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Optics Express

Optics Express

  • Editor: Andrew M. Weiner
  • Vol. 21, Iss. 13 — Jul. 1, 2013
  • pp: 15382–15388
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Investigation of ablation thresholds of optical materials using 1-µm-focusing beam at hard X-ray free electron laser

Takahisa Koyama, Hirokatsu Yumoto, Yasunori Senba, Kensuke Tono, Takahiro Sato, Tadashi Togashi, Yuichi Inubushi, Tetsuo Katayama, Jangwoo Kim, Satoshi Matsuyama, Hidekazu Mimura, Makina Yabashi, Kazuto Yamauchi, Haruhiko Ohashi, and Tetsuya Ishikawa  »View Author Affiliations


Optics Express, Vol. 21, Issue 13, pp. 15382-15388 (2013)
http://dx.doi.org/10.1364/OE.21.015382


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Abstract

We evaluated the ablation thresholds of optical materials by using hard X-ray free electron laser. A 1-µm-focused beam with 10-keV of photon energy from SPring-8 Angstrom Compact free electron LAser (SACLA) was irradiated onto silicon and SiO2 substrates, as well as the platinum and rhodium thin films on these substrates, which are widely used for optical materials such as X-ray mirrors. We designed and installed a dedicated experimental chamber for the irradiation experiments. For the silicon substrate irradiated at a high fluence, we observed strong mechanical cracking at the surface and a deep ablation hole with a straight side wall. We confirmed that the ablation thresholds of uncoated silicon and SiO2 substrates agree with the melting doses of these materials, while those of the substrates under the metal coating layer are significantly reduced. The ablation thresholds obtained here are useful criteria in designing optics for hard X-ray free electron lasers.

© 2013 OSA

1. Introduction

X-ray free-electron lasers (XFELs) [1

1. B. W. J. McNeil and N. R. Thompson, “X-ray free-electron lasers,” Nat. Photonics 4(12), 814–821 (2010). [CrossRef]

], such as the Linac Coherent Light Source [2

2. P. Emma, R. Akre, J. Arthur, R. Bionta, C. Bostedt, J. Bozek, A. Brachmann, P. Bucksbaum, R. Coffee, F.-J. Decker, Y. Ding, D. Dowell, S. Edstrom, A. Fisher, J. Frisch, S. Gilevich, J. Hastings, G. Hays, Ph. Hering, Z. Huang, R. Iverson, H. Loos, M. Messerschmidt, A. Miahnahri, S. Moeller, H.-D. Nuhn, G. Pile, D. Ratner, J. Rzepiela, D. Schultz, T. Smith, P. Stefan, H. Tompkins, J. Turner, J. Welch, W. White, J. Wu, G. Yocky, and J. Galayda, “First lasing and operation of an ångstrom-wavelength free-electron laser,” Nat. Photonics 4(9), 641–647 (2010). [CrossRef]

] and SPring-8 Angstrom Compact free electron LAser (SACLA) [3

3. T. Ishikawa, H. Aoyagi, T. Asaka, Y. Asano, N. Azumi, T. Bizen, H. Ego, K. Fukami, T. Fukui, Y. Furukawa, S. Goto, H. Hanaki, T. Hara, T. Hasegawa, T. Hatsui, A. Higashiya, T. Hirono, N. Hosoda, M. Ishii, T. Inagaki, Y. Inubushi, T. Itoga, Y. Joti, M. Kago, T. Kameshima, H. Kimura, Y. Kirihara, A. Kiyomichi, T. Kobayashi, C. Kondo, T. Kudo, H. Maesaka, X. M. Maréchal, T. Masuda, S. Matsubara, T. Matsumoto, T. Matsushita, S. Matsui, M. Nagasono, N. Nariyama, H. Ohashi, T. Ohata, T. Ohshima, S. Ono, Y. Otake, C. Saji, T. Sakurai, T. Sato, K. Sawada, T. Seike, K. Shirasawa, T. Sugimoto, S. Suzuki, S. Takahashi, H. Takebe, K. Takeshita, K. Tamasaku, H. Tanaka, R. Tanaka, T. Tanaka, T. Togashi, K. Togawa, A. Tokuhisa, H. Tomizawa, K. Tono, S. Wu, M. Yabashi, M. Yamaga, A. Yamashita, K. Yanagida, C. Zhang, T. Shintake, H. Kitamura, and N. Kumagai, “A compact X-ray free-electron laser emitting in the sub-ångstrom region,” Nat. Photonics 6(8), 540–544 (2012). [CrossRef]

], have started to provide intense, coherent, and ultrafast pulses in the hard X-ray region, which promote the development of new approaches in various fields, such as atomic physics [4

4. L. Young, E. P. Kanter, B. Krässig, Y. Li, A. M. March, S. T. Pratt, R. Santra, S. H. Southworth, N. Rohringer, L. F. Dimauro, G. Doumy, C. A. Roedig, N. Berrah, L. Fang, M. Hoener, P. H. Bucksbaum, J. P. Cryan, S. Ghimire, J. M. Glownia, D. A. Reis, J. D. Bozek, C. Bostedt, and M. Messerschmidt, “Femtosecond electronic response of atoms to ultra-intense X-rays,” Nature 466(7302), 56–61 (2010). [CrossRef] [PubMed]

