Thomas Schwarz-Selinger Max-Planck-Institut für Plasmaphysik, Garching, Germany
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1 Deuterium retention and isotope exchange studies in self-ion damaged tungsten exposed to neutral atoms Project: Hydrogen retention in self-damaged and Heirradiated tungsten and alloys for PFC Sabina Markelj, Anže Založnik, Primož Vavpetič, Mitja Kelemen, Primož Pelicon, Iztok Čadež Jožef Stefan Institute, Jamova cesta 39, 1000 Ljubljana, Slovenia Thomas Schwarz-Selinger Max-Planck-Institut für Plasmaphysik, Garching, Germany Olga Ogorodnikova National Research Nuclear University- MEPhI, Moscow, Russia This work was supported and carried out within the framework of the European Fusion Development Agreement and EUROfusion Consortium.
2 Outline The accelerator facility Motivation Study of D retention in self-ion damaged tungsten D atom loading at different sample temperatures Study of defect annealing + D atom loading Experimental set-up for in situ NRA and ERDA measurements Isotope exchange in bulk in self-ion damaged tungsten Preliminary results on simultaneous W ion irradiation and D atom loading Conclusion 2
3 Introduction - The accelerator 2 MV HVEE Tandem accelerator Tandetron, Jozef Stefan Institute, Ljubljana 3
4 Ion beam studies at JSI - The accelerator Multicusp ion source enabled duoplasmatron source to be permanently configured for He beam analysis by 4 He or 3 He for NRA. 3 He consumption optimized by construction of 3 He/ 4 He gas mixing set-up. Broad beam NRA set for static and in situ D depth profile measurements and experiments and micro beam NRA for startic measurements. Separate smaller experiment for fusion research: Vibrational spectrometer for hydrogen molecules atom recombination studies 4
5 Motivation GF Matthews, PSI 2013 Study of deuterium retention in selfion damaged tungsten Tungsten is the material of choice for divertor target plates Retention studies in damaged tungsten simulate neutron damage by W ion irradiation D retention - a way to determine the trap concentrations Gentle exposure to damaged W Study processes with hydrogen/deuterium atoms (0.2 ev) no additional defect production as in the case of plasma/ion exposure 5
6 Processes: atoms versus ions Proceses: neutral atom exposure versus ion/plasma exposure Effect of neutrals in plasma experiments don t play major role? Diffusion Trapping Ions > few ev Atoms H(g) E H-Me Potential energy Parameters for W ½ D e = 2.25 ev E ch = ev E des =2E ch Q s =1 ev ½ D e E s E diff ½ H 2 (g) physisorption E ch Q s E trap Distance From surface E barr Q s +E ch +E s E diff =0.39 ev E trap = ev chemisorption surface bulk 6
7 Damaged W + D atom different exposure temperatures 7
8 dpa Neutron-like damage - W ion irradiation W samples - mirror polished polycrystalline tungsten (at IPP), manufactured by Plansee GA - large grains perpendicular to sample surface (ITER grade) Damaging at room temperature at IPP, 20 MeV W ions, fluence 1.4x10 18 W/m dpa 2.4 mm Calculation by SRIM irradiation by 20 MeV W + F=1.4x10 18 W/m dpa ( 0.45 dpa) O.V. Ogorodnikova, H workshop (2012) ScanningTransmission Electron Microscopy (STEM) od W [L. Ciupinski et al. NIM B 317 (2013) 159] Calculation of damage profile by SRIM is in very good agreement with TEM observation 0.5 W, E th =90 ev depth, mm 8
9 Hydrogen atom beam source D 2 K.G. Tschersich, J.P. Fleischhauer and H. Schuler, J. Appl. Phys. 104, (2008); HABS D atom flux density profile D/D2 Sample Heater Maximum atom flux = 3.5x10 19 D/m 2 s Different exposure temperatures 9
10 Damaged W + D atom different exposure temperatures Deuterium depth profiles measured by Nuclear Reaction Analysis - NRA Analyzing protons ( 12 MeV) from nuclear reaction D( 3 He,p) 4 He at different 3He energies from 650 (500) kev up to 4.5 MeV Different exposure temperatures different saturation levels At lower temperatures higher fluence needed to saturate traps 10
