ANALYSIS OF PLASMA FACING MATERIALS IN CONTROLLED FUSION DEVICES. Marek Rubel

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ANALYSIS OF PLASMA FACING MATERIALS IN CONTROLLED FUSION DEVICES Marek Rubel Alfvén Laboratory, Royal Institute of Technology, Association EURATOM VR, Stockholm, Sweden

Acknowledgements Paul Coad and Guy Matthews Jari Likonen Volker Philipps and Peter Wienhold Tetsuo Tanabe Nikolas Bekris and Ralf-Dieter Penzhorn

STRUCTURE OF THE TALK What is to be analysed? Why is it to be analysed? How is the analysis carried out?

What is to be analysed? 2003 Toroidal belt pump limiter Poloidal limiters A large number of: limiter plates divertor plates other wall components optical components instrumented tiles long-term probes short-term probes 1999-2001 2002-03. 2004 [At least tiles from one poloidal cross section.]

Layers of Re-deposited Material Tiles of a toroidal limiter Cross-section of a re-deposited layer Erosion zone Deposition zone ~ 43 μm Flaking re-deposited layer

EROSION BY MELTING Beryllium antenna screen at JET T m (Be) = 1278 o C Limiter from FTU TZM coated with 2 mm VPS Tungsten T m (W) = 3683 o C

Atoms to be Analysed in Re-deposited Layers FUEL Z = 1 (H D T ) PLASMA IMPURITY ATOMS: Eroded species Z > 2 For instance: Li Be 10 B 11 B 12 C 13 C 14 C Si Ni Cr Fe Mo W Re

We are to answer some basic questions! What has happened? Why has it happened? How to deal with the problem? We are paid NOT only to find and emphasize problems but TO FIND AND PROVIDE SOLUTIONS.

How?? ANALYSIS Methods, selected Results & Instrumentation

ION BEAMS for Material Characterisation SURFACE BULK

Methods Based on Ion Surface Interactions MODIFIED SURFACE and SUB-SURFACE REGION

Collisions & Scattering Projectile Detector Detector Projectile Target atom Target atom RBS & (EPS) ERDA & (HI-ERDA)

Kinematic Factor k p is unique for a given M p -M r combination: unambiguous determination of a given mass in the spectrum for a given M p mass separation decreases for increasing M r. better separation of larger M r with heavier M p only target atoms heavier than projectiles can be determined for M p M r only forward scattering possible k p increases with Θ. better detection at large scattering angles.

Efficiency in RBS: Differential Cross-section (Θ, M p, M r ) σ p Ω cross-section solid angle in detection system Z p, Z r atomic numbers Important: For a given projectile σ p scales with (Z r / E 0 ) 2 higher sensitivity for heavy elements and at lower E 0.

Rutherford Backscattering Spectrum ( 4 He + beam): Elements Co-deposited on Graphite PFC Backscattering yield (counts) Number of counts 250 0 C (substrate) O Ne DEPOSIT Si Inconel (Ni + Cr + Fe) Channel number Mo 100 400 N O = 10 17 cm -2 N Si = 10 15 cm -2 N Mo = 10 14 cm -2 Good separation of low masses, poorer for medium and high. No detection of deuterium with a 4 He + beam. Very difficult (not possible) to detect co-deposited boron on the graphite target. High sensitivity for heavy elements.

There is no free parameter left. RBS is an absolute quantitative method. No standards for calibration are required.* Quantification N t = A/σ Ω Q N t A Q σ p Ω Z p, Z r concentration of species number of counts in multi-channel analyser ion dose measured by current integrator cross-section solid angle in detection system atomic numbers All parameters in the system are directly measured (Q, A) and independently calculated (Ω, σ) knowing the scattering geometry, detector active area, atomic masses and numbers.

NUCLEAR RESONANCE & ENHANCED PROTON BACKSCATTERING: C-13 Resonance and C-12 enhanced scattering Carbon transport studies by tracer techniques 97 % 12 C(p,p) 12 C 13 C(p,p) 13 C d(p,p)d D Al substrate 3 % Al Gas inlet hole Very good separation of small masses (but hopeless for high). High sensitivity for low-z (not attainable with a 4 He beam).