6

6. S. M. Vinko, O. Ciricosta, B. I. Cho, K. Engelhorn, H.-K. Chung, C. R. D. Brown, T. Burian, J. Chalupský, R. W. Falcone, C. Graves, V. Hájková, A. Higginbotham, L. Juha, J. Krzywinski, H. J. Lee, M. Messerschmidt, C. D. Murphy, Y. Ping, A. Scherz, W. Schlotter, S. Toleikis, J. J. Turner, L. Vysin, T. Wang, B. Wu, U. Zastrau, D. Zhu, R. W. Lee, P. A. Heimann, B. Nagler, and J. S. Wark, “Creation and diagnosis of a solid-density plasma with an X-ray free-electron laser,” Nature 482(7383), 59–62 (2012). [CrossRef] [PubMed]

] and structural biology [7

7. H. N. Chapman, P. Fromme, A. Barty, T. A. White, R. A. Kirian, A. Aquila, M. S. Hunter, J. Schulz, D. P. DePonte, U. Weierstall, R. B. Doak, F. R. N. C. Maia, A. V. Martin, I. Schlichting, L. Lomb, N. Coppola, R. L. Shoeman, S. W. Epp, R. Hartmann, D. Rolles, A. Rudenko, L. Foucar, N. Kimmel, G. Weidenspointner, P. Holl, M. Liang, M. Barthelmess, C. Caleman, S. Boutet, M. J. Bogan, J. Krzywinski, C. Bostedt, S. Bajt, L. Gumprecht, B. Rudek, B. Erk, C. Schmidt, A. Hömke, C. Reich, D. Pietschner, L. Strüder, G. Hauser, H. Gorke, J. Ullrich, S. Herrmann, G. Schaller, F. Schopper, H. Soltau, K. U. Kühnel, M. Messerschmidt, J. D. Bozek, S. P. Hau-Riege, M. Frank, C. Y. Hampton, R. G. Sierra, D. Starodub, G. J. Williams, J. Hajdu, N. Timneanu, M. M. Seibert, J. Andreasson, A. Rocker, O. Jönsson, M. Svenda, S. Stern, K. Nass, R. Andritschke, C. D. Schröter, F. Krasniqi, M. Bott, K. E. Schmidt, X. Wang, I. Grotjohann, J. M. Holton, T. R. Barends, R. Neutze, S. Marchesini, R. Fromme, S. Schorb, D. Rupp, M. Adolph, T. Gorkhover, I. Andersson, H. Hirsemann, G. Potdevin, H. Graafsma, B. Nilsson, and J. C. Spence, “Femtosecond X-ray protein nanocrystallography,” Nature 470(7332), 73–77 (2011). [CrossRef] [PubMed]

,8

8. M. M. Seibert, T. Ekeberg, F. R. N. C. Maia, M. Svenda, J. Andreasson, O. Jönsson, D. Odić, B. Iwan, A. Rocker, D. Westphal, M. Hantke, D. P. DePonte, A. Barty, J. Schulz, L. Gumprecht, N. Coppola, A. Aquila, M. Liang, T. A. White, A. Martin, C. Caleman, S. Stern, C. Abergel, V. Seltzer, J.-M. Claverie, C. Bostedt, J. D. Bozek, S. Boutet, A. A. Miahnahri, M. Messerschmidt, J. Krzywinski, G. Williams, K. O. Hodgson, M. J. Bogan, C. Y. Hampton, R. G. Sierra, D. Starodub, I. Andersson, S. Bajt, M. Barthelmess, J. C. H. Spence, P. Fromme, U. Weierstall, R. Kirian, M. Hunter, R. B. Doak, S. Marchesini, S. P. Hau-Riege, M. Frank, R. L. Shoeman, L. Lomb, S. W. Epp, R. Hartmann, D. Rolles, A. Rudenko, C. Schmidt, L. Foucar, N. Kimmel, P. Holl, B. Rudek, B. Erk, A. Hömke, C. Reich, D. Pietschner, G. Weidenspointner, L. Strüder, G. Hauser, H. Gorke, J. Ullrich, I. Schlichting, S. Herrmann, G. Schaller, F. Schopper, H. Soltau, K.-U. Kühnel, R. Andritschke, C.-D. Schröter, F. Krasniqi, M. Bott, S. Schorb, D. Rupp, M. Adolph, T. Gorkhover, H. Hirsemann, G. Potdevin, H. Graafsma, B. Nilsson, H. N. Chapman, and J. Hajdu, “Single mimivirus particles intercepted and imaged with an X-ray laser,” Nature 470(7332), 78–81 (2011). [CrossRef] [PubMed]

].

Although XFEL light provides great capabilities, the intense beam could induce damage to optical elements, which would lead to degradation of the beam quality. The irradiation tolerance of optical elements is evaluated by comparing the absorption dose with the melting threshold. The melting threshold has been considered as a reasonable guide in designing optical components [9

9. R. M. Bionta, “Controlling dose to low Z solids at LCLS ,” LCLS Technical Note No. LCLS-TN-00–3 (2000).

11

11. M. Yabashi, A. Higashiya, K. Tamasaku, H. Kimura, T. Kudo, H. Ohashi, S. Takahashi, S. Goto, and T. Ishikawa, “Optics development for Japanese XFEL project,” Proc. SPIE 6586, 658605, 658605-9 (2007). [CrossRef]

]. Damage by FEL irradiation has been investigated in the extreme ultraviolet (EUV) and the soft X-ray regions [12

12. N. Stojanovic, D. von der Linde, K. Sokolowski-Tinten, U. Zastrau, F. Perner, E. Förster, R. Sobierajski, R. Nietubyc, M. Jurek, D. Klinger, J. Pelka, J. Krzywinski, L. Juha, J. Cihelka, A. Velyhan, S. Koptyaev, V. Hajkova, J. Chalupsky, J. Kuba, T. Tschentscher, S. Toleikis, S. Düsterer, and H. Redlin, “Ablation of solids using a femtosecond extreme ultraviolet free electron laser,” Appl. Phys. Lett. 89(24), 241909 (2006). [CrossRef]

