1 Florian Irrek, GRK1203-Seminar in Bad Breisig 11.10.2007 Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation.

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1 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ In-situ measurement of the hydrogen content of a-C:H Layers with Laser-induced Thermal Desorption F. Irrek, B. Schweer, S. Brezinsek, A. Pospieszczyk V. Philipps, U. Samm

2 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ T-Inventory of a Fusion Reactor Graphite for high heat-flux areas  Erosion and Redeposition of Carbon  Formation of Hydrogenated Carbon Layers – Hydrogen Retention Max. Tritium Inventory (Safety Limit) in ITER: 350 g Diagnostics for in-situ Measurement of retained Tritium needed A. Kirschner

3 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ Hydrogen Measurement by Means of Laser Desorption and Emission Spectroscopy In-situ measurement at plasma-wetted surfaces Rapid surface heating Release of D 2, H 2, HD, CD 4, C 2 D 4 Emission spectroscopy: H , D 2 -Fulcher n e, T e measured by other diagnostics Calibration at TEXTOR with previously coated and characterized samples

4 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ Power Density and Temperature 1-dim Heat Conduction sufficient for Spot Centre: Restrictions: 1.Temperature 1300…2000 K 2.Laser spot size 4 … 6 mm 2 Laser power on surface < 14 kW 3.Pulse Length < 4ms Laser-Desorbed Spot ( a-C:D on Graphite) Temperature Rise  T [kK] Laser Pulse Duration t [ms]  T [K] Heat Load [kW/cm 2 ]

5 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ Thermal Desorption of a-C:H Layers Number of Released Particles normalized Temperature in centre of laser spot [K] Released Particles after laser shotParticle flux (Time derivative) laser heating 10 6 K/s Heating in oven 1 K/s Different configurations of C-atoms graphitic (sp 2 ) aromatic (sp 2 + H) alkane-like (sp 3 + nH) [*] J. Küppers – Surf. Sci. Reports 22 (1995) 249 Ref: [*]

6 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ depends on Substrate Properties and Layer Properties (damping and refractive index) Reflexion of Laser Light from the Surface P. Wienhold Refractive Index of Layer depends on H content A. Annen

7 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ D Release: Pressure Rise 250 nm a-C:D Layer >80% Reduction of released D Flow in 2 nd Shot Applied mean Laser Power Density: 95 kW/cm 2 D 2 -Flow peaks below 1000 °C D 2 : CD 4 = 17 CD 4 D2D2 1 st shot: 6x st shot: below detection limit 1 st shot: 1x10 16

8 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ Layer Centre Border Centre Border Inventory / a.u. Spot  1.2 mm D Release: SIMS SIMS Measurement: Hydrogen Inventory in Sample Surface 96% Reduction of D-Inventory, Charcoal-like Spot Surface H from reabsorbed H 2 O

9 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ Heating, Surface Effects Rapid Heating: –1300…2000 K reached by 70 kW/cm 2 x 1.5 ms irradiation Target substrate + roughness Layer optical properties: thickness, H/C Short-time Outgassing Flux (0.2 ms): –H 2, CH 4, 4:1 – 8:1 –~10 18 Molecules/(cm 2 nm s) Inevitable Consequences: –Thermal Cracks in substrate –Formation of Blisters: Thermal stress and loss of adhesion –Sublimation of Blisters: 1 µm 3 of material Absorption > during last 0.1 ms is sufficient View 20° to surface

10 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ LDS measurements in laboratory: Principle Sample 10 cm Nd:YAG-Laser 1064 nm, 1.5 ms x 70 kW/cm 2 QMA112 Photodiode Reflected Laser light Repititive Mass scan (1 Hz) of mass 2 to 50 Before and after laser pulse Total duration 51 s

11 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ LDS measurements in laboratory: Principle Superimposed mass spectra from laser desorption (here: thick soft co-deposit from old ALT tile) Dark lines: early Bright lines: late

12 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ LDS measurements in laboratory: Principle Superimposed mass spectra from laser desorption here: Graphite sample, coated in PADOS (360 nm), Dark lines: early Bright lines: late Before Textor exposure Total D: 1.5 x H 2 /D 2 : 0.16 D 2 /CD 4 : 6.0 After Textor exposure (3 units) Total D: 6.6 x H 2 /D 2 : 0.39 D 2 /CD 4 : 11

13 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ LDS measurements in laboratory: Data evaluation m=2  U=0.203 V m=3  U=0.368 V m=4  U=0.518 V 1.Extract mass channels 2.Plot over time 3.Fit exponential before and after laser pulse 4.Return Voltage difference of fit curves at time of laser pulse 5.Apply Calibration factors (H 2, CH 4 & Isotopologues) and sum up relevant channels  N D, N H, H/D, D 2 /CD 4

