Investigation of Deuterium Permeation and Retention in ...44 Materials Temperature Thickness l...

48
H.-S. Zhou, H.-D. Liu, Y.-P. Xu and G.-N. Luo Fusion Reactor Materials Science and Technology Division Institute of Plasma Physics, CAS, Hefei, China ASIPP EAST CFETR Investigation of Deuterium Permeation and Retention in RAFM Steel The 3 rd Research Coordination Meeting of the CRP on Plasma-wall Interaction with Reduced- activation Steel Surfaces in Fusion Devices, 25 - 27 March 2019, IAEA Headquarters, Vienna

Transcript of Investigation of Deuterium Permeation and Retention in ...44 Materials Temperature Thickness l...

Page 1: Investigation of Deuterium Permeation and Retention in ...44 Materials Temperature Thickness l Diffusivity D Diffusion time l2/D K m m2s-1 s CLF-1 600 6.9×10-4 4.4×10-9 108 W 600

H.-S. Zhou, H.-D. Liu, Y.-P. Xu and G.-N. Luo

Fusion Reactor Materials Science and Technology Division Institute of Plasma Physics, CAS, Hefei, China

ASIPP

EAST CFETR

Investigation of Deuterium Permeation

and Retention in RAFM Steel

The 3rd Research Coordination Meeting of the CRP on Plasma-wall Interaction with Reduced-

activation Steel Surfaces in Fusion Devices, 25 - 27 March 2019, IAEA Headquarters, Vienna

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– Motivation • RAFM as first wall of TBM in ITER

• T permeation issue

– PMI studies on RAFM • D plasma-driven permeation through RAFM

• He effects on sputtering and D retention

• D PDP through PFC mockup made by RAFM

– Summary

Outline

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Outline

Motivation

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Chinese Helium Cooled Ceramic Breeder TBM

RAFMs will be used to fabricate the first wall of ITER TBM (~mm thickness).

K.M. Feng et al., FED 89 (2014) 1119

Tritium breeding blanket concepts

will be tested in ITER.

The helium-cooled ceramic breeder

(HCCB) test blanket module (TBM) is

the primary option of the Chinese

TBM program.

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H particle flux to the wall

H flux (H m-2s-1) Energy (eV) Temperature

First wall 1020-1021 ~100 eV ~500 C

After R. Behrisch and A.S. Kukushkin et al.

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T permeation through the first wall

60x1015

40

20

0

P

DP(H

/m2/s

)

100806040200

Time (s)

Shot: 3188 - 3197 H2_3188 (87.4 kW)

H2_3190 (79.2 kW)

H2_3191 (69.1 kW)

H2_3192 (58.4 kW)

H2_3193 (48.1 kW)

H2_3194 (37.4 kW)

H2_3195 (27.9 kW)

H2_3196 (19.0 kW)

H2_3197 (11.4 kW)

H2_3189 (4.65 kW)

After S. Sharma et al.

Knowledge learned from QUEST permeation experiments

Un-confined neutral H

particles can go to

anywhere in the

vacuum vessel and induce H permeation!

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Outline

Plasma driven permeation of

D through a Chinese reduced

activation martensitic/ferritic

steel CLF-1

H.D. Liu et al., J. Nucl. Mater. 514 (2019) 109-113.

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Sample preparation and experiments

Materials: 0.75 mm RAFMs membrane, polished

Experiments:

Methods Plasma-driven permeation (PDP) Gas-driven permeation (GDP)

Purpose Surface effects Permeation parameters

measurements

(wt %) C Si Mn Cr Ni Mo W Ta V Nb Al N P

CLF-1 0.12 <0.05 0.51 8.50 <0.01 <0.01 1.5 0.10 0.25 <0.01 <0.03 0.0067 <0.005

The authors would like to thank Profs. K.M. Feng and Y.J. Feng from SWIP for providing CLF-1.