16

16. S. P. Hau-Riege, R. A. London, A. Graf, S. L. Baker, R. Soufli, R. Sobierajski, T. Burian, J. Chalupsky, L. Juha, J. Gaudin, J. Krzywinski, S. Moeller, M. Messerschmidt, J. Bozek, and C. Bostedt, “Interaction of short x-ray pulses with low-Z x-ray optics materials at the LCLS free-electron laser,” Opt. Express 18(23), 23933–23938 (2010). [CrossRef] [PubMed]

]. David et al. have reported on the ablation phenomenon of gold at a photon energy of 8 keV [17

17. C. David, S. Gorelick, S. Rutishauser, J. Krzywinski, J. Vila-Comamala, V. A. Guzenko, O. Bunk, E. Färm, M. Ritala, M. Cammarata, D. M. Fritz, R. Barrett, L. Samoylova, J. Grünert, and H. Sinn, “Nanofocusing of hard X-ray free electron laser pulses using diamond based Fresnel zone plates,” Sci Rep 1, 57 (2011). [CrossRef] [PubMed]

]. In this paper, we report on our systematic study of the damage thresholds for various optical materials by using a hard X-ray free electron laser (FEL).

We used a focused XFEL beam at a photon energy of 10 keV, which has a sufficient power density to study ablation phenomena. We designed and installed a dedicated experimental chamber for the precise alignment of the position and incident angle of the samples. We used uncoated silicon and SiO2 substrates, as well as the metal (platinum and rhodium) coating on these substrates, which are widely used for X-ray optics as samples. We performed irradiation studies on a single shot and for a normal incidence condition.

2. Experiment

The experiments were carried out at beamline 3 (BL3) of the SACLA [3

3. T. Ishikawa, H. Aoyagi, T. Asaka, Y. Asano, N. Azumi, T. Bizen, H. Ego, K. Fukami, T. Fukui, Y. Furukawa, S. Goto, H. Hanaki, T. Hara, T. Hasegawa, T. Hatsui, A. Higashiya, T. Hirono, N. Hosoda, M. Ishii, T. Inagaki, Y. Inubushi, T. Itoga, Y. Joti, M. Kago, T. Kameshima, H. Kimura, Y. Kirihara, A. Kiyomichi, T. Kobayashi, C. Kondo, T. Kudo, H. Maesaka, X. M. Maréchal, T. Masuda, S. Matsubara, T. Matsumoto, T. Matsushita, S. Matsui, M. Nagasono, N. Nariyama, H. Ohashi, T. Ohata, T. Ohshima, S. Ono, Y. Otake, C. Saji, T. Sakurai, T. Sato, K. Sawada, T. Seike, K. Shirasawa, T. Sugimoto, S. Suzuki, S. Takahashi, H. Takebe, K. Takeshita, K. Tamasaku, H. Tanaka, R. Tanaka, T. Tanaka, T. Togashi, K. Togawa, A. Tokuhisa, H. Tomizawa, K. Tono, S. Wu, M. Yabashi, M. Yamaga, A. Yamashita, K. Yanagida, C. Zhang, T. Shintake, H. Kitamura, and N. Kumagai, “A compact X-ray free-electron laser emitting in the sub-ångstrom region,” Nat. Photonics 6(8), 540–544 (2012). [CrossRef]

]. During the experiments, SACLA was operated at a mean pulse energy of 130 µJ, a pulse duration of 20 fs [18

18. Y. Inubushi, K. Tono, T. Togashi, T. Sato, T. Hatsui, T. Kameshima, K. Togawa, T. Hara, T. Tanaka, H. Tanaka, T. Ishikawa, and M. Yabashi, “Determination of the pulse duration of an X-ray free electron laser using highly resolved single-shot spectra,” Phys. Rev. Lett. 109(14), 144801 (2012). [CrossRef] [PubMed]

], and a pulse repetition rate of 10 Hz. The X-ray photon energy was chosen to be 10 keV. The unwanted contamination of higher-order harmonics and gamma-rays were suppressed using a double-mirror system in the optics hutch. The XFEL light was focused down to a diameter of 1 µm (FWHM) using the mirror system [19

19. H. Yumoto, H. Mimura, T. Koyama, S. Matsuyama, K. Tono, T. Togashi, Y. Inubushi, T. Sato, T. Tanaka, T. Kimura, H. Yokoyama, J. Kim, Y. Sano, Y. Hachisu, M. Yabashi, H. Ohashi, H. Ohmori, T. Ishikawa, and K. Yamauchi, “Focusing of X-ray free electron laser with reflective optics,” Nat. Photonics 7(1), 43–47 (2012). [CrossRef]

] that consists of two carbon-coated elliptical mirrors in a Kirkpatrick–Baez configuration. The focusing mirror system was located 115 m downstream from the exit of the final undulator.

An irradiation chamber was designed and installed at the focal point of the focusing mirror system, as shown in Fig. 1(a)
Fig. 1 (a) Photograph of experimental chamber. OM: Optical microscope for observation of the sample surface. (b) Photograph of area around sample holder inside chamber. (c) Schematic drawing of sample stage configuration. The sample holder is mounted on the XYZ translation stages. These stages are placed on the rotation stage.
. The samples were mounted on high precision stages at a motion range of 50 mm in the vertical and horizontal directions perpendicular to the optical axis, as well as at 15 mm along the optical axis, as shown in Figs. 1(b) and 1(c). A rotation stage was used for adjusting the incident angle, the motion range of which is from −10 to + 100 degrees. The stage specifications are summarized in Table 1

Table 1. Stage specifications

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. The surface of the samples is monitored by an optical microscope at an angle of 30 degrees for the normal incidence condition, and at an angle of 90 degrees for the grazing incidence condition, as shown in Fig. 1(a). A knife-edge scanning method was used for measuring the profile of the focused beam. The excellent pointing stability of the XFEL light from SACLA made it possible to accurately evaluate the beam profile and the irradiation area.

