Folie 1 - Indico

PWIE, SP B.3 NCSRD activities in 2021: analysis of reference and plasma-exposed samples – plans and capabilities

D. Mergia, A. Lagoyannis, P. Tsavalas, M. Axiotis

NCSR “Demokritos” (NCSRD)

PWIE

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Experimental capabilities for surface analysis of plasma

facing materials (1)

Ion Beam Analysis

Rutherford Backscattering Spectroscopy

(RBS)

Nuclear Reaction Analysis (NRA)

Particle Induced X-ray/Gamma-ray

Emission (PIXE/PIGE) spectroscopy

Time-of-Flight Elastic Recoil Detection

Analysis (ToF-ERDA) from early 2022

Milli- and micro-beam μ-B

eam

RBS , NRA, ERDA …

Charged-particle induced X-rays

Auger Spectrom.

Ato

mic

ph

ys

ics

multipurpose

scattering chamber 4 HPGe detect.

array γ - spectrometry charged-part.

irradiations

d-filled gas-cell

Tritiated Ti-target (rotating) n

eu

tro

n i

rrad

iati

on

s

γ - calorimetry

5.5 MV TANDEM Accelerator

Contact: Tassos Lagoyannis, [email protected]

New ion sources (TORVIS & SNICS II) to

be installed in early 2022 providing the

ability to use ions up to Iodine

Ion sources

Analyzing

magnet

Switching

magnet

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Chamber’s features: Load – lock chamber 3 – axis motorized sample holder Rotatable target holder Heating / Cooling Long range microscope for precision CCD camera for sample Monitoring

Detectors:

PIXE low energy Si(Li) detector at 45o

PIGE HPGe detector at 45o

STIM detector at 0o

RBS SSB detector at 170o

NRA SSB detector at 150o

Experimental capabilities for surface analysis of plasma

facing materials (2)

µ-beam Facility

Spatial resolution 1.2 μm x 2 μm

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Experimental capabilities for surface analysis of plasma

facing materials (3)

X-ray Fluorescence Spectroscopy (XRF)

Elemental analysis for Z>11

X-ray diffraction/reflectivity (XRD/XRR)

Normal and incidence angle

High speed linear position sensitive detector

In-situ studies from LN2 up to 1500C (XRD) or up to 800 C (XRR)

Scanning Electron Microscopy (SEM) with EDX spectroscopy

<1 nm resolution 0.2-30 kV (new FEG-SEM microscope purchase under way)

Transmission Electron Microscopy (TEM)

Atomic Force Microscopy (AFM)

X-ray Photoelectron Spectroscopy (XPS)

Mechanical properties using depth-sensing nano- & micro-indentation

XRF

XRD/XRR - furnace setup

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ILW-1

OPL

Enhanced erosion (>11 μm)

and deposited particles rich in

Ni are observed.

50 μm

50 μm

Ni rich Be rich

Be top layer became

thinner: erosion <11 μm

Comparison between ILW-1 and ILW-2

4D14

OPL

Be Tiles from JET tokamak: Erosion Combined NRA and SEM investigation

P. Tsavalas et al, Phys. Scr. T170 (2017) 014049

ILW-2

OPL 3.5 4.0 4.5

Inte

nsity (

Arb

. U

nits)

Energy (MeV)

Be

Bulk

Be

Top Layer Ni

Interlayer

Be Bulk

ILW-2 OPL

Reference

3.5 4.0 4.5

Be

Bulk Ni

Interlayer

Be

Top Layer

Be

Bulk

Inte

nsity (

Arb

. U

nits)

Energy (MeV)

Be

Top Layer Ni

Interlayer

ILW-1 OPL

Reference

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4 6 8 10

CuNiFeTi

Inte

nsity (

Lo

g A

rb. U

nits)

Energy (keV)

ILW-2 IWGL OUTER

ILW-1 IWGL OUTER

Reference

Ti Cr Mn Fe NiCu Zr W

0.01

0.1

1

10

100

Ti Cr Mn Fe Ni W

Rel

ativ

e C

on

c. (

at%

)

Element

ILW-1 DP

ILW-1 OPL

ILW-2 OPL

ILW-1 IWGL CENTRE

ILW-1 IWGL OUTER

ILW-2 IWGL OUTER

ILW-1 IWGL WING

Reference

40 50 60 70 80

ILW-1 IWGL WING

ILW-2 IWGL OUTER

ILW-1 IWGL OUTER

Reference

ILW-1 OPL

ILW-2 OPL

ILW-1 IWGL CENTRE

BeNi

BeO

Ni

Fe

Be

Inte

nsity (

arb

. u

nits)

