Development of a system to analyse the structure of a submicrometre-sized single crystal by synchrotron X-ray diffraction

A system has been developed for the analysis of the structure of a submicrometer-sized single-crystal using synchrotron radiation (SR) at the Photon Factory (PF), KEK. The Laue method combined with an imaging plate was employed for the collection of diffracted intensities. To reduce background, the experiment was carried out in a vacuum and with a very thinly collimated incident X-ray beam. The system has been shown to reach a level where a molybdenum sphere with diameter as small as 0.8 μm was found to be twinned and the volume ratio of the twin domains was determined, together with an isotropic temperature factor, which was comparable with the value determined in the same experiment on another single-crystal sphere of almost the same size. It was in good agreement with that determined by a powder diffraction study. The present study showed that any single-crystal detectable under an optical microscope can be analysed and, further, that the diffraction intensities from a crystal with volume of 0.02 μm³, which is composed of 10⁹ atoms, can be detected.