The pulse energy was controlled by silicon attenuators of various thicknesses inserted in front of the focusing mirrors. The shot-to-shot fluctuations of the pulse energy were monitored by using a scattering-based beam intensity monitor [20

20. K. Tono, T. Kudo, M. Yabashi, T. Tachibana, Y. Feng, D. Fritz, J. Hastings, and T. Ishikawa, “Single-shot beam-position monitor for x-ray free electron laser,” Rev. Sci. Instrum. 82(2), 023108 (2011). [CrossRef] [PubMed]

], which was calibrated by a cryogenic radiometer [21

21. M. Kato, T. Tanaka, T. Kurosawa, N. Saito, M. Richter, A. A. Sorokin, K. Tiedtke, T. Kudo, K. Tono, M. Yabashi, and T. Ishikawa, “Pulse energy measurement at the hard x-ray laser in Japan,” Appl. Phys. Lett. 101(2), 023503 (2012). [CrossRef]

]. Measured pulse energy accuracy was within the range of ± 3.5% around the X-ray energy used in this experiment. Single shot irradiations at a normal incidence condition at a pulse energy ranging from 0.001 to 100 µJ were used in this experiment. The sample was moved with constant speed during the exposure. The number of shots was controlled by using a pulse selector [22

22. T. Kudo, T. Hirono, M. Nagasono, and M. Yabashi, “Vacuum-compatible pulse selector for free-electron laser,” Rev. Sci. Instrum. 80(9), 093301 (2009). [CrossRef] [PubMed]

]. The ablation thresholds of the samples were evaluated by measuring the diameters of the imprinted ablation profiles using scanning probe microscopy (SPM) and scanning electron microscopy (SEM).

3. Results and discussion

Figure 2
Fig. 2 (a) Optical microscope image of irradiated silicon viewed from surface at fluence of 57 µJ/µm2. (b) Cross sectional SEM image of (a) prepared by focused ion beam sampling.
shows one of the typical imprints of silicon irradiated at high fluence without any attenuators. The optical microscope image for the surface is shown in Fig. 2(a). The irradiated fluence inside the crater was 57 µJ/µm2, which was several tens of orders of magnitude higher than the melting dose of silicon. Spallation and cracks were observed around an area of 40 µm on the surface. The cross sectional SEM image prepared using focused ion beam sampling is shown in Fig. 2(b). For the cross sectional SEM image, the crater depth and the diameter were measured to be 40 and 4 µm, respectively. A large volume of melted and/or evaporated silicon was ejected from the inside, and a straight side wall was formed. Therefore, a deep ablation phenomenon was observed. Although the attenuation length of silicon is 134 µm for 10 keV of photon energy, the 40-µm crater depth is small. The reason for this may be as follows. Ablated silicon in the region deeper than the bottom of the crater cannot be ejected outside, so solidification occurs and it is probably in the amorphous state. It is difficult to observe from the SEM images because they are only sensitive to the surface morphology.

We evaluated the ablation thresholds of uncoated silicon and SiO2 substrate by varying the intensity using Liu’s technique [23

23. J. M. Liu, “Simple technique for measurements of pulsed Gaussian-beam spot sizes,” Opt. Lett. 7(5), 196–198 (1982). [CrossRef] [PubMed]

]. The imprint areas were plotted as a function of the fluence, as shown in Fig. 3(a)
Fig. 3 Imprint areas plotted as function of fluence. (a) Uncoated Si and SiO2 substrates, (b) Pt coating layer and SiO2 substrate under this layer.
. The obtained threshold fluence Fth was 0.78 ± 0.04 µJ/µm2 (4.5 ± 0.7 µJ/µm2) in silicon (SiO2), which was converted to the dose D for a single atom [9

9. R. M. Bionta, “Controlling dose to low Z solids at LCLS ,” LCLS Technical Note No. LCLS-TN-00–3 (2000).

11

11. M. Yabashi, A. Higashiya, K. Tamasaku, H. Kimura, T. Kudo, H. Ohashi, S. Takahashi, S. Goto, and T. Ishikawa, “Optics development for Japanese XFEL project,” Proc. SPIE 6586, 658605, 658605-9 (2007). [CrossRef]

], as follow; the dose D is given by D=FthμA/(ρNA), where μ, A, σ, ρ, and NA are the absorption coefficient, the average atomic weight, the RMS beam size, the average density, and the Avogadro’s constant, respectively. Converted dose was 0.73 ± 0.04 eV/atom (1.7 ± 0.3 eV/atom). This value reasonably agrees with the calculated melting dose of 0.88 eV/atom (1.1 eV/atom). The melting dose was calculated from the thermodynamic properties, which took into consideration the temperature dependent heat capacity and the latent heat of melting [24

24. NIST Chemistry WebBook, NIST Standard Reference Database Number 69. http://webbook.nist.gov/chemistry/

]. Note that we did not include effects of electron transport in this calculation.