GDP permeability and diffusivity

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The PREFACE facility

9

Permeation and Retention Evaluation FACility for

fusion Experiments (PREFACE) at ASIPP

Facility parameters:

Max. ECR power: 2 kW

ne: 1014 -1017 m-3

Te: 3-6 eV

Ion flux : 1018 - 1021 m-2s-1

Thermo

couples

Probe

ECR plasma

source

QMS for PDP

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Plasma-driven permeation setup

CLF-1 sample for

PDP studies

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H. Zhou et al., J. Nucl. Mater. 493 (2017) 398

H. Zhou et al., Nucl. Fusion 58 (2018) 056017

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Steady-state PDP model

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• RR

• RD

• DD ip

RJ J

L

ip

up

JDJ

L K

i

up

p

up d

KJ J

K K

B. L. Doyle, JNM 111&112 (1982) 628.

R: recombination D: diffusion

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Permeation flux vs incident flux

12

0 4000 8000 12000 16000

1017

1018

Perm

eati

on

flu

x (

D m

-2 s

-1)

Time (s)

Permeation flux

550

600

650Plasma off

Power=650 W

Te=2.6 eV

ne=1.4E16 m-3

Power=500 W

Te=2.5 eV

ne=7.0E15 m-3

transient peak

Power=200 W

Te=6.0 eV

ne=6.0E14 m-3

Plasma on

The incident flux is controlled by changing ECR input power.

3

0

1

(1 R ) N (T T )=

2

j

j j e i

j D

j kJ

m

*H. Zhou et al., FST 63 (2013) 36.

*

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Permeation regime

13

1018

1019

1018

Pe

rme

ati

on

flu

x(D

m-2 S

-1)

Permeation Flux

Fitting line

Implantation flux (D m-2 s

-1)

0.47p iJ J

Permeation takes place in the recombination-diffusion regime.

Estimate the permeation flux for TBM.

• RR

• RD

• DD ip

RJ J

L

ip

up

JDJ

L K

i

up

p

up d

KJ J

K K

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Bias effects

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Cleaner surface, lower permeation flux*

Higher recombination at front surface

*H. Zhou et al., JNM 463 (2015) 1066

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Permeability and diffusivity of CLF-1

Both D permeability and diffusivity in CLF-1 are close to those of F82H.

Diffusivity + RD model

Permeability (P) Diffusivity (D)

15

ip

up

JDJ

L K

upK

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Upstream recombination coefficients (Kr)

Assuming PDP takes place in RD regime, Kr are estimated from

permeation model.

D has higher Kr than H. 16

1.3 1.4 1.5 1.6 1.710

-27

10-26

10-25

10-24

10-23 (K)

Reco

mb

inati

on

co

eff

icie

nt

(m4/s

)

1000/T (K-1)

0 V D,CLF-1

-50 V D,CLF-1

-100 V D,CLF-1

-100 V H,F82H

750 700 650 600

Larger mass, better cleaning effects?

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Evaluate T breeding ability of TBMs?

ITER fusion power: 500 MW T TBR: 1.3 Surface area: 700 m2

T produced in per m2 blanket: 3.3×1017 T/s

0.75 mm CLF-1 (D data)

Permeation flux may be comparable with the T breeding rate…

5 mm F82H (H data)

Y. Hirooka, H. Zhou et al., FST 64 (2013)345

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Evaluate T breeding ability of TBMs?

ip

up

JDJ

L K

For RAFMs, the Kr estimated from existing model is so scattered.

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Outline

Surface erosion of F82H by

He-plasma exposure

Y.-P. Xu et al., Nucl. Fusion 57, 056038 (2017)

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Facilities

STEP in Beihang University

(Simulator of Tokamak Edge Plasma)

Exposure condition

Ions: He

Flux: ~1.8×1022 He/m2/s;

Ions energy: ~80eV;

Sample Temperature: 773 K–873 K;

F82H before exposure

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Surface morphology after plasma exposure

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Cross-sections SEM images

1×1025 He/m2 sample

Voids with different sizes and shapes can be found in the sample in a depth up to 3.5 μm.

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Cross-sections EDS mapping

The tendrils are enriched in W. The enrichment of W can be explained by preferential

sputtering between low-Z and high-Z materials with He particles.