11 Deuterium release rate, 10 D concentration, at.% 19 D/m 2 s TDS spectra (heating rate 2K/s) [ Yu. Gasparyan et al. JNM 463 (2015) 1013] higher temperature less D inside Small peak shift Fill level dependent de-trapping energies [Fernandes et al. Acta Mater. 94 (2015) 307, Schmidt et al. JAP 2014] 10 Damaged W + D atom different exposure temperatures 8 6 alf=2 K/s 600 K 2x10 24 D/m K 3,78x10 23 D/m atoms 0.2 ev K 700 K K K x10 23 D/m x10 23 D/m Temperature, K Yu. Gasparyan et al. JNM 463 (2015) Depth, mm O.V. Ogorodnikova, H workshop (2012) 11
12 Damaged W + D atom different exposure temperatures - comparison Comparison to with plasma loading PlaQ - 20 ev ion energy (IPP) Exposure at different sample temperatures O. Ogorodnikova et al. in preparation 12
13 Annealing of damaged W + D atom the same temperature 13
14 Damaged W material the annealing study W samples prepared at IPP - mirror polished polycrystalline tungsten, manufactured by Plansee GA grains parallel to surface (MF reference material ) Recrystallization 2 K Damaging at room temperature, 20 MeV W ions, fluence 7.8x10 17 W/m dpa 2 µm STEM analysis by L. Ciupinski collaboration within EUROfusion A. Založnik et al., PFMC 2015, submitted to Phys. Scripta 14
15 Damaged W material the annealing study D 2 HABS Sample Temp. 1 h hold Time Sample Heater D/D 2 Sample Heater 500 K for 144 h D central flux density 2.6x10 19 Ds -1 m -2 15
16 Study of defect annealing Depth profiles Long exposure time/fluence (6 days-144 h) needed to saturate traps intermediate NRA measurement after 72 h of D atom exposure (final depth profiles shown). Observed effect of the annealing of damaged samples on the trap concentration reduction of traps at higher annealing temperatures A. Založnik et al., PFMC 2015, submitted to Phys. Scripta 16
17 Study of defect annealing Depth profiles Long exposure time/fluence (6 days-144 h) needed to saturate traps intermediate NRA measurement after 72 h of D atom exposure (final depth profiles shown). Observed effect of the annealing of damaged samples on the trap concentration reduction of traps at higher annealing temperatures 17
18 Study of defect annealing total amounts Reduction of total D amount by 60% from 52x10 19 D/m 2 at 500 K to 21x10 19 D/m 2 at 1200 K Comparison with plasma loading PlaQ floating potential ( K, fluence 1x10 25 D/m 2-70% reduction of total amount Difference in maximum concentration D thermal detrapping different fluxes [ E. Markina et al. JNM 463 (2015) 329 ] 18
19 Study of defect annealing total amounts TDS TDS performed at IPP heating rate 15 K/min Comparison of reduction of total amount NRA vs. TDS in good agreement Between K single vacancies become mobile and form larger defects or annihilate stage III Annealing between 800 K and 1000 K intermediate recovery region Between 920 and 1220 K large vacancy recovery stage IV [L.K. Keys and J. Moteff, JNM 34 (1970) 260] [H. Schultz Mater. Sci. Eng. A141 (1991) 149] A. Založnik et al., PFMC 2015, submitted to Phys. Scripta 19
20 Defect annealing versus D exposure at high temperatures Significant decrease of D retention when exposure at higher temperatures 90% decrease ( K) Thermal D desorption is the dominant process at elevated temperatures Defect annealing Exposure at higher temperatures 20
21 In situ studies by ERDA/NRA The isotope exchange Wikipedia: IN SITU is a Latin phrase that translates literally to on site or in position. 21
22 In situ studies by Ion Beam Methods In situ = Hydrogen/Deuterium concentration measured during the exposure, annealing,.. No transport trough air between sample exposure and analysis Possibility to study the dynamics of processes on the surface and in the bulk Measurements of all parameters - computer control of the system Possible beam effect on retention 22
23 The isotope exchange process Process where one isotope is exchanged by the other. The purpose of this is to study the efficiency of the process on the surface and in bulk as cleaning method to reduce amount of tritium in the walls in fusion device during operation. Langmuir-Hinshelwood Eley-Rideal VACUUM VACUUM D METAL D METAL Hot-Atom CONTROL T S CONTROL Isotope exchange is a well studies surface science process, where adsorbed atoms on the surface are abstracted by incoming free atoms, the so called Eiley-Rideal or Hot-Atom recombination mechanisms. T S 23
