Energy Spectrometer on a Diffractometer using Charge-Coupled Device X-ray Detector

Hiroshi Abe,a Hiroyuki Saitoh,b Hironori Nakao,c Kazuki Itod and Ken-ichi Ohshimae

aDepartment of Materials Science and Engineering, National Defense Academy, 1-10-20 Hashirimizu, Yokosuka 239-8686, Japan
bSynchrotron Radiation Research Center, Japan Atomic Energy Research Institute, Mikazuki-cho, Sayo-gun, Hyogo 679-5148, Japan
cDepartment of Physics, Tohoku University, Sendai 980-8578, Japan
dLaboratory for Structural Biochemistry, RIKEN Harima Institute SPring-8 Center, 1-1-1 Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5148, Japan
eInstitute of Materials Science, University of Tsukuba, 1-1-1 Tennoudai, Tsukuba 305-8573, Japan

J. Appl. Cryst. 39 (2006) 767.

Abstract
A charge-coupled device (CCD) X-ray detector for inelastic X-ray scattering was installed at beamline BL-4C of the Photon Factory at the High Energy Accelerator Research Organization in Japan. A wavelength-dispersive X-ray spectrometer was mounted on a six-circle diffractometer. Energy spectra were obtained by the CCD X-ray detector and a curved highly oriented pyrolytic graphite analyser. By the combination of energy spectroscopy and diffraction, simultaneous real-time data acquisition of both the momentum and the energy transfer was performed.

Figure 1 Wavelength-dispersive X-ray spectroscopy was attached on the conventional 6-circle diffractometer. The charge-coupled device X-ray detector was mounted on 2qA arm. A curved highly oriented pyrolytic graphite was placed inside the analyzer house.



Figure 2 (a) Schematic of the mosaic crystal analyzing spectrometer. Focusing geometry in the beam optics was designed. (b) Schematic drawing of an inelastic scattering experiment in reciprocal space.


Figure 3 Channel positions of the charge-coupled device camera depend on the incident energies at the fixed 2qA value. Open circles show the channel positions of the observed peaks at each incident energies. The solid curve reveals the calculation result. The broken line shows linear relationship for a comparison. The scattered energy was corrected within 1 eV by the optic geometry (See text).




Figure 4 The inelastic X-ray scattering was observed at 8.330 keV using 220 Bragg reflection of Ni polycrystalline. Two peaks correspond to Bragg reflection and kb1 fluorescence, respectively. (a) The raw image of the charge-coupled device (CCD) X-ray detector, (b) two peak profiles after integration along the vertical direction of the CCD image. Experimental energy resolution, DE, was 20 eV and (c) a schematic diagram of 1s3p process.

Figure 5 Excitation energy dependence of the inelastic X-ray scattering spectra of Ni polycrystalline.

Figure 6 Excitation energy dependence of Bragg reflection and fluorescence (Kb1) with the charge-coupled device X-ray detector.

References

Abe, H., Saitoh, H., Ueno, T., Nakao, H., Matsuo, Y., Ohshima, K. & Matsumoto, H. (2003). J. Phys. Condens. Matter, 15, 1665.1676.
Gruner, S. M., Tate, M. W. & Eikenberry, E. F. (2002). Rev. Sci. Instrum. 73, 2815.2842.
Hamalainen, K., Hill, J. P., Huotari, S., Kao, C.-C., Berman, L. E., Kotani, A., Ide, T. Peng, J. L. & Greene, R. L. (2000). Phys. Rev. B, 61, 1836.1840.
Hayashi, H., Takeda, R., Udagawa, Y. & Kawamura, N. (2003). Phys. Rev. B, 68, 045122.
Ice, G. E. & Sparks, C. J. (1990). Nucl. Instrum. Methods A, 291, 110.116.
Reinhard, L., Robertson, J. L.,Moss, S. C., Ice, G. E., Zschack, P. & Sparks, C. J. (1992). Phys. Rev. B, 45, 2662.2676.
Schonfeld, B., Ice, G. E., Sparks, C. J., Haubold, H.-G., Schweika,W. & Shaffer, L. B. (1994). Phys. Status Solidi B, 183, 79.95.
Stragier, H., Cross, J. O., Rehr, J. J. & Sorensen, L. B. (1992). Phys. Rev. Lett. 69, 3064.3067.
Tate,M.W., Gruner, S.M. & Eikenberry, E. F. (1997). Rev. Sci. Instrum. 68, 47. 54.
Warren, B. E. (1990). X-ray Diffraction. New York: Dover.

ab@nda.ac.jp
Department of Materials Science and Engineering
National Defense Academy

Last Modified: April 1, 2009