We used a 200-nm-thick platinum layer coated on silicon and SiO2 substrates as the metal coating samples. The inserted adhesive layer was 5-nm-thick chromium. The imprint areas of the platinum layer and the SiO2 substrate under the coating layer were plotted in Fig. 3(b) as a function of the fluence. The ablation threshold of the platinum was evaluated to be 0.023 ± 0.004 µJ/µm2 (0.52 ± 0.09 eV/atom). This value reasonably agrees with the calculated melting dose of 0.78 eV/atom. However, the ablation threshold of the SiO2 substrate under the coating layer was evaluated to be 0.11 ± 0.03 µJ/µm2 (0.04 ± 0.01 eV/atom), while that of the uncoated SiO2 substrate was 4.5 ± 0.7 µJ/µm2 (1.7 ± 0.3 eV/atom) as obtained above. This value was 40 times lower than that of the uncoated substrate. Figures 4(a)
Fig. 4 (a–c) Imprint SEM images of platinum coated SiO2 at fluences of 0.3, 2.6, and 8.6 µJ/µm2. Observed SEM images were viewed under an angle of 30°. The imprint diameters of the platinum layer were 2.1, 4.0, and 4.9 µm, respectively. (d–f) Cross sectional profiles of these craters measured by SPM. In the case of the crater irradiated by a fluence of 8.6 µJ/µm2, the SPM probe cannot reach the bottom of the crater. The dashed line indicated the interface between the Pt layer and the SiO2 substrate.
4(c) show the SEM images of the imprints formed on the platinum layer coated SiO2 substrate for a detailed observation of the surface morphology. Figures 4(d)4(f) show cross sectional profiles of these craters. Shallow craters appeared in the substrate region for the 0.3 µJ/µm2 and 2.6 µJ/µm2 fluences. Notably, these fluences are lower than the threshold fluence for the uncoated SiO2 substrate (4.5 µJ/µm2). Similar results were observed for the silicon substrate and other coating materials such as rhodium. In the case of silicon substrate under platinum coating layer, the ablation threshold was evaluated to be 0.065 ± 0.008µJ/µm2 (0.060 ± 0.007 eV/atom). This value was 10 times lower than that of the uncoated substrate. Furthermore, we used a 75-nm-thick rhodium layer coated on silicon and SiO2 substrates as the other metal coating samples. The inserted adhesive layer was 10-nm-thick chromium. We confirmed that the substrate behavior was the same with platinum coatings.

The measured threshold fluences and calculated melting doses were summarized in Table 2

Table 2. Measured threshold fluences, corresponding doses, and calculated melting doses.

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. The measured threshold values for the uncoated substrate and metal coating layer agreed with the calculated melting dose. However, the thresholds of the substrates under the coating layer were significantly lower than that for the uncoated substrates; the ratio was 1/10 for silicon and 1/40 for SiO2.

As seen in Fig. 3(b), differential coefficient of the measured imprint area of SiO2 underneath coating as a function of fluence is changed clearly. The inflection point is nearly threshold fluence of uncoated substrate. For higher fluence than the threshold, large size craters were formed, as shown in Fig. 4(c), by direct interaction with intense X-rays to the substrate. Note that X-ray transmissions through the coating are as high as 95.4% for 200-nm-thick platinum layer and 99% for 75-nm-thick rhodium layer for 10 keV X-rays. On the other hand, for lower fluence, shallow craters were formed as shown in Fig. 4(a) and 4(c). The damage of the substrate underneath coating could originate from collisions of energetic particles (electrons, ions, and neutrals) that are generated with intense X-rays in the coating region.

4. Summary

We have measured the ablation thresholds of optical materials that are widely use as X-ray mirrors. A focusing hard X-ray FEL beam at a beam size of 1 µm was used. We found that the measured ablation thresholds of uncoated silicon and a SiO2 substrate, as well as a metal (platinum and rhodium) thin film are comparable to the melting dose, while the substrates under the metal coating layer showed that they are easily damaged. These results should be useful criteria for designing X-ray optics.

Acknowledgments

The authors would like to sincerely thank Takanori Miura for his support in measuring the samples, and Hikaru Kishimoto and the SACLA engineering team for their help during the beam time. This work was performed at the BL3 of SACLA with the approval of the Japan Synchrotron Radiation Research Institute (JASRI) (Proposal No. 2012A8056). This research was partially supported by a Grant-in-Aid for Scientific Research (S) (23226004) from the Ministry of Education, Sports, Culture, Science and Technology, Japan (MEXT).

References and links

1.

B. W. J. McNeil and N. R. Thompson, “X-ray free-electron lasers,” Nat. Photonics 4(12), 814–821 (2010). [CrossRef]

2.

P. Emma, R. Akre, J. Arthur, R. Bionta, C. Bostedt, J. Bozek, A. Brachmann, P. Bucksbaum, R. Coffee, F.-J. Decker, Y. Ding, D. Dowell, S. Edstrom, A. Fisher, J. Frisch, S. Gilevich, J. Hastings, G. Hays, Ph. Hering, Z. Huang, R. Iverson, H. Loos, M. Messerschmidt, A. Miahnahri, S. Moeller, H.-D. Nuhn, G. Pile, D. Ratner, J. Rzepiela, D. Schultz, T. Smith, P. Stefan, H. Tompkins, J. Turner, J. Welch, W. White, J. Wu, G. Yocky, and J. Galayda, “First lasing and operation of an ångstrom-wavelength free-electron laser,” Nat. Photonics 4(9), 641–647 (2010). [CrossRef]

3.

