Bridging model and real systems with laboratory experiments: dynamic retention of deuterium in tungsten

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1 dynamic retention of deuterium in tungsten PIIM laboratory Aix-Marseille Université - CNRS Marseille, France Régis Bisson

2 summary of common laboratory experiments same parameters, similar retention but different TPD profile: sample preparation? 200 ev/d F= D/m 2 Ogorodnikova et al. J. Nucl. Mater , 469 (2003) Ogorodnikova et al., Phys. Scr. T138, (2009) Tian et al., J. Nucl. Mater. 399, 101 (2010) 1

3 summary of common laboratory experiments same parameters, similar retention but different TPD profile: sample preparation? 200 ev/d F= D/m 2 Ogorodnikova et al. J. Nucl. Mater , 469 (2003) Ogorodnikova et al., Phys. Scr. T138, (2009) Tian et al., J. Nucl. Mater. 399, 101 (2010) different apparatuses used for D implantation and TPD retention measurement air exposure generates many deuterated products than cannot all be recorded underestimation of retention [Wang et al. Nucl. Instr. Meth. Phys. Res. B 300, 54 (2013)] 2

4 selecting ideal conditions Retention measurement best approach: all-in-situ apparatus (no air exposure) a rare example in the literature: Ogorodnikova et al. J. Nucl. Mater , 469 (2003) Ogorodnikova et al. Flux: D.m -2.s -1 Fluence: D.m -2 T s : 300 K E k : 200 ev/d 3

5 selecting ideal conditions Retention measurement best approach: all-in-situ apparatus (no air exposure) a rare example in the literature: Ogorodnikova et al. J. Nucl. Mater , 469 (2003) Ogorodnikova et al. Flux: D.m -2.s -1 Fluence: D.m -2 T s : 300 K E k : 200 ev/d this work D.m -2.s D.m K 250 ev/d in Aix-Marseille University (AMU): our W samples present a single low temperature desorption peak (low defect density) 4

6 selecting ideal conditions this work D.m -2.s D.m K 250 ev/d Polycrystalline sample with low defect concentration - Annealed at (1573 K ; 1h) in vacuum by A.L.M.T. (Japan) - Electro-polished in-house for mirror finish - Annealing at 1300 K in ultra-high vacuum 5

7 the AMU apparatus differentially pumped QMS chamber Polycrystalline sample with low defect concentration - Annealed at (1573 K ; 1h) in vacuum by A.L.M.T. (Japan) - Electro-polished in-house for mirror finish - Annealing at 1300 K in ultra-high vacuum 6

8 the AMU apparatus differentially pumped QMS chamber D 2 + 7

9 the AMU apparatus differentially pumped QMS chamber D 2 8

10 the AMU apparatus differentially pumped QMS chamber D 2 Absolute calibration of the TPD in desorption rate (D 2 /s) and retention (D/m 2 ) checked with NRA measurements (JSI, Slovenia) Absolute retention sensitivity down to D.m -2 9

11 retention measurements: extending to low fluences retention orders of magnitude smaller than implantation probability from SRIM model non-linear dependence of Retention α Fluence [1] Ogorodnikova et al., J. Nucl.Mater , 469 (2003) 10

12 retention measurements: extending to low fluences retention orders of magnitude smaller than implantation probability from SRIM model non-linear dependence of Retention α Fluence Retention α Fluence [1] Ogorodnikova et al., J. Nucl.Mater , 469 (2003) Bisson et al., in preparation 11

13 retention measurements: extending to low fluences retention similar to SRIM implantation probability when reaching low fluences non-linear dependence of Retention α Fluence Retention α Fluence [1] Ogorodnikova et al., J. Nucl.Mater , 469 (2003) Bisson et al., in preparation 12

14 retention measurements: explaining discrepancies retention similar to SRIM implantation probability when reaching low fluences non-linear dependence of Retention α Fluence Retention α Fluence discrepancy in the D/m 2 range where different fluxes were used [1] Ogorodnikova et al., J. Nucl.Mater , 469 (2003) Bisson et al., in preparation 13

15 retention measurements: explaining discrepancies retention similar to SRIM implantation probability when reaching low fluences 2 min non-linear dependence of Retention α Fluence Retention α Fluence hour [1] Ogorodnikova et al., J. Nucl.Mater , 469 (2003) discrepancy in the D/m 2 range where different fluxes were used i.e. different implantation duration could it be that release (desorption) of deuterium occurs during implantation?! Bisson et al., in preparation 14