24 In situ ERDA measurements 7 Li H, D, (He) 24
25 In situ ERDA measurements Typical mean atom flux density at the beam position was for D 6.4x10 18 at.m -2 s -1 and for H 1.0x10 19 at.m -2 s
26 Isotope exchange on surface - ERDA Isotope exchange study Measurement of both H and D One can study surface processes ERDA method not sensitive enough for bulk D signal in undamaged W exposed to D atoms close to detection sensitivity Markelj et al. JNM 438 (2013) S
27 Isotope exchange on surface - modelling Markelj et al. Submitted to JNM - under review 27 ] ][ [ ] [ 2 ] [ ] [ 2 H s D s d D s d D s exc H D S c c k c k c dt c d ] ][ [ ] [ 2 ] [ ) ]/ [ ]/ [ )(1 (1 ] [ 2 H s D s d H s d H s exc H o D s o H s r H H s c c k c k c N c N c P dt c d σ 480 (H D)=1.2± m 2, P r480 (H D)=0.94±0.2 σ 480 (D H)=1.7± m 2, P r480 (D H)=0.88±0.05 σ 380 (H D)=0.9± m 2, P r380 (H D)=0.74±0.15 Isotope effect also observed on W in theory R. Petuya et al. J Phys. Chem. C 2015
28 ERDA vs. NRA studies in self-damaged W ERDA undamaged/self-damaged W Measurement of both H and D One can study surface processes ERDA method not sensitive enough for bulk NRA self-damaged W D atoms can penetrate onto bulk and saturate the traps induced by heavy ion irradiation Damage profile dominates the D retention large NRA signal Perfect case for studying dynamics of D atom diffusion and isotope exchange in bulk Isotope exchange - Possible tritium removal technique MPS workshop, June
29 In situ NRA measurements 3 He Sample Heater D depth profiling during atom exposure down to 7 µm Mean flux ion beam position 5.8x10 18 D/m 2 s 29
30 In situ NRA measurements Nuclear Reaction Analysis (NRA) - detecting proton signal from nuclear reaction D( 3 He,p) 4 He Depth profile - 5 different energies: 776, 1550, 2580, 3400 and 4300 kev Calibration measurements at on standard: a-c:d layer (60 nm) Takes about 1.5 h to go through the whole cycle, avoid too much current due to temperature increase. Time of studied processes - hours/days Markelj et al. Phys. Scr. T159 (2014)
31 In situ NRA measurements D atom exposure Exposure to D atom 600 K for 48 h. D atom beam flux density: D/m 2 s. Filling of damaged area by D atoms. Markelj et al. Submitted to JNM - under review 31
32 In situ NRA measurements D atom exposure Exposure to D atom 600 K for 48 h. D atom beam flux density: D/m 2 s. Filling of damaged area by D atoms. 32
33 In situ NRA measurements D atom exposure Exposure to D atom 600 K for 48 h. D atom beam flux density: D/m 2 s. Filling of damaged area by D atoms. 33
34 In situ NRA measurements D atom exposure Exposure to D atom 600 K for 48 h. D atom beam flux density: D/m 2 s. Filling of damaged area by D atoms. 34
35 In situ NRA measurements D atom exposure Exposure to D atom 600 K for 48 h. D atom beam flux density: D/m 2 s. Filling of damaged area by D atoms. 35
36 In situ NRA measurements thermal 600 K Exposure to D atom 600 K for 48 h, fluence 1x10 24 D/m 2. Atomic beam switch off; 43 h at 600 K D self desorption 36
37 In situ NRA measurements thermal 600 K Exposure to D atom 600 K for 48 h, fluence 1x10 24 D/m 2. Atomic beam switch off; 43 h at 600 K D self desorption 37
38 In situ NRA measurements thermal 600 K Exposure to D atom 600 K for 48 h, fluence 1x10 24 D/m 2. Atomic beam switch off; 43 h at 600 K D isothermal desorption 38
39 In situ NRA measurements thermal 600 K Atomic beam switch off; 43 h at 600 K D self desorption 30 % decrease in total concentration in damaged layer Previous study on IW only 590 K for 20 h -> 27% decrease Markelj et al. Submitted to JNM - under review 39
40 In situ NRA measurements bulk isotope exchange Exposure to D atom 600 K for 48 h, fluence 1x10 24 D/m 2. Atomic beam switch off; 43 h at 600 K D self desorption Additional exposure to D beam for 24 h after hold 40
41 In situ NRA measurements bulk isotope exchange H D Exposure to H atoms for 96h - bulk isotope exchange at 600 K H atom beam flux density: H/m 2 s D removal in damaged layer by isotope exchange Markelj et al. Submitted to JNM - under review 41