1×1025 He/m2 zone

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EAST plasma exposure

Samples

EAST material and plasma evaluation system (MAPES)

Time: 2015 spring;

Shots: 56564-56994(367 shots);

Exposure time: 2005.296s;

Plasma condition:

Te=5-10 eV, ne=~1×1018 m-3;

Sample temperature:323-623 K。

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Sample after EAST plasma exposure

SEM images of the center of the sample after exposure to He plasma to a central fluence of 4×1025

He/m2 and 367 D plasma pulses of varied durations in EAST

After exposure to D plasma in EAST, the tendril-like features with a maze-like

pattern were cracked, part of tendrils collapsed to the bottom of the ridges while

part of tendrils were missing.

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Outline

He effects on D retention

H.-S. Zhou et al., Nucl. Fusion 58, 056017 (2018)

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He effects on H transport (1)

Sample No.

DPA Peak value

1 0.001

2 0.01

3 0.05

Experimental results:

The permeability and diffusion coefficient of CLF-1 steel decreased after high dose He ion irradiation.

Permeability Diffusion coefficient

RAFM steel

D2 gas-driven permeation

3.5 MeV He ion

irradiation

Our previous permeation experiments for RAFMs after energetic He

ion irradiation: Y.-P. Xu, H.-S. Zhou et al., NIMB, 2016.

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He effects on H transport (2)

In this work, we try to investigate D retention behavior in

RAFMs by separating the effects of surface conditions,

bulk damage and He bubbles.

He pre-damage

Available literature data:

H/D loading

Accelerator

Ion gun

Plasma

Energy range:

~ eV–0.8 MeV

Accelerator

Ion gun

Plasma

Energy range:

~ eV – 0.3 MeV

Increase?

Decrease?

Irradiation damage?

Surface condition?

He effects?

H/D retention

measurement

e.g. IBA

TDS

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Experimental

3.5 MeV He+

RAFM steel

Thermal desorption

D plasma exposure

Energy degrader

4.5 MeV Fe2+

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High energy ion injection

4.5 MV electrostatic accelerator

Accelerators at Peking University

2x1.7 MV tandem accelerator

He+ ion energy: 3.5 MeV

Sample temp.: R.T.

He implantation

He/m2

dpa peak value

He peak concentration

He/m3

6×1017 0.001 1.88×1024

3×1019 0.05 9.373×1025

Fe2+ ion energy: 4.5 MeV

Sample temp.: R.T.

Fe implantation ions/m2

dpa peak value

8×1016 0.013

4×1017 0.066

4×1018 0.66

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Material damages predicted by SRIM 3.5 MeV He in RAFMs

4.5 MV electrostatic accelerator

Accelerators at Peking University

2x1.7 MV tandem accelerator 31

4.5 MeV Fe in RAFMs

Range: ~6.1 μm

Range: ~1.2 μm

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Plasma exposure in PREFACE

Plasma parameters in this work

Te: ~2 eV

ne:(1-1.5)x1017 m-3

Ion fluence: ~ 6x1023 D m-2

Sample temp.: 280 oC

Te and ne profiles (~360W ECR) Te and ne as a function of D2 gas

pressure (~360W ECR)

32

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Surface damage by shifting dpa peak

Energetic

He ions

13 μm or 2 μm

Al foil

RAFMs

RAFMs

“Surface” damage

“Bulk” damage

33

SRIM-2008: 3.5 MeV He in RAFMs

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He bubbles in RAFMs

TEM after irradiation by 3.5 MeV He+ (without Al foil)

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He bubbles in RAFMs

TEM after irradiation by 3.5 MeV He+ (with Al foil)

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D retention

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A short summary

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Knowledge from retention & permeation studies on RAFMs

D in W

Retention from

postmortem

measurement

D retention does not increase after extended plasma exposure.

D can perpetrate 1 mm thick RAFMs within tens of seconds.

