钢铁材料复合夹杂物的聚焦离子束定位加工及结构表征

Structural characterization and focused ion beam in-situ processing of complex inclusions in steel materials

钢铁材料复合夹杂物的检测与表征,需要解决样品制备和微区相鉴定的难题。实验主要利用聚焦离子束精确定位功能,定位制备出复合夹杂物的透射电镜剖面样品,最大限度的呈现整个夹杂物的多种物相形态,再结合能谱仪的面分析功能和透射电镜的晶体结构分析技术对复合夹杂物进行全面的表征。通过对夹杂物的成分分析和物相衍射花样的标定,最终得到复合夹杂物的物相组成。结果表明,所分析复合夹杂物的形态和组成非常复杂,包括晶态的Mn2TiO4相、MgAl2O4相、Mn0.33Zr0.33Ti0.33O1.67相和非晶态的Ca-Al硅酸盐相。

The sample preparation and micro-zone phase identification were two challenges for the detection and characterization of complex inclusions of steel materials.The samples of complex inclusions for transmission electron microscope（TEM）profile characterization were in-situ prepared by the accurate positioning function of focused ion beam（FIB）.The morphologies of multi-phases in inclusions could be mostly presented.The surface analysis function of energy disperse spectroscopy（EDS）and the crystal structure analysis technique of TEM were also used for the comprehensive characterization of complex inclusions.The phase composition of complex inclusions was finally obtained by the component analysis of inclusions as well as the calibration of phase diffraction pattern.The results indicated that the morphology and composition of complex inclusions were very complicated,including the crystalline state Mn2TiO4 phase,MgAl2O4 phase,Mn0.33Zr0.33Ti0.33O1.67 phase and amorphous Ca-Al silicate phase.