Ultrafast X-Ray-Matter Interaction and Damage of Inorganic Solids October 10, 2008

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1 Ultrafast X-Ray-Matter Interaction and Damage of Inorganic Solids October 10, 2008 Richard London Workshop on Interaction of Free Electron Laser Radiation with Matter Hamburg This work performed under the auspices of the U.S. Department of Energy by under Contract DE-AC52-07NA27344

2 Outline of talk "Theory" for hard x rays X-ray/matter interaction physics X-ray optics damage Experiments with soft x rays and UV Single-pulse experiments with FLASH Multi-pulse experiments with a UV laser Conclusions 2

3 Fundamental x-ray interaction processes absorption bound-bound, bound-free, free-free emission for hard x rays, bound-free (photo-ionization) usually dominates inverse of these processes generally occurs for hot plasmas on long timescales scattering coherent (Thomson, forward scattering) incoherent (Compton) 3

4 Atomic physics and x-ray absorption schematic energy level diagram energy principal quantum no. 3 2 shell M L... continuum maximum # electrons 8 1 K 2 4

5 Typical photo-ionization cross sections cross-section cm 2 /atom Si C Fe Au 0.03 E (kev) 5

6 x-ray absorption and subsequent electron processes inner shell photo-ionizaton e-e slowing down auger ionization e-ion coupling collisional ionization recombination 6

7 Energy-time picture of x-ray material interaction 10 kev 1 kev 10 ev x-ray absorption auger emission electron slowing down particle energy 1 ev 0.1 ev 1 fs FEL pulse duration non-thermal ion motion 10fs 100 fs 1 ps 10ps 100 ps 1 ns time electron-ion thermalization melting spallation thermal fracture 7

8 Methods for simulating x-ray interaction with solids 10 kev 1 kev Monte Carlo Molecular dynamics 10 ev Rate equations particle energy continuum ("hydro") dynamics 1 ev 0.1 ev 1 fs XFEL pulse 10fs 100 fs 1 ps 10ps 100 ps 1 ns time 8

9 Monte Carlo simulation of photo-electron cascade in bulk materials bulk sample x-ray photo electron secondary electrons many ( ) trajectories are tracked in space and time collisions are simulated from known cross sections using random numbers to choose location and scattering angle. 9

10 Time dependent evolution of electrons after absorption of a 10 kev photon in diamond T (ev) N e t [fs] Conclusions from Monte Carlo study It is important to include effects of both electron and holes. cascade timescale ~ 10 fs. # secondary electrons per photo-electron E ph /(2*E gap ), 800 for this example. Ziaja, et al., J. App. Phys. (2005) 10

11 Response of solid matter is characterizeed by the local x-ray energy deposition, i.e. the dose Dose absorbed energy per unit mass, volume, or atom. Natural units are ev/atom, since binding energies of solid materials are of this order. In most cases, the time to transport energy out of x-ray deposition region is longer than XFEL pulse duration. absorbed dose remains confined during pulse. In some cases, the definition of dose must be generalized to include electron transport, which broadens the energy deposition region. 11

12 X-ray matter interaction spans a wide range of dose and applications x-ray optics hot solids Warm Dense Matter Dense plasmas Biomolecular imaging high field interactions energy density ( dose, ev/atom) I now focus on x-ray optics damage, at the low end of the dose line 12

13 Damage consideration for the LCLS optics Layout of LCLS X-ray areas linac undulator optics enclosure near experimental hall far experimental hall Distance (m) 13

14 There are variety of x-ray optics in the LCLS Front End Optics Enclosure Gas Detectors Solid Attenuator Monochrometer collimators Direct Imager Soft X-Ray Offset Mirror System Muon Shield High-Energy Slit Gas Attenuator Soft X-Ray Grating normal incidence Total Energy Detector Hard X-Ray Offset Mirror System grazing incidence 14

15 What is damage? Damage is defined as any process that will cause failure or degradation of an optic. possible damage mechanisms melting phase change high pressure effects (spallation, shear) thermal stress, thermal fatigue photo-chemical processes Theoretical analysis of x-ray processes and experience from optical laser-matter studies suggest that we should certainly avoid melting the optics surface in a single pulse. Calculation of the melt dose D m = " T m C (T )dt + H m T r T r = room temp. T m = melting temp. C = heat capacity H m = latent heat of melting 15

16 Melting damage threshold complete melt 2 D m (ev/atom) reach T m Candidate optics materials Material C Si B 4 C Quantity T melt (K) D melt (ev/atom) H atomic number U 16

17 Expected dose from LCLS at normal incidence Gaussian beam model: F = F o ( 1+ L" / w 2 ) #2 Cold opacity model for surface dose: D = F σ a unfocused dose at 20 m from LCLS undulator 10 F = fluence (J/cm 2 ) D = dose L = distance λ = wavelength w = beam waist σ a = abs. xsect/atom E (kev) Dose (ev/atom) H atomic number U.01