14 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ Emission Spectroscopy Radial Position / cm rel. Toroidal Position / cm DD Intensity / a.u I tot Sample Conversion from spectral line intensity I tot to atomic flux  A Electron density n e [10 18 m -3 ] Electron Temperature T e [eV] S/XB (T e,n e ) Electron density n e [10 18 m -3 ] Electron Temperature T e [eV] S/XB (T e,n e )

15 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ Radial Position toroidal Measurements at TEXTOR: Principle diamater = 11 cm HH H2H Radial Position / cm Toroidally Integrated Signal H  x 5% H2H2 toroidal Sample Surface

16 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ Time: 1 ms/Frame Frames before and after Pulse = Background Signal w/o Background Integrated Signal, Background subtracted Measurements at TEXTOR: Data evaluation Lorentz Fit Area Width Position of Maximum

17 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ Measurements at TEXTOR: Overview by shot Shot#Filter D+H/cm 2 /10 18 D:HD 2 :CD 4 Raw Single frames Scaled signal HH : CH H2H : C II HH 1 75:16: HH 0.1 r = 49 cm (2 nd Laser Pulse) 1 st 2 nd

18 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ Shot#Filter D+H/cm 2 /10 18 D:HD 2 :CD 4 Raw Single frames Scaled signal C2C : C2C HH : CH C2C : C II 1 r = 49 cm Measurements at TEXTOR: Overview by shot

19 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ Shot#Filter D+H/cm 2 /10 18 D:HD 2 :CD 4 Raw Single frames Scaled signal H2H : HH : HH 0.03 r = 50 cm 49 cm Measurements at TEXTOR: Overview by shot

20 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ Measurements at TEXTOR: Overview H  Shot#Filter D+H/cm 2 /10 18 D:HD 2 :CD 4 Raw Single frames Integral / V x pixel HH : :16: : :17: r = 49 cm 2 nd Laser Pulse 1 st 2 nd r = 50 cm

21 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ Measurements at TEXTOR: Overview H 2, CH, C 2 Shot#Filter D+H/cm 2 /10 18 D:HD 2 :CD 4 Raw Single frames Integral / V x pixel H2H : : CH 10.71: : C2C : :1 870 r = 49 cm

22 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ Approx. 20 free spots on 8 old samples Coating of 9 samples scheduled for beginning of next week –Non-polished samples –360 nm (effective thickness / on Silicon) –Coated side clearly marked –Characterized with LDS prior to TEXTOR exposure Presently ready samples

23 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ Sample surface at 48 cm 7 x D+H 49 cm 6 x D+H 50 cm 6 x D+H Measurements at TEXTOR: H  Radial Position r / cm FWHM: 3.3 cm FWHM: 5.3 cmFWHM: 2.0 cm Total: HH HH HH

24 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ Measurements at TEXTOR: H x (H+D)/cm 2 53 normalized raw 50 cm 47

25 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ Summary Laser-induced heating and thermal desorption: –Power density of 70 kW/cm 2 for 1.5 ms –Complete desorption at 1400 … 1600 K –Release of H 2, CH 4, C 2 H 4 (75:15:10) Spectroscopic measurement with Interference filters: –H  : S/XB, H atom per released molecular species –H 2 (Fulcher-Band): D/XB, amount of H released as H 2 (60%)

26 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ Measurements at TEXTOR: H  : Filter: 3%, H  N D+H = 0.7 x /cm 2 D:H = 1: : Filter: 5%, H  N D+H = 0.6 x /cm 2 D:H = 3: Integral/ND-Filter: V x pixel 2 Integral/ND-Filter: V x pixel 2

27 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ Measurements at TEXTOR: H  : Sample at 50 cm Filter: 3%, H  N D+H = 1.9 x /cm 2 D:H = 4: : Filter: 5%, H  N D+H = 0.6 x /cm 2 D:H = 3:1 Integral/ND-Filter: V x pixel 2 Integral/ND-Filter: V x pixel 2

28 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ Measurements at TEXTOR: H : Filter: 100%, H 2 N D+H = 0.6 x /cm 2 D:H = 1: : Filter: 100%, H 2 N D+H = 3.2 x /cm 2 D:H = 4:1 Integral: 94 V x pixel 2 Integral: 430 V x pixel 2 Different penetration depth?

29 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ Measurements at TEXTOR: C : Filter: 10%, C 2 N D+H = 0.4 x /cm 2 D:H = 1: : Filter: 10%, C 2 N D+H = 2.2 x /cm 2 D:H = 5:1 Integral/ND-Filter: 118 V x pixel 2 Integral/ND-Filter: 870 V x pixel 2

30 Florian Irrek, GRK1203-Seminar in Bad Breisig Forschungszentrum Jülich in der Helmholtz-Gemeinschaft Institut für Energieforschung – PlasmaphysikAssociation EURATOM - FZJ Measurements at TEXTOR: CH : Filter: 100%, CH N D+H = 0.7 x /cm 2 D:H = 1: : Filter: 100%, CH N D+H = 0.6 x /cm 2 D:H = 3:1 Integral: 105 V x pixel 2 Integral: 252 V x pixel 2