X線分析の進歩38 別刷

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1 X kev Instrumentation for High-Resolution X-Ray Fluorescence Spectroscopy in kev Region Kenji SAKURAI, Mari MIZUSAWA and Yasuko TERADA Copyright The Discussion Group of X-Ray Analysis, The Japan Society for Analytical Chemistry

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3 X kev Instrumentation for High-Resolution X-Ray Fluorescence Spectroscopy in kev Region Kenji SAKURAI, Mari MIZUSAWA and Yasuko TERADA National Institute for Materials Science Sengen, Tsukuba, Ibaraki , Japan Japan Synchrotron Radiation Research Institute, SPring-8 Sayo-gun, Hyogo , Japan Corresponding author: (Received 2 January 2007, Accepted 23 January 2007) Generally, it is not difficult to obtain X-ray fluorescence spectra with energy resolution of E/ E=1000 or even better, by employing suitable analyzing crystals. This, however, depends on the energy of X-rays to be measured - it is not valid for high energy region like kev. The present paper summarizes the technical difficulties of high-energy X-ray fluorescence spectroscopy, and describes the instrumentation to solve the problems. [Key words] Undulator radiation, High-energy X-rays, Spectrometer, Energyresolution, Lanthanides, Heavy elements, K-shell excitation E/ E = 1000 X X 35~60 kev X sakurai@yuhgiri.nims.go.jp Adv. X-Ray. Chem. Anal., Japan 38, pp (2007)

4 X K 1. X K 50 Sn 1 25 kev X X X X K 57 (La) 71 (Lu) K X kev L M K X 2,3 X X 3 ESRF European Synchrotron Radiation Facility, APS Advanced Photon Source SPring-8 3 X X SPring-8 8 GeV X 2003 BL37XU B 75.5 kev X 4 X Ge 5 kev 100 kev 5.9 kev X 150 ev E/ E = kev E/ E =

5 100 / 1 6 7,8 Kβ E/ E = 1000 X KEK PF-AR 160 Si(422) 3000 mm E/ E 800 at GdKβ ,10,11 X 60 kev 10 kev 70 kev X X X SPring-8 BL37XU-B 12 X 10 kev E/ E = ,14 X 2. X E/ E d [ ] θ θ E [kev] /(2d sinθ) E/ E tanθ / θ kev E E/ E = kev X X 10 kev 5 1 d sinθ 5 1 θ θ d / 3 = θ

6 2 θ θ X X θ X X 3 50 kev 10 kev 125 X X θ X Fig.1 Kβ 1 E/ E = 1000 X X Ge(220) Ge(331) 3 6 m 3 Ge(660) Ge(993) 1 2 m Spectrometer Length m La Ce Pr Nd Ge(220) Pm Sm Eu Gd Tb Ge(331) Dy Ho Er Tm Yb Lu Ge(660) Ge(993) Fig X-Ray Energy (kev) Design consideration of high-energy X-ray fluorescence spectrometer. The required spectrometer length is calculated for several different analyzing crystals. The condition is to obtain the energy resolution is E/ E = The effective size of illuminated part of the sample is assumed as 0.35 mm

7 X 0.35 mm mm 1 mm X 1 2 m 3. X SPring-8 BL37XU-B kev X Fig.2 Ge (t) mm mm X kev KEK PF-AR 1355mm Image plate Vac. pipe Ge(993) Shielding Box X-Y Slit Vac. pipe 325mm Ionization Chamber Incident X-rays (75.5keV) Sample Beam Stop Fig.2 470mm 1200mm Schematic drawings of the high-energy X-ray fluorescence spectrometer

8 422 9 X X 75.5 kev 10 ID mm 1 Si(111) photons/sec/mm 2 X ID mm 0.5 mm 1 mm Fig.2 XY X X X XY X mm X

9 1 2 BAS-IP MS mm 20 mm CCD 5 6 CCD X 4. E/ E = 1000 Kβ Kβ 1 Kβ 2 7 E/ E = 1000 Kβ 3 3p 1/2-1s Kβ 1 3p 3/2-1s Kβ 2 4p-1s KO II,III 5p-1s Kβ 2 1 1/3 X 3 20 µm Kα kev E/ E = 1000 Fig X Fig