2 (degrees)

DP

• Presence of BeO compound

• Formation of BeNi compound

Be Tiles from JET tokamak: Material deposition & compound formation

XRF & XRD investigation

XRD XRF

P. Tsavalas et al, Phys. Scr. T170 (2017) 014049

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Be castellated Tiles from JET tokamak Carbon deposition on the castellated sides - µ-beam NRA using a deuterium beam

4D14 2XR10

2B(C)2

DP

IWGL OPL

divertor

500 1000 1500

1000

500

0

012345678910111213

ILW-1 DP (80) C

500 1000 1500

1000

500

0

0

1

2

3

4

5

ILW-1 OPL (120) ILW-2 OPL (320)

ILW-1 IWGL outer (191)

500 1000 1500

1000

500

0

0

1

2

3

4

5

6

7

8

9

10

11

500 1000 1500

1000

500

0

0

8

16

24

32

ILW-1 IWGL outer (27)

500 1000 1500

1000

500

0

0

1

2

3

4

5

500 1000 1500

1000

500

0

01234567891011121314151617

ILW-1 IWGL centre (174) ILW-1 IWGL wing (76)

500 1000 1500

1000

500

0

0123456789101112131415

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NRA results from W lamellae – use of 2H micro-beam Carbon deposition

0 5 10 15 20 25 30 350.0

0.2

0.4

0.6

Depth (1018

at/cm2)

0.0

0.2

0.4

0.6

(ILW1) A23, 7

(ILW1) C3, 12 area 1 0.0

0.2

0.4

0.6

Ca

rbo

n C

on

ce

ntr

atio

n (

at%

) (ILW1) C3,12 area 2

0 2 4

1

10

100

1000

10000

100000

Inte

nsity (

co

un

ts)

Energy (MeV)

experimental

simulatedW(d,d)W

12C(d,p

0)

13C

16O(d,p

0)

17O

Pile up Be reactions

Sample 7

250 500 750 1000

250

500

750

1000(ILW1) A23, 7

250 500 750 1000

250

500

750

1000

(ILW1) C3,12 (2)

250 500 750 1000

250

500

750

1000(ILW1) C3, 12 (1)

Lamella Exp.

Period

Sample C Amount (1017 at/cm2)

Deposition

Thickness (1018 at/cm2)

C3 ILW1 12 (2) 24.8 10.7

C3 ILW1 12 (1) 166 33

A23 ILW1 7 2.21 10

ILW

1

ILW1

Measure

d surface

Measured

surface

Measured

surface

Investigation of carbon deposition &

carbon depth profile in W lamellae

from JET tokamak

P. Tsavalas et al. PFMC-18, 2021

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1000 2000 3000 4000 5000 600010

0

101

102

103

104

Inte

nsity (

co

un

ts)

Energy (keV)

data

simulation

9Be(d,p

1)

10Be

2H(d,p

0)

3H

12C(d,p

0)

13C

16O(d.p

0)

17O

9Be(d,p

0)

10Be

14N(d,a

1)

12C

(b)

NRA and XRD results from W/CFC Tiles from the JET divertor

NRA spectrum using a 2H beam

0 20 40 60 800

20

40

60

80

100

W

C

Be

D

O

N

Co

nce

ntr

ation

(at%

)

Depth (1018

at/cm2)

Tile 6

0 2 4 6 8 10

Depth (m)

20 30 40 50 60 70 80 90

G6C

G7A

G8B

Inte

nsity (

arb

. u

nits)

2(degrees)

C-CFC W

Mo Be

W2C C

G4D

XRD spectra

Absence of Be-W intermetallics that

could affect the thermomechanical

properties

A. Lagoyannis et al, Nucl. Fusion (2017) 076027 (7pp)

Assessment of

Fuel retention

Seeding species retention

Material migration

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Elemental mapping from W/CFC Tiles from the JET divertor

μ-PIXE mapping

C

Mo

O

W

SEM Images EDX Mapping

50 μm SE

Mo

O

W

Ni

100 μm

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2021 workplan

Analysis of reference and plasma exposed Be or W samples from the various devices

Problems to be addressed

• Material deposition, depth profiles, compound formation

• Erosion

• Fuel retention

• Seeding species retention

• Microstructural changes

• Mechanical properties using depth-sensing indentation techniques

In-situ XRD annealing of plasma exposed samples to assess

i) temperature effects on compound formation due to material deposition

ii) microstructural changes.

Samples to be identified and specific problems to de defined

Suggestions for collaborations welcome (please send an email to [email protected] to discuss)

D007 RBS, SEM, XRD and XRF characterization of selected Be reference coatings and plasma-exposed

samples