16 retention measurements: explaining discrepancies repeated this implantation many times with different storage time between the end of implantation and the TPD measurement [1] Ogorodnikova et al., J. Nucl.Mater , 469 (2003) could it be that release (desorption) of deuterium occurs during implantation?! Bisson et al., in preparation 15

17 dynamic retention of deuterium in tungsten Deuterium release on the time scale of hours and days Release of deuterium during long implantation (explains the discrepancy in the D/m 2 range between our data and Ogorodnikova et al. data) Bisson et al., in preparation 16

18 dynamic retention of deuterium in tungsten Deuterium release on the time scale of hours and days Best fit obtained with a double exponential decay (with a constant): at least 3 populations of traps but a single desorption peak! Bisson et al., in preparation 17

19 dynamic retention of deuterium in tungsten Deuterium release on the time scale of hours and days Best fit obtained with a double exponential decay (with a constant): at least 3 populations of traps but a single desorption peak! Bisson et al., in preparation 18

20 dynamic retention of deuterium in tungsten Deuterium release on the time scale of hours and days The single desorption peak has a structure evolving with storage time: it is composed of several sub-peaks Several trapping energies are related to the low desorption temperature peak (at least 3 trapping energies from previous retention decay analysis) Bisson et al., in preparation 19

21 origin of the dynamic retention of deuterium a single TPD peak = at least 3 trapping energies a single trap: the W vacancy = at least 4 groups of trapping energies for 300 K implantation Bisson et al., in preparation Fernandez, Kato, Ferro, in preparation DFT calculations + statistical model PIIM lab + NIFS (D. Kato) 20

22 double checking the origin of the dynamic retention of deuterium At low fluences: retention = SRIM implantation probability: dynamic retention is non operative Why? deuterium density is low (10-5 at. density) mostly 1H or 2H-vacancy complexes (VH 1-2 ) Bisson et al., in preparation 21

23 double checking the origin of the dynamic retention of deuterium At low fluences: retention = SRIM implantation probability: dynamic retention is non operative Why? deuterium density is low (10-5 at. density) mostly 1H or 2H-vacancy complexes (VH 1-2 ) Fernandez, Kato, Ferro, in preparation VH 1-2 complexes: binding energy is high desorption temperature should be higher for low fluences Bisson et al., in preparation 22

24 double checking the origin of the dynamic retention of deuterium At low fluences: retention = SRIM implantation probability: dynamic retention is non operative Why? deuterium density is low (10-5 at. density) mostly 1H or 2H-vacancy complexes (VH 1-2 ) Fernandez, Kato, Ferro, in preparation VH 1-2 complexes: binding energy is high desorption temperature should be higher for low fluences this is verified Bisson et al., in preparation 23

25 summary all-in-situ apparatus implantation at 300 K ; TPD up to 1300 K retention measured down to D/m 2 observation of D release at 300 K on at least 3 time scales with an evolution of the TPD peak consistent with W vacancy trap filling

26 summary all-in-situ apparatus implantation at 300 K ; TPD up to 1300 K retention measured down to D/m 2 observation of D release at 300 K on at least 3 time scales with an evolution of the TPD peak consistent with W vacancy trap filling R. Bisson, C. Grisolia (CEA), T. Angot Researchers O. Saïdi, F. Ghiorghiu PhD students S. Markelj (JSI, Slovenia) visiting scientist (Euratom) O. Mourey Master student J.-B. Faure Mechanical engineer from ANR, CNRS, AMU, EFDA/EUROfusion

27 perspectives Starting 2015 an extensive model experiment theory collaboration on D retention in tungsten through a project supported by the A*MIDEX foundation (Aix-Marseille Université) a large set of samples (single and poly-crystals) surface and bulk preparation techniques (e - /p + /W n+ accelerators, surface science) complete set of analysis tools (TPD, XPS, SEM, TEM, NRA, SIMS, PAS ) multi-scale modeling approach (DFT, OKMC, MRE) Y. Ferro, C. Becquart, C. Grisolia, B. Rousseau, R. Bisson, T. Angot, G. Cartry, C. Pardanaud, C. Martin, P. Roubin, M.-F. Barthe, L. Gallais PIIM, Fresnel, CEA, CEMHTI, UMET, LSPM Thank you for your attention

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