42 In situ NRA measurements bulk isotope exchange H D Exposure to H atoms for 96h - bulk isotope exchange at 600 K H atom beam flux density: H/m 2 s D removal in damaged layer by isotope exchange 42
43 In situ NRA measurements bulk isotope exchange H D Exposure to H atoms for 96h - bulk isotope exchange at 600 K H atom beam flux density: H/m 2 s D removal in damaged layer by isotope exchange 43
44 In situ NRA measurements bulk isotope exchange H D Exposure to H atoms for 96h - bulk isotope exchange at 600 K H atom beam flux density: H/m 2 s D removal in damaged layer by isotope exchange 44
45 In situ NRA measurements bulk isotope exchange H D Exposure to H atoms for 96h - bulk isotope exchange at 600 K H atom beam flux density: H/m 2 s D removal in damaged layer by isotope exchange 45
46 In situ NRA measurements bulk isotope exchange H D Exposure to H atoms for 96h - bulk isotope exchange at 600 K H atom beam flux density: H/m 2 s D removal in damaged layer by isotope exchange 46
47 In situ NRA measurements bulk isotope exchange H D Exposure to H atoms for 96h - bulk isotope exchange at 600 K H atom beam flux density: H/m 2 s D removal in damaged layer by isotope exchange after 96 h of H exposure, fluence 2.4x10 24 H/m 2, 20 % of D still remained, 10 % at DP 47
48 In situ NRA measurements bulk isotope exchange H D Exposure to H atoms for 96h - bulk isotope exchange at 600 K H atom beam flux density: H/m 2 s Comparison to isothermal desorption - after 20 h the signal drops by 48% and after 43 h it has decreased by 68%. Signal MeV, 0.78 MeV 48
49 In situ NRA measurements bulk isotope exchange H D Exposure to H atoms for 96h - bulk isotope exchange at 600 K H atom beam flux density: H/m 2 s D removal in damaged layer by isotope exchange after 96 h of H exposure, fluence 2.4x10 24 H/m 2, 20 % of D still remained, 10 % at DP Possible 3 He beam effect stronger binding of D around He interstitials SRIM calculation 49
50 In situ NRA measurements bulk isotope exchange D H Exposure to D atoms for 71 h - bulk isotope exchange at 600 K D atom beam flux density: D/m 2 s. H removal in damaged layer by isotope exchange 50
51 In situ NRA measurements bulk isotope exchange D H Exposure to D atoms for 71 h - bulk isotope exchange at 600 K D atom beam flux density: D/m 2 s. H removal in damaged layer by isotope exchange 51
52 In situ NRA measurements bulk isotope exchange D H Exposure to D atoms for 71 h - bulk isotope exchange at 600 K D atom beam flux density: D/m 2 s. H removal in damaged layer by isotope exchange 52
53 In situ NRA measurements bulk isotope exchange D H Exposure to D atoms for 71 h - bulk isotope exchange at 600 K D atom beam flux density: D/m 2 s. H removal in damaged layer by isotope exchange 53
54 In situ NRA measurements bulk isotope exchange D H Exposure to D atoms for 71 h - bulk isotope exchange at 600 K D atom beam flux density: D/m 2 s. H removal in damaged layer by isotope exchange 54
55 In situ NRA measurements bulk isotope exchange D H Exposure to D atoms for 71 h - bulk isotope exchange at 600 K D atom beam flux density: D/m 2 s. H removal in damaged layer by isotope exchange 55
56 In situ NRA measurements bulk isotope exchange D H Exposure to D atoms for 71 h - bulk isotope exchange at 600 K D atom beam flux density: D/m 2 s. H removal in damaged layer by isotope exchange 56
57 Bulk isotope exchange Total amounts of D in damaged area Only D loading and exchnage D H similar dynamics Approximately 2 times higher fluence needed for H D isotope exchange Isotope exchange is efficient 57
![Bulk isotope exchange - modelling d [ cb D ] ( 1) 2 / H excb [ cb D ] B D dt d[ c dt ] [ c Ed kt c e B H 1) d H excb B D B H E / kt c e (1 c / c c / c ) s ] ( 2 B D B0 Observed isotope effect B H σ](/docs-images/82/85102303/images/58-7.jpg "excb (H D;#1)=5.2±0.6 10-25 m 2 σ excb (H D;#2)=6.5±0.3 10-25 m 2 σ excb (D H)=1.1±0.5 10-24 m 2 B0 H Uptake only d[ c dt ] E / kt c e (1 c / c ) ( ) B D 1) d B D B D B0 D ( 2 bulk Markelj et al.")