T. Ishikawa, H. Aoyagi, T. Asaka, Y. Asano, N. Azumi, T. Bizen, H. Ego, K. Fukami, T. Fukui, Y. Furukawa, S. Goto, H. Hanaki, T. Hara, T. Hasegawa, T. Hatsui, A. Higashiya, T. Hirono, N. Hosoda, M. Ishii, T. Inagaki, Y. Inubushi, T. Itoga, Y. Joti, M. Kago, T. Kameshima, H. Kimura, Y. Kirihara, A. Kiyomichi, T. Kobayashi, C. Kondo, T. Kudo, H. Maesaka, X. M. Maréchal, T. Masuda, S. Matsubara, T. Matsumoto, T. Matsushita, S. Matsui, M. Nagasono, N. Nariyama, H. Ohashi, T. Ohata, T. Ohshima, S. Ono, Y. Otake, C. Saji, T. Sakurai, T. Sato, K. Sawada, T. Seike, K. Shirasawa, T. Sugimoto, S. Suzuki, S. Takahashi, H. Takebe, K. Takeshita, K. Tamasaku, H. Tanaka, R. Tanaka, T. Tanaka, T. Togashi, K. Togawa, A. Tokuhisa, H. Tomizawa, K. Tono, S. Wu, M. Yabashi, M. Yamaga, A. Yamashita, K. Yanagida, C. Zhang, T. Shintake, H. Kitamura, and N. Kumagai, “A compact X-ray free-electron laser emitting in the sub-ångstrom region,” Nat. Photonics 6(8), 540–544 (2012). [CrossRef]

4.

L. Young, E. P. Kanter, B. Krässig, Y. Li, A. M. March, S. T. Pratt, R. Santra, S. H. Southworth, N. Rohringer, L. F. Dimauro, G. Doumy, C. A. Roedig, N. Berrah, L. Fang, M. Hoener, P. H. Bucksbaum, J. P. Cryan, S. Ghimire, J. M. Glownia, D. A. Reis, J. D. Bozek, C. Bostedt, and M. Messerschmidt, “Femtosecond electronic response of atoms to ultra-intense X-rays,” Nature 466(7302), 56–61 (2010). [CrossRef] [PubMed]

5.

N. Rohringer, D. Ryan, R. A. London, M. Purvis, F. Albert, J. Dunn, J. D. Bozek, C. Bostedt, A. Graf, R. Hill, S. P. Hau-Riege, and J. J. Rocca, “Atomic inner-shell X-ray laser at 1.46 nanometres pumped by an X-ray free-electron laser,” Nature 481(7382), 488–491 (2012). [CrossRef] [PubMed]

6.

S. M. Vinko, O. Ciricosta, B. I. Cho, K. Engelhorn, H.-K. Chung, C. R. D. Brown, T. Burian, J. Chalupský, R. W. Falcone, C. Graves, V. Hájková, A. Higginbotham, L. Juha, J. Krzywinski, H. J. Lee, M. Messerschmidt, C. D. Murphy, Y. Ping, A. Scherz, W. Schlotter, S. Toleikis, J. J. Turner, L. Vysin, T. Wang, B. Wu, U. Zastrau, D. Zhu, R. W. Lee, P. A. Heimann, B. Nagler, and J. S. Wark, “Creation and diagnosis of a solid-density plasma with an X-ray free-electron laser,” Nature 482(7383), 59–62 (2012). [CrossRef] [PubMed]

7.

H. N. Chapman, P. Fromme, A. Barty, T. A. White, R. A. Kirian, A. Aquila, M. S. Hunter, J. Schulz, D. P. DePonte, U. Weierstall, R. B. Doak, F. R. N. C. Maia, A. V. Martin, I. Schlichting, L. Lomb, N. Coppola, R. L. Shoeman, S. W. Epp, R. Hartmann, D. Rolles, A. Rudenko, L. Foucar, N. Kimmel, G. Weidenspointner, P. Holl, M. Liang, M. Barthelmess, C. Caleman, S. Boutet, M. J. Bogan, J. Krzywinski, C. Bostedt, S. Bajt, L. Gumprecht, B. Rudek, B. Erk, C. Schmidt, A. Hömke, C. Reich, D. Pietschner, L. Strüder, G. Hauser, H. Gorke, J. Ullrich, S. Herrmann, G. Schaller, F. Schopper, H. Soltau, K. U. Kühnel, M. Messerschmidt, J. D. Bozek, S. P. Hau-Riege, M. Frank, C. Y. Hampton, R. G. Sierra, D. Starodub, G. J. Williams, J. Hajdu, N. Timneanu, M. M. Seibert, J. Andreasson, A. Rocker, O. Jönsson, M. Svenda, S. Stern, K. Nass, R. Andritschke, C. D. Schröter, F. Krasniqi, M. Bott, K. E. Schmidt, X. Wang, I. Grotjohann, J. M. Holton, T. R. Barends, R. Neutze, S. Marchesini, R. Fromme, S. Schorb, D. Rupp, M. Adolph, T. Gorkhover, I. Andersson, H. Hirsemann, G. Potdevin, H. Graafsma, B. Nilsson, and J. C. Spence, “Femtosecond X-ray protein nanocrystallography,” Nature 470(7332), 73–77 (2011). [CrossRef] [PubMed]

8.