3 He(d,p) 4 He Q = 18.3636 MeV Detected particle: proton 11 14 MeV range Proton spectrum can be converted into a deuterium depth profile. CROSS SECTION dσ/dq [mbarn/sr] Cross- section versus energy E th 3 He ENERGY [MeV] 3 He ENERGY [MeV] Information depth in C matrix

Nuclear Reaction Analysis depth profile of deuterium in a flake from the ALT II tile 3 He beam 1.8 MeV PROTON YIELD (counts) Layer Structure and D concentration: 9 x 10 17 D at μm -1 = 9 x 10 21 D at / g C D/C = 0.1

Deuterium Depth Profiles in Plasma Facing Components Deposition zone Erosion zone

MATERIAL MIGRATION STUDIES: TRACER TECHNIQUES Probe How is carbon transported and where is it re-deposited? How to answer these questions? Controlled injection of 13C tracer. 1.4x1017 Hf 4.5x1021 B Analysis of tiles to quantify the amount of 13C tracer re-deposited in different locations. 4.29x1023 13C at

Why accelerator-based IBA techniques? Summary Efficiency: Combination of various techniques in one system. Analysis of many elements and isotopes in the same system. Relatively quick analysis over large areas. Sensitivity & Selectivity & Quantification (no standards). Neither special sampling nor sample preparation needed. Depth profiling (limited in some cases). Chemical state of atoms is of secondary importance.

SIMS Analysis of Tracer Experiment: Depth Distribution of Re-deposited 13 C 10 5 Intensity (cps) 10 4 10 3 10 2 10 1 12 C 13 C 10 0 0 10 20 30 40 50 Depth (μm) Message: vast amount of C-13 is found in a thin surface layer (< 2 μm). Question: Why are the carbon profiles hollow?

SIMS: Depth Distribution of Species 10 5 9 Be 2 H Intensity (cps) 10 4 10 3 10 2 10 1 9 Be 12 C 13 C 10 0 0 10 20 30 40 50 Depth (μm)

Secondary Ion Mass Spectrometry: Advantages and Limitations Ultra-high sensitivity. Unbeatable in qualitative analysis. Depth profiling. Poor quantification because of matrix and crater effects.

TRITIUM ANALYSIS LIQUID SCINTILLOGRAPHY (LSC) OF TRITIATED WATER IMAGING PLATE (IP) BETA-INDUCED X-RAY SPECTROSCOPY (BIXS)

JET Divertor: Tritium retention after D-T Operation Inner wall 7.6 Outer poloidal limiter 18.7 How was the analysis performed? 198.0 1 1.7 2 3 0.4 0.7 10.8 1.1 5 6 0.2 4 7 0.4 0.9 7.3 0.8 5.1 T Content in TBq 8 9 10 JG98.115/4c Coring Full combustion Liquid scintillography of Q 2 O Q 2 = DT, HT, T 2 R-D Penzhorn, N Bekris, FZK, Karlsruhe

Sampling and Analysis Example of a divertor tile TRITIUM: Full combustion LSC of Q 2 O D, Be and C: NRA with a 3 He + beam The aims of sampling: Reduction of total radioactivity to be handled in further studies Comparative analysis of D and T

Imaging Plate Technique for Tritium Analysis Tritium on the divertor plate from JET Shadowed area Exfoliated area 0 PSL intensity[psl/mm 2 ] 800 600 400 200 1000 1200 1400 Courtesy: Tetsuo Tanabe, Kyushu University, Japan Back side of exfoliated layer

INSTRUMENTATION

INSTRUMENTATION FOR ANALYSIS OF PFM Accelerator Analysis chamber with detectors Targets

Instrumentation: Analysis chamber

d = 330 mm Analysis chamber Vertical manipulator: Vertical travel Z= 250 mm Limitations: sample size: < 145 x 250 mm sample weight: 1 kg 2.5 MeV Beam: 1 H +, 3 He +, 4 He + NRA RBS ERDA h = 450 mm Horizontal manipulator for semi-spherical samples: Weight limit: 20 kg PIXE

Instrumentation: Limiter manipulator Weight: 23 kg Capabilities: Probes up to 20 kg Rotation X and Y: 180 o Positioning: ± 50 μm

MATERIAL TRANSPORT STUDIES: TRACER TECHNIQUES and COLLECTOR PROBES Probe BN 1.4x1017 Hf Si targets 4.5x1021 B Collector probe before and after exposure 4.29x1023 13C at

Concluding Remarks: Overview of Material Migration in JET Mach Probe This picture is based on: Tile analysis QMB Deposition Chemical Erosion Net Erosion: physical & chemical Tile analysis Tracer injection experiments Probe measurements Quartz micro-balance data Limited Physical Erosion and Deposition

Simple concluding remarks and recommendations Use a relevant set of methods for solving a given problem. NEVER EVER claim that MY METHOD solves all problems (possible and impossible). Cross-check your results! There is NO single method that can answer all questions but there are methods that can provide answers to specific questions. CO-OPERATE!!

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