2017-9/22 4th RaDIATE 1

PSI SINQ specimen PIE at JAEA-WASTEF

Shigeru SAITO, Nariaki Okubo, Shinya EndoTarget Technology Development Section, Transmutation Division, J-PARC Center, JAEAKazuhiro Suzuki, Yuuichi HatakeyamaDept. of Hot Laboratories and Facilities, JAEAKenji KikuchiFrontier Research Center, Ibaraki Univ.

Hot Laboratory of PSI

SINQ

2017-9/22 4th RaDIATE2

Content

1. Outline of STIP and MEGAPIE

2. Preparation for PIE-Transportation-Testing machine

3. PIE results at JAEA

4. Summary

1. Outline of STIP and MEGAPIE

To evaluate the lifetime of the beam window, STIP (SINQ target irradiation program,SINQ; Swiss spallation neutron source) at the SINQ target at the Paul ScherrerInstitute (PSI) was initiated in 1996 and has been progressing.

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Irradiation rod

Ring cyclotron

SINQ target

Irradiation rod and specimens

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Accelerator irradiation：・ Small irradiation volume,large gradient of temperatureand dose.・Large activation

Smaller specimens are usedcompare to fission reactorirradiation.

Irradiation have been done by replacing Pb-rod to the sample installed rod.

Small specimen testtechnique (SSTT)

Samples irradiated in STIP-I

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Materials ID TensileBend-fatigue

TEM Sum

1 JPCA-SA F 8 3 5 16

2 316F-SA G 13 5 7 25

3 316F-CW H 8 - 2 10

4 F82H P - 4 - 4

5 F82H TIG Q 7 4 6 17

6 F82H EBW R 8 4 4 16

7 F82H EBW* S - 4 - 4

Sum 44 24 24 92

JAEA samples

Irradiation :July 1998 to Dec. 1999Irradiation temp.：80 - 400℃Irradiation dose ：-12dpa

Y. Dai, et al., “Status of the first irradiation experiment, STIP-I”, J. Nucl. Mater. 296, 43-53 (2001).

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STIP-II

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Irradiation :March 2000 to December 2001Irradiation temp.：80 - 450℃Irradiation dose ：-20dpa

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Samples irradiated in STIP-II

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Hg and LBE capsule irradiation

Y. Dai, et al., “The second SINQ target irradiation program, STIP-II”, J. Nucl. Mater. 343, 33-44 (2005).

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Samples irradiated in STIP-II

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Samples transported to JAEA.Materials ID Tensile(S) Tensile(L) Bend-fatigue TEM Sum

1 JPCA D 27 9 12 10 58

2 Alloy800H E 20 9 12 9 50

3 Nb IA - - - 3 3

4 Ta IB 14 - 3 13 30

5 Cr IC - - 3 5 8

6 W/Nb(1Zr) ID - - 6 3 9

7 W/Ta IE - - 5 - 5

8 W/Cr IF - - 4 4 8

9 W IG - - - 5 5

10 W-TiC 4 - - 4 8

11 W-SUS 3 - - 5 8

12 W-Poly 4 - - 1 5

13 W-CVD 4 - - 0 4

14 W-Sin 1 - - 0 1

Sum 77 18 45 62 202

※Au, Pt, SiCf/SiC specimens were not transported to JAEA and PIE of the specimens were performed at PSI HL.

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STIP-III

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Irradiation :2002 to 2003Irradiation temp.： - 800℃Irradiation dose ：-20dpa

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Samples irradiated in STIP-III

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• No specimen was not transported to JAEA.

• PIE had been done at PSI HL.

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STIP-IV

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Irradiation : 2004 to 2005Irradiation temp.： - 600℃Irradiation dose ：-25dpa※High temperature experience due to over-focused beam size.PIE of limited specimens had been done.

Y. Dai, et al., “The fourth SINQ Target Irradiation Program, STIP-IV”, J. Nucl. Mater. 431, 2–9 (2012).

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MEGAPIE2006, MEGAPIE (MEGAwatt Pilot Irradiation Experiment)

-Irradiation experiment of LBE flowing target-Samples were cut from components and transported to each

institution.-JAEA has performed PIE of MEGAPIE samples.

Beam window Flow guide tube

H02-1 H03-2 H04-2

T91 SS316L Total

Tensile 9 8 6 23

TEM 12 10 8 30

Bend bar - - 8 8

OM 2 (Spitze) 0 4 6

Total 23 18 26 67

Spitze:triangle part

W. Wagner, et al., JNM. 377, (2008)12–16.M. Wohlmuther, W. Wagner, JNM. 431, (2012)10-15 .

Beam window

STIP-V~VIII

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• 2007-2008, STIP-V (No JAEA sample)• 2013-2014, STIP-VI (No JAEA sample)• 2015-2016, STIP-VII (No JAEA sample)

• 2018?, STIP-VIII-JAEA rod (T91 with/without LBE, F82H) will be installed.-Dismantling technique for LBE capsule and off-gas

processing apparatus.-Mechanical testing in LBE.