M. M. Seibert, T. Ekeberg, F. R. N. C. Maia, M. Svenda, J. Andreasson, O. Jönsson, D. Odić, B. Iwan, A. Rocker, D. Westphal, M. Hantke, D. P. DePonte, A. Barty, J. Schulz, L. Gumprecht, N. Coppola, A. Aquila, M. Liang, T. A. White, A. Martin, C. Caleman, S. Stern, C. Abergel, V. Seltzer, J.-M. Claverie, C. Bostedt, J. D. Bozek, S. Boutet, A. A. Miahnahri, M. Messerschmidt, J. Krzywinski, G. Williams, K. O. Hodgson, M. J. Bogan, C. Y. Hampton, R. G. Sierra, D. Starodub, I. Andersson, S. Bajt, M. Barthelmess, J. C. H. Spence, P. Fromme, U. Weierstall, R. Kirian, M. Hunter, R. B. Doak, S. Marchesini, S. P. Hau-Riege, M. Frank, R. L. Shoeman, L. Lomb, S. W. Epp, R. Hartmann, D. Rolles, A. Rudenko, C. Schmidt, L. Foucar, N. Kimmel, P. Holl, B. Rudek, B. Erk, A. Hömke, C. Reich, D. Pietschner, G. Weidenspointner, L. Strüder, G. Hauser, H. Gorke, J. Ullrich, I. Schlichting, S. Herrmann, G. Schaller, F. Schopper, H. Soltau, K.-U. Kühnel, R. Andritschke, C.-D. Schröter, F. Krasniqi, M. Bott, S. Schorb, D. Rupp, M. Adolph, T. Gorkhover, H. Hirsemann, G. Potdevin, H. Graafsma, B. Nilsson, H. N. Chapman, and J. Hajdu, “Single mimivirus particles intercepted and imaged with an X-ray laser,” Nature 470(7332), 78–81 (2011). [CrossRef] [PubMed]

9.

R. M. Bionta, “Controlling dose to low Z solids at LCLS ,” LCLS Technical Note No. LCLS-TN-00–3 (2000).

10.

R. A. London, R. M. Bionta, R. O. Tatchyn, and S. Roesler, “Computational simulations of high intensity x-ray matter interaction,” Proc. SPIE 4500, 51–62 (2001). [CrossRef]

11.

M. Yabashi, A. Higashiya, K. Tamasaku, H. Kimura, T. Kudo, H. Ohashi, S. Takahashi, S. Goto, and T. Ishikawa, “Optics development for Japanese XFEL project,” Proc. SPIE 6586, 658605, 658605-9 (2007). [CrossRef]

12.

N. Stojanovic, D. von der Linde, K. Sokolowski-Tinten, U. Zastrau, F. Perner, E. Förster, R. Sobierajski, R. Nietubyc, M. Jurek, D. Klinger, J. Pelka, J. Krzywinski, L. Juha, J. Cihelka, A. Velyhan, S. Koptyaev, V. Hajkova, J. Chalupsky, J. Kuba, T. Tschentscher, S. Toleikis, S. Düsterer, and H. Redlin, “Ablation of solids using a femtosecond extreme ultraviolet free electron laser,” Appl. Phys. Lett. 89(24), 241909 (2006). [CrossRef]

13.

S. P. Hau-Riege, R. A. London, R. M. Bionta, M. A. McKernan, S. L. Baker, J. Krzywinski, R. Sobierajski, R. Nietubyc, J. B. Pelka, M. Jurek, L. Juha, J. Chalupský, J. Cihelka, V. Hájková, A. Velyhan, J. Krása, J. Kuba, K. Tiedtke, S. Toleikis, Th. Tschentscher, H. Wabnitz, M. Bergh, C. Caleman, K. Sokolowski-Tinten, N. Stojanovic, and U. Zastrau, “Damage threshold of inorganic solids under free-electron-laser irradiation at 32.5 nm wavelength,” Appl. Phys. Lett. 90(17), 173128 (2007). [CrossRef]

14.

R. Sobierajski, D. Klinger, M. Jurek, J. B. Pelka, L. Juha, J. Chalupský, J. Cihelka, V. Hakova, L. Vysin, U. Jastrow, N. Stojanovic, S. Toleikis, H. Wabnitz, J. Krzywinski, S. Hau-Reige, and R. London, “Interaction of intense ultrashort XUV pulses with silicon,” Proc. SPIE 7361, 736107 (2009). [CrossRef]

15.

J. Gaudin, C. Ozkan, J. Chalupský, S. Bajt, T. Burian, L. Vyšín, N. Coppola, S. D. Farahani, H. N. Chapman, G. Galasso, V. Hájková, M. Harmand, L. Juha, M. Jurek, R. A. Loch, S. Möller, M. Nagasono, M. Störmer, H. Sinn, K. Saksl, R. Sobierajski, J. Schulz, P. Sovak, S. Toleikis, K. Tiedtke, T. Tschentscher, and J. Krzywinski, “Investigating the interaction of x-ray free electron laser radiation with grating structure,” Opt. Lett. 37(15), 3033–3035 (2012). [CrossRef] [PubMed]

16.

S. P. Hau-Riege, R. A. London, A. Graf, S. L. Baker, R. Soufli, R. Sobierajski, T. Burian, J. Chalupsky, L. Juha, J. Gaudin, J. Krzywinski, S. Moeller, M. Messerschmidt, J. Bozek, and C. Bostedt, “Interaction of short x-ray pulses with low-Z x-ray optics materials at the LCLS free-electron laser,” Opt. Express 18(23), 23933–23938 (2010). [CrossRef] [PubMed]

17.

C. David, S. Gorelick, S. Rutishauser, J. Krzywinski, J. Vila-Comamala, V. A. Guzenko, O. Bunk, E. Färm, M. Ritala, M. Cammarata, D. M. Fritz, R. Barrett, L. Samoylova, J. Grünert, and H. Sinn, “Nanofocusing of hard X-ray free electron laser pulses using diamond based Fresnel zone plates,” Sci Rep 1, 57 (2011). [CrossRef] [PubMed]

18.

