Sub-micron single crystal structure analysis using micro-focus synchrotron radiation - A development of X-ray pinpoint structure measurement at the SPring-8 (2)

Research and Utilization Division, Japan Synchrotron Radiation Research Institute (JASRI/SPring-8) / CREST* Graduate School of Material Science, University of Hyogo / CREST** Department of Inorganic Materials, Tokyo Institute of Technology*** RIKEN / CREST**** The Graduate School of Pure and Applied Sciences, Tsukuba University / CREST***** Department of Physical Science, Hiroshima University / CREST****** RIKEN / JASRI / CREST*******
â—‹Nobuhiro Yasuda* Haruno Murayama* Jungeun Kim* Yoshimitsu Fukuyama* Yoshiki Ozawa** Kimihiro Kimura** Nobuyuki Kitayama** Shingo Yoshida** Satoshi Wada*** Yoshihito Tanaka**** Yutaka Moritomo***** Shigeru Kimura* Yoshihiro Kuroiwa****** Koshiro Toriumi** Masaki Takata*******

X-ray pinpoint structure measurement is the research project carried out at the SPring-8. The purpose is to develop an advanced X-ray measurement technique in nano-meter spatial scale and/or pico-second time scale by using the pulse characteristics, high brilliance and high efficiency of third generation synchrotron radiation X-ray.
One of the key techniques of the project is "the sub-micron single crystal structure analysis technique", which can be attained by applying "high brilliance micro-focus technique". This technique shall not only allow the single crystal structure analysis even from single grain of powder sample for powder X-ray diffraction, but also enables us to investigate dynamics of chemical reaction and phase transition caused by applied field within sub-micron scale domain of device and materials.
The high-precision diffractometer system was developed and installed at BL40XU beamline. The main features for single crystal analysis are (1)zone plate X-ray focusing up to 1μm at sample point, (2)a high precision goniometer system which realize sample rotation within ±100nm/360deg., and (3)CCD detector for 2 dimensional data collection.
To achieve the technique for the sub-micron single crystal structure analysis, the intensity data measurements were applied for 2 x 2 x 2μm3 cytidine (C9H13N3O5) and 500 x 500 x 500nm3 BaTiO3 single crystals. By the one hour ω-oscillation measurements with the total oscillation range of 180 deg., data collection and structure analyses have succeeded. The reliability factors of the present refinements were R1=6.4% for cytidine and 4.8% for BaTiO3, respectively.
Details of the data collection and structure analysis and precision of the refined structures will be discussed in the presentation.