Development of Full-field XRD (FFXRD) imaging method realized in the laboratory using a straight polycapillary and in situ observation of the oxidation process of cu by heat treatment

Abstract

We developed a full-field X-ray diffraction (FFXRD) imaging method using a straight polycapillary realized in the laboratory that can obtain X-ray diffraction (XRD) images with a large area in a short time throughout the simple process without the synchrotron radiation facility. The FFXRD imaging instrument can obtain the XRD images of several millimeter sizes in several hundreds of seconds at each lattice plane. The positional resolution and the spatial resolution was improved by using a straight polycapillary with long type. The FFXRD imaging instrument was attached to the heat treatment system and Cu plate was heat-treated at 300°C. As an example of in situ monitoring of the change in the crystal structure distribution, a high-temperature oxidation process of Cu was observed. The XRD images of Cu, Cu2O, and CuO at each lattice plane were obtained every hour. While the crystal structure distribution of Cu was reduced, the crystal structure distribution of Cu2O and CuO were increased with the oxidation process of Cu by the heat treatment. The change of the crystal structure distribution near the surface by the oxidation process of Cu was confirmed. The XRD image obtained by the FFXRD imaging instrument was analyzed by micro-XRD measurements and confirmed that the FFXRD imaging instrument can accurately obtain the crystal structure distribution. In order to obtain the XRD image with a large area, the FFXRD imaging instrument that can be realized in the laboratory has advantages regarding the exposure time of X-rays and in situ analysis.