10 Integrated Intensity (Norm.) Kα Energy [ev] Kα 1 Fig.3 Zr Kα spectra from metallic zirconium foil (20 micron thick). The spectra are obtained by 311 reflection of Ge flat single crystal ( (t) mm). Incident beam size was 0.3 mm (H) 1 mm (V). The energy resolution is better than E/ E = The inset shows raw X-ray image appeared on the image plate. Fig.4 Integrated Intensity (Norm.) Kβ 3 Kβ 1 Kβ 5 Kβ 2 Kβ 4 KO II,III Energy [ev] La Kβ spectra from LaAlO 3 single crystal. The spectra are obtained by 933 reflection of the same analyzing crystal used for the data shown in Fig.3. Incident beam size 0.5 mm (H) 1 mm (V). Measuring time 5h. The inset is the image plate data. Fig.4 LaAlO 3 LaKβ LaKβ kev Kβ 1 39 ev E/ E 1000 Kβ 1 Kβ

11 Integrated Intensity (Norm.) Kβ 3 Kβ 1 5 KO II,III Energy [ev] Fig.5 Gd Kβ spectra from pure metallic Gd pellet. The spectra are obtained by 933 reflection of the same analyzing crystal used for the data shown in Fig.3. Incident beam size 0.5 mm (H) 1 mm (V). Measuring time 5h. The inset is the image plate data. Kβ 1, Kβ 3, Kβ 5 Kβ 2, KO II,III 5 Kβ 3 Kβ 1 Kβ 2 KO II,III La Kβ 1 32 ev Fig.5 Gd Kβ GdKβ kev Kβ 1 52 ev Kβ 3 Kβ 1 Kβ 2 KO II,III 5 Kβ 2 Gd 7, s 5p 5s 4f 3d

12 s 2 4f 5d f 2 4 X X SPring kev X 2 Kβ SPring-8 BL37X-B 2004A0012-NXb, 2004B0244-NXb, 2005A0253-NXb, 2006A1022-NXb X 1 R.Jenkins: "An Introduction to X-Ray Spectrometery", (1974), (Heyden). 2 M.Harada, K.Sakurai: Jpn. J. Appl. Phys., 37, 2740 (1998). 3 M.Harada, K.Sakurai: Spectrochimica Acta, B54, 29 (1999). 4 Y.Terada, S.Goto, N.Takimoto, K.Takeshita, H.Yamazaki, Y.Shimizu, S.Takahashi, H.Ohashi, Y.Furukawa, T.Matsushita, T.Ohata, Y.Ishizawa, T.Uruga, H.Kitamura, T.Ishikawa, S.Hayahawa: AIP Conference Proceedings, 705 (Synchrotron Radiation Instrumentation 2003, San Francisco, USA) 376 (2004). 5 I.Nakai: "X-Ray Spectrometry: Recent Technological Advances", Edited by K.Tsuji, J.Injuk, R.Van Grieken, p.355 (2004), (John. Wiley Sons, New York)

13 6 S.Ali, S.F.Terracol, O.B.Drury, S.Friedrich: Nucl. Instrum. & Methods, A559, 542 (2006). 7 X 34, 195 (2003). 8 55, 433 (2006). 9 Y.Sakurai, M.Ito, T.Urai, Y.Tanaka, N.Sakai, T.Iwazumi, H.Kawata, M.Ando: Rev. Sci. Instrum., 63, 1190 (1992). 10 M.Harada, H.Eba, M.Shoji, K.Sakurai, I.Matsumoto, H. Kawata: Photon Factory Activity Report, #20, 287 (2002). 11 M.Shoji, M.Harada, K.Sakurai: Photon Factory Activity Report, #20, 288 (2002). 12 K.Sakurai, M.Mizusawa, Y.Terada: 5th International Conference on Synchrotron Radiation in Materials Science, Chicago, USA, July 30 - August 2, 2006, pp.srms K.Sakurai, H.Eba, KInoue, N.Yagi: Nucl. Instrum, & Methods, A , 1549 (2001). 14 X 35, 201 (2004). 15 (1999),

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