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2. Preparation for PIE Transportation of the irradiated samples

・Size and weight : Outer cask 1,300 X 1,000 X 1,030 (mm)Inner cask φ460 X 460 (mm)Inner container φ270 X 255 (mm)

・Weight : 1,250 kg (450 kg + 630 kg + 170 kg )・Shielding : 150 mm Pb (80 mm + 70 mm)・Inner space : φ100 X 80 mm

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Outer cask Sample containersInner container

Inner cask

PIE flow

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・Gas measurement(Hydrogen, Helium)NDC, NFD

・ Gas measurement （Tritium）

Lab. building No.4, TPL・Positron annihilation(Kyoto Univ., Kagoshima Univ.)

PSI

TEM

Electro-chemical etchingFIB (Focused Ion Beam)

Cutting SEM(Fracture surface)

βγ cell

Loading and Storage

αγ cell

Micro hardness test

OM/SEM (Cross section)

WASTEF RFEF

βγ cell

Tensile testBend fatigue test

•Mounting•Polishing•Etching

βγ room

Thinning

HITACHI HF-2000

HITACHI FB-2000a

JEOL JSM-5410

SHIMADZU HMV-1

Other facilities

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Tensile testing machine for STIP specimensS-size

CCD camera

Gold image furnace

Rod Robot arm

Specimen setting jig

Robot hand

Tensile test• Testing machine for small specimens• Test temperature :R.T., 250℃, 350℃• Environment :in air• Cross head speed :0.1-0.2 mm/min.• Measurement :Load, displacement,

strain (CCD camera) Fracture surface observation by SEM

L-size

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Load cellMarker

Specimen

Pin

Measurement window

Cursor

Tensile testing machine

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Bend-fatigue testing machine for STIP specimens

Bend-fatigue test• Testing machine for small specimens• Test temperature :R.T.• Environment :in air• Frequency :26Hz• Test ：Displacement Fracture surface observation by SEM

Auxiliary specimen

holder

Eddy-current displacement

meter

Piezoelectric-ceramic actuators

Specimen

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Specimen holder

Strain (ε11) distribution of the JPCA-SA specimen simulated by FEM.

2

13

3mm

Specimen holder

Loading point

S. Saito, et. al., JNM. 307-311, (2002) 1609-1612.

Bend-fatigue testing machine

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3. PIE results at JAEA- Tensile tests on austenitic steels-

• The YS increase of the proton irradiation increase shows a tendency to exceed the upper bound of the fission neutron data band at higher dose (>5dpa).

• Degradation of ductility on JPCA stopped around 10 dpa.• JPCA specimens irradiated up to 19 dpa still have ductility.• The results will be explained by the results of TEM observation.• All specimen fractured in ductile manner.

SS curve (RT） ΔYS vs dpa Ductility vs dpa

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S. Saito, et. al., JNM, 431, (2012) 44-51.

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Bend-fatigue tests on austenitic steels

• Similar to STIP-I results, the fatigue life of JPCA specimens irradiated at lower and middle dpa is almost the same as that of unirradiated specimens.

• The specimens irradiated at higher dpa show rather longer fatigue life.• Both unirradiated and irradiated JPCA specimen show the fracture surfaces of ductile

transgranular morphology. Brittle transgranular and intergranular surface are not observed.

Unirr. 150℃, 8.0 dpa 253℃,13.8 dpa 352℃,19.3 dpa

SN-curve（RT） Fracture surface (SEM)

2017-9/22 4th RaDIATES. Saito, et. al. JNM, 450, (2014) 27-31.

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Microstructural observationon austenitic steels

X 2

50nm

19.5dpa, 420℃1600appmHe

Dose (dpa) Avarage temp. (℃) Density (m-3) Size (nm)

5.7 150 - -

7.9 230 4.98×1023 3.0

10.1 285 1.21×1023 2.7

19.3 420 4.22×1023 1.8

densitysize

• He bubble formation on JPCA was observed at lower temperature comparedto fission reactor irradiated samples• There is small change in density and size of He bubble between 10-19 dpa.• He bubbles distribute homogeneously and precipitation of He is not observed.

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Tensile tests on heavy metals

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•Irradiation effect on W-alloys and pure TaSome specimens were broken before testing.Most of W-alloys and pure Ta fractured in brittle manner.W-single crystal specimen showed ductility after the irradiation.

•Un-irradiated specimens fractured before yield and shows brittle cleavage surface with no necking.•The specimen irradiated up to 7.1 dpa has ductility and its total elongation is 6%.•The irradiated specimen shows well-necked chisel edge surface and its RA is 78%.

S. Saito, et. al., Ghent, Belgium, IWSMT-11 (2012).

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Surface and cross sectional observation on MEGAPIE beam window

T91 Spitze(triangle part )

Cross section(SEM)

Inner surface (SEM)

20μm

No cracksaround the pits.

500μm

50μm

50μm50μm Corrosion?Large number of pits

Small number of pits

Top

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S. Saito, et. al., IWSMT-12, Bregenz, Austria, (2014).S. Saito, et. al., IWSMT-13, Chattanooga, USA, (2016).

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4. Summary

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• PIE of STIP-I, STIP-II and MEGAPIE samples have been performed at JAEA HLs.

• Cooperation with HL staff -Licensing, Transportation-Development of new testing techniques-Mock-up tests and final tests

• We could get useful and valuable data.

• These experiences were reflected to the design activity of TEF-T hot cells and PIE preparation for STIP-VIII samples.