面向古陶瓷无损分析的2D/3D微束X射线荧光谱仪的研制

The non-destructive analysis of chemical compositions of ancient ceramics based on X-ray fluorescence is an important method for the study of provenance and age and techniques and identifications of ancient ceramics. Due to its particularity and diversity, the 2D/3D micro-X-ray fluorescence based on polycapillary optics can not only non-destructive analysis of chemical compositions of thin glazes and color glaze in micro-area, but also can non-destructive analysis of chemical compositions of colors underglaze and elemental distributions in depth. This proposal will be continuous to develope in further based on the previous study. The high precision and high scale and heavy loading of four dimensions stage which controlled by closed loop stepper motors. The measured positions of samples will be accurate fixed by laser displacement sensor. The light elements will be detected by SDD detector with thin Be window in He path in the air. The total integrates of 2D/3D X-ray fluorescence spectrometer with 50W low power X-ray tube,polycapillary optics and auto control software will be developed. This proposal will provide the scientific instrument for the study and identifications of ancient ceramics. Moreover, it l will be widely used in the environmental science, geological science and materials science,etc.

基于X射线荧光分析的古陶瓷化学成分的无损分析是研究古陶瓷的产地、年代、工艺和真伪辨别等重要的分析手段。由于古陶瓷样品的特殊性和多样性，毛细管X光透镜聚焦的2D/3D微束X射线荧光分析不仅能无损分析古瓷器表面的薄釉层和微区的彩料，而且还能无损的分析釉下彩料的化学成分和元素深度分布等。本项目在前期项目资助的基础上，自主的研发重复度小于1微米闭环步进电机控制的高精度、大量程、高负荷的三维样品台；利用激光位移传感器精确地控制样品被测量点的位置；在大气中利用吹氦气和薄铍窗SDD X射线探测器等方法测量样品中轻元素的含量；再结合50瓦小功率微焦斑的X射线管、汇聚毛细多管X光透镜、谱仪自动化控制软件，研制微束X射线荧光分析和三维共聚焦的微束X射线荧光分析一体化的2D/3D X射线荧光荧光谱仪，为古陶瓷科技研究和真伪辨别等提供科学的分析仪器。本项目的研究在环境、地学和材料等领域也有着广泛的应用前景。

本项目根据国内外文物、环境、地学、材料和电子行业的需求，以古陶瓷的无损分析为主要目标，研制了一种毛细管聚焦的微束X射线荧光谱仪，具有元素的点、线和面分布的二维面扫描和三维共聚焦扫描分析的功能。主要研究内容包括，毛细管X光透镜与微焦斑X射线管的集成、激光位移传感器校正古陶瓷表面的不平整效应、CCD相机对样品分析点或扫描区域的精确定位、高精度大量程的四维样品台的研发、基于Labview的仪器控制软件的开发、matlab数据处理软件的开发（小波变换的能谱噪音降低、元素峰面积的拟合、基本参数法的元素定性和定量分析等）等。在本项目的资助下，已经完成了微束X射线荧光谱仪的研发工作，并研发样机一台，各项参数满足微束分析的要求，部分指标已经超越美国EDAX产品；本项目的研究为国内微束X射线荧光分析技术在环境、地学、考古和新材料等样品的分析提供了工具。