W. Jacob, IAEA steel

CRP meeting

Permeation data

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thickness

+ =

0 H in solution site

C C

Almost

completely

released

When plasma is on:

When the plasma is off:

Plasma

side

D in W

D retention in RAFMs: retention saturation?

No new

traps,

no more

retention.

thickness 0

Trapped H

e.g.

dislocation,

GB, vacancy

0

C

thickness

Total H

retention

Trapped H

thickness 0

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thickness

+ =

0

C C

When plasma is on:

When the plasma is off:

Plasma

side

Trapped H H in solution site

Barrier Barrier

vs.

Speculation: in the presence of a barrier

thickness 0 0

C

thickness

Total H

retention

C

Trapped H

Barrier

thickness 0

Trapped H

thickness 0

None

Barrier

case

C

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Outline

D PDP through PFC mockup

made by RAFM

H.S. Zhou et al., Nucl. Fusion 59 (2019) 014003

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Motivation

Large surface area Thick W armor

Small area fraction for gaps Thin structural material

Permeation speed?

Permeation flux?

Gap effects have been widely studied in erosion/deposition studies.

How about permeation through the gap?

Intuitive image Reality Neutrals from

(i) plasma and

(ii) flection on wall

will impinge on the heat sink.

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PFC mock-up

Key points of the mock-up:

― W bulk: 8 mm the thickness;

― Gaps: 0.5 mm wide, made by electrospark wire cutting;

― Angle between the gaps and magnetic field lines: 5o

(after R. A. Pitts)

Electron density: ~5×1015 m-3

Electron temperature: ~5 eV

Implantation flux: ~5×1019 D m-2s-1

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Materials Temperature Thickness l Diffusivity D Diffusion time l2/D

K m m2s-1 s

CLF-1 600 6.9×10-4 4.4×10-9 108

W 600 8.0× 10-3 2.2× 10-10 [2] 2.9× 105

0.06 Pa D2 gas for plasma discharge. No

gas-driven permeation can be detected.

Significantly enhanced D permeation

has been recorded when D plasma is on.

We confirm:

D can transport through the mock-up

without passing through W because the

8 mm thick W cannot be penetrated by H

diffusion.

[1] Xu Y.P.et al., NIMB 388(2016) 5

[2] R. Frauenfelder et al., JVST 6 (1969) 388

H permeation through gaps is fast

0.69 mm thick CLF-1 membrane

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(0.05 mm)

(0.75 mm) (0.23 mm)

The permeation data are normalized to the same membrane

thickness, assuming the permeation is recombination-diffusion

limited (B. Doyle, JNM 111&112 (1982) 628).

Steady-state permeation flux through CuCrZr is about one order of

magnitude higher than that through W under the same incident flux

and membrane thickness.

Permeation data normalized to 1 mm

0

r

DJ

l

J

K

Assuming R-D limited

Comparison of PDP for W and structural materials

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Comparison of PDP for W and structural materials

Assuming:

5% surface area fraction;

Incident flux 1×1024 Dm-2s-1

0

r

DJ

l

J

K

ITER divertor case:

After taking into account the surface area coverage (5%), steady

state D PDP flux through CuZrCr is still one order of magnitude

higher than that through W.

The first wall should have the same problem.

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Z.-X. Sun et al., FED 121 (2017) 60

The washer did not show any adverse effects on the performance in

HHF test .

IDTF test

organized by ITER IO

5000 cycles@10MW/m2 + 300 cycles@20MW/m2

One feasible solution to the problem (EAST way)

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Summary

Thank you for your attention!

H permeation and retention in RAFM steel under plasma exposure

conditions have been intensively investigated at ASIPP.

H transport parameters (including Kr) in RAFM have been evaluated

by experiments.

He has significant effects on surface morphology and H behavior.

Structural materials may be a “short cut” of T permeation for

existing PFC design of DEMO. PWI on RAFM steel should be

investigated in a systematic manner even if they are not directly

exposed to plasma.

Our recent interests: surface condition effects, permeation barrier…

This work is supported by the National Natural Science Foundation of China (No. 11505232), the

National Magnetic Confinement Fusion Science Program of China (No.2015GB109001)