1 Unirr P3 G2 Unirr P2 G1 Unirr P1 G1

G1 tests are all in the same grain G2 tests are all in the same grain Hi Vo, A. Reichardt unpublished data 2016

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NOT OXIDIZED (WITH CARBIDES) AND OXIDIZED GRAIN BOUNDARY

25 Oxidized grain boundary with carbide Unoxidized grain boundary with carbide

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MICRO BEND TESTING ON IRRADIATED MATERIALS

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MICRO 3 POINT BEND TESTING ON HIGHLY IRRADIATED REACTOR RETRIEVED MATERIALS

GS3-6 Low Temperature (Sxx) GS3-12 High Temperature (GB)

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TAKING IT TO THE NEXT LEVEL-NON AMBIENT CONDITION

In-situ Micro bending at 570°C on UO2; D. Frazer

Chilled nitrogen gas (in and out) gk Sample Cu wires for thermal contact Nano- indenter Nanoindenter Stage SEM Stage Cooling System Stage

In-situ Micro compression testing at -145C A. Lupinacci Acta Mat 2014 D. Frazer 2017 RT pillars

  • 145C pillars
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SUMMARY ON MICROMECHANICAL TESTING

Outline the importance and potential impact small scale mechanical testing can have to the nuclear materials community Indentation

n 10dpa appears to be the saturation dose after which no further hardening can be detected. n Hardness over temperature follows reasonably well the tensile data over temperature.

Micro compression testing

n Significant slip step differences can be found between irradiated and unirradiated materials. n An energy balance approach to quantify the slip steps is introduced. n Evaluation of fiber/matrix composites.

Micro tensile testing:

n A significant difference between the irradiated and unirradiated strain can be

  • bserved failure mode as well as quantitative numbers.
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Thank you for your attention!

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