Y. Inubushi, K. Tono, T. Togashi, T. Sato, T. Hatsui, T. Kameshima, K. Togawa, T. Hara, T. Tanaka, H. Tanaka, T. Ishikawa, and M. Yabashi, “Determination of the pulse duration of an X-ray free electron laser using highly resolved single-shot spectra,” Phys. Rev. Lett. 109(14), 144801 (2012). [CrossRef] [PubMed]

19.

H. Yumoto, H. Mimura, T. Koyama, S. Matsuyama, K. Tono, T. Togashi, Y. Inubushi, T. Sato, T. Tanaka, T. Kimura, H. Yokoyama, J. Kim, Y. Sano, Y. Hachisu, M. Yabashi, H. Ohashi, H. Ohmori, T. Ishikawa, and K. Yamauchi, “Focusing of X-ray free electron laser with reflective optics,” Nat. Photonics 7(1), 43–47 (2012). [CrossRef]

20.

K. Tono, T. Kudo, M. Yabashi, T. Tachibana, Y. Feng, D. Fritz, J. Hastings, and T. Ishikawa, “Single-shot beam-position monitor for x-ray free electron laser,” Rev. Sci. Instrum. 82(2), 023108 (2011). [CrossRef] [PubMed]

21.

M. Kato, T. Tanaka, T. Kurosawa, N. Saito, M. Richter, A. A. Sorokin, K. Tiedtke, T. Kudo, K. Tono, M. Yabashi, and T. Ishikawa, “Pulse energy measurement at the hard x-ray laser in Japan,” Appl. Phys. Lett. 101(2), 023503 (2012). [CrossRef]

22.

T. Kudo, T. Hirono, M. Nagasono, and M. Yabashi, “Vacuum-compatible pulse selector for free-electron laser,” Rev. Sci. Instrum. 80(9), 093301 (2009). [CrossRef] [PubMed]

23.

J. M. Liu, “Simple technique for measurements of pulsed Gaussian-beam spot sizes,” Opt. Lett. 7(5), 196–198 (1982). [CrossRef] [PubMed]

24.

NIST Chemistry WebBook, NIST Standard Reference Database Number 69. http://webbook.nist.gov/chemistry/

OCIS Codes
(140.2600) Lasers and laser optics : Free-electron lasers (FELs)
(160.4670) Materials : Optical materials
(340.0340) X-ray optics : X-ray optics

ToC Category:
Materials

History
Original Manuscript: March 29, 2013
Revised Manuscript: May 22, 2013
Manuscript Accepted: May 22, 2013
Published: June 20, 2013

Citation
Takahisa Koyama, Hirokatsu Yumoto, Yasunori Senba, Kensuke Tono, Takahiro Sato, Tadashi Togashi, Yuichi Inubushi, Tetsuo Katayama, Jangwoo Kim, Satoshi Matsuyama, Hidekazu Mimura, Makina Yabashi, Kazuto Yamauchi, Haruhiko Ohashi, and Tetsuya Ishikawa, "Investigation of ablation thresholds of optical materials using 1-µm-focusing beam at hard X-ray free electron laser," Opt. Express 21, 15382-15388 (2013)
http://www.opticsinfobase.org/oe/abstract.cfm?URI=oe-21-13-15382


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References

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  13. S. P. Hau-Riege, R. A. London, R. M. Bionta, M. A. McKernan, S. L. Baker, J. Krzywinski, R. Sobierajski, R. Nietubyc, J. B. Pelka, M. Jurek, L. Juha, J. Chalupský, J. Cihelka, V. Hájková, A. Velyhan, J. Krása, J. Kuba, K. Tiedtke, S. Toleikis, Th. Tschentscher, H. Wabnitz, M. Bergh, C. Caleman, K. Sokolowski-Tinten, N. Stojanovic, and U. Zastrau, “Damage threshold of inorganic solids under free-electron-laser irradiation at 32.5 nm wavelength,” Appl. Phys. Lett.90(17), 173128 (2007). [CrossRef]
  14. R. Sobierajski, D. Klinger, M. Jurek, J. B. Pelka, L. Juha, J. Chalupský, J. Cihelka, V. Hakova, L. Vysin, U. Jastrow, N. Stojanovic, S. Toleikis, H. Wabnitz, J. Krzywinski, S. Hau-Reige, and R. London, “Interaction of intense ultrashort XUV pulses with silicon,” Proc. SPIE7361, 736107 (2009). [CrossRef]
  15. J. Gaudin, C. Ozkan, J. Chalupský, S. Bajt, T. Burian, L. Vyšín, N. Coppola, S. D. Farahani, H. N. Chapman, G. Galasso, V. Hájková, M. Harmand, L. Juha, M. Jurek, R. A. Loch, S. Möller, M. Nagasono, M. Störmer, H. Sinn, K. Saksl, R. Sobierajski, J. Schulz, P. Sovak, S. Toleikis, K. Tiedtke, T. Tschentscher, and J. Krzywinski, “Investigating the interaction of x-ray free electron laser radiation with grating structure,” Opt. Lett.37(15), 3033–3035 (2012). [CrossRef] [PubMed]
  16. S. P. Hau-Riege, R. A. London, A. Graf, S. L. Baker, R. Soufli, R. Sobierajski, T. Burian, J. Chalupsky, L. Juha, J. Gaudin, J. Krzywinski, S. Moeller, M. Messerschmidt, J. Bozek, and C. Bostedt, “Interaction of short x-ray pulses with low-Z x-ray optics materials at the LCLS free-electron laser,” Opt. Express18(23), 23933–23938 (2010). [CrossRef] [PubMed]
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