18 Compare melt dose to x-ray dose x-ray dose = maximum over LCLS energy range (0.8-8 kev) 10 L = 100 m 100 L = 400 m melt dose x-ray dose 1 good bad atomic number light, refractory elements must be used near XFEL other materials can be used in far hall 18

19 Grazing incidence optics are a special case x-ray laser beam reflected beam θ heated region d h mirror d x = x-ray range d e = photo-electron collisional range d h [d x 2 + d e 2 ] 1/2 Three factors lead to a greatly reduce dose at grazing incidence: high reflectivity evanescent wave limit to x-ray range electron transport 19

20 Design for LCLS Soft-X-ray Offset Mirror System (SOMS) Operation range is to be between 0.8 and 2 kev. Design criteria maximize reflectivity (> 90%) minimize length (i.e. maximize grazing angle) minimize dose 2 options have been considered: Si and B 4 C coating on Si Findings B 4 C/Si provides good solution for full energy range θ = 0.8 deg. L = 25 cm D < 0.04 ev/atom Si provides an alternate solution for 0.8 to 1.8 kev This option may be considered if manufacturing or damage is a problem for B 4 C layer. 20

21 Reflectivity and Dose for grazing incidence mirrors Si 0.6 K-edge θ 1.5 Reflectivity 1.5 B 4 C θ Dose (ev/atom) θ θ E (kev) E (kev) E (kev) 21

22 We have recently performed damage experiments on the FLASH facility in Hamburg collaboration with groups from Warsaw, Prague, Hamburg, Uppsala and Essen. Laser parameters wavelength = 32, 22 and 14 nm pulse length 25 fs focal spot diameter 20 µm Option:UCRL# Option:Additional Information 22

23 Goals and setup for FLASH experiments determine damage thresholds at shortest available wavelengths relate this to hard x-ray case through calculated dose. focusing mirror vacuum chamber gas attenuator FEL beam Samples: C, Si, SiC, B 4 C motion stage Samples were exposed to single pulses at various fluences and then later analyzed with various microscopes. 23

24 Damage sites measured by optical interferometry height Images of SiC samples exposed to 32 nm radiation (a) F < 0.28 J/cm 2 (c) F = 0.72 J/cm (b) 2 20 µm depth (nm) position (µm) lineouts through center S. P. Hau-Riege, et al. Appl. Phys. Lett. (2007). 24

25 The crater depth increases with pulse energy λ = 14 nm focus on low-fluence region 25

26 Low fluence region yields damage thresholds λ = 14 nm 26

27 Summary of FLASH results damage threshold (ev/atom) wavelength (nm) Si SiC (bulk) material SiC layer on Si B 4 C (bulk) B 4 C layer on Si calculated melt Damage thresholds are comparable to the melt threshold. The damage threshold is smaller for layered samples than for bulk. this might be caused by the layer structure or the interface. The wavelength variations might be due to a combination of concentration gradient in the layers and the variation of penetration depth. 27

28 Multiple-pulse damage experiments with a UV laser Multi-pulse damage might occur at lower fluences than for single pulses due to thermal fatigue or photochemical processes. Such experiments are difficult at FLASH due to its large pulse-to-pulse energy variation. Excimer UV lasers have excellent pulse-to-pulse stability. We have used long UV pulses (25 ns), allowing heat conduction to produce thermal dose profiles similar to those for x-ray irradiated grazing-incidence optics. 28

29 We find that the damage threshold decreases approx. logarithmically with the number of pulses damage map for layered B 4 C/Si sample * no damage damage observed Hau-Riege et al., submitted to Appl. Phys. Lett. 29

30 Summary of multiple pulse damage results damage thresholds (ev/atom) Si B 4 C SiC UV (1 pulse) > UV (10 5 pulses) melting fatigue LCLS HOMS 1 x x x 10-6 LCLS SOMS multi-pulse damage thresholds 1/2 single pulse value. Si: single pulse threshold > melt, multi-pulse threshold < melt. B 4 C: both single pulse and multi-pulse thresholds < melt. all observed thresholds > estimated fatigue threshold. all observed thresholds < LCLS optics doses 30

31 Conclusions The advent of XFELs will open an exciting new field of ultra-short, high intensity, x-ray material interaction. A large range of energy densities and physical phenomena can be accessed. X-ray optics must be designed to withstand damage. Melting is an important threshold damage mechanism. To avoid damage use: low-z materials placement at a large distance from the XFEL. grazing incidence Experiments on FLASH and conventional lasers are helping to determine damage thresholds for XFEL optics. 31

32 Thanks to many collaborators! some of them (but not all!) LLNL Hamburg Uppsala Prague Warsaw Essen S. Hau-Riege, A. Szoke, R. Bionta, D. Ryutov B. Ziaja, H. Wabnitz, S. Toleikis, et al. (FLASH) J. Hajdu, M. Bergh & C. Caleman L. Juha, J. Chalupsky J. Krzywinski & R. Sobieraski K. Sokolowski-Tinten, N. Stojanovic, FLASH 32

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