58 Bulk isotope exchange - modelling d [ cb D ] ( 1) 2 / H excb [ cb D ] B D dt d[ c dt ] [ c Ed kt c e B H 1) d H excb B D B H E / kt c e (1 c / c c / c ) s ] ( 2 B D B0 Observed isotope effect B H σ excb (H D;#1)=5.2± m 2 σ excb (H D;#2)=6.5± m 2 σ excb (D H)=1.1± m 2 B0 H Uptake only d[ c dt ] E / kt c e (1 c / c ) ( ) B D 1) d B D B D B0 D ( 2 bulk Markelj et al. Submitted to JNM - under review D (bulk)=3.5± D/m 2 s R= D (bulk)/ D =
59 Preliminary results on Simultaneous high energy W ion irradiation and D atom loading 59
60 Simultaneous W irradiation and D loading The set up In-beam mesh charge collector 4 mm A W MeV A V 600 K Heater Mean flux ion beam position 5.4x10 18 D/m 2 s 60
61 Simultaneous W irradiation and D loading Damage W samples by MeV self-implantation at different temperatures + simultaneous loading by D atoms Sample A0897-A Simultaneous W irradiation and D atom 600 K Current-W 6+ = 1.2 na Irrad. Time = s W Fluence = W/m 2 Sample A0894-A Simultaneous W irradiation and D atom 800 K Current-W 6+ = 1.15 na Irrad. Time = s W Fluence = W/m 2 Sample A0896-A Simultaneous W irradiation and D atom 450 K Current-W 6+ = 1.15 na Irrad. Time = s W Fluence = W/m 2 SRIM calculation 61
62 Simultaneous W irradiation and D loading Deuterium depth profiles measured by Nuclear Reaction Analysis - NRA Analyzing protons ( 12 MeV) from nuclear reaction D( 3 He,p) 4 He at 5 different 3 He energies from 780 kev to 4.2 MeV Additional D atom loading for 19h 2 mm 3 He beam TARGET 62
63 Simultaneous W irradiation and D loading Comparison of simultaneous W irradiation + D loading to sequential W irradiation and exposure at 600 K 63
64 Conclusions and Outlook for RCP Penetration of atomic D into bulk, saturation of the traps induced by W ion irradiation. D retention in self-ion damaged studied different exposure temperatures versus damage annealing Less retention at higher temperatures In situ measurements gave direct information about the dynamics of D migration and isotope exchange in radiation-induced defects in W. Efficient isotope exchange of D in bulk of damaged tungsten by H atoms at 600 K Simultaneous W ion irradiation and D exposure under evaluation Isotope exchange at lower temperatures (500 K) Detail study of the effect of He beam implantation on D retention: simultaneous irradiation with high-energy ( kev) 4 He beam and atomic D beam, followed by D NRA profiling Installation of ion gun for simultaneous irradiation with high-energy W ions and low energy D ions (500 ev 5 kev) Effect of heavy ion irradiation on deuterium retention in W-based advanced materials 64
65 Thank you for your attention! 65
66 Study of defect annealing total amounts STEM analysis by Ł. Ciupiński (Poland) of damaged W annealed at indicated temperatures Reduction od dislocation density by 66% - good agreement with NRA A. Založnik et al., PFMC 2015, submitted to Phys. Scripta 66
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