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采用石英管真空封装高纯度的Sb、Se粉末,在800℃下熔炼12 h,冷却后制成Sb2Se3粉末,在真空下进行热压烧结(470℃,60 MPa)并保温0.5 h,成功制备出Sb2Se3块体材料。运用XRD,SEM和EDS方法对材料的物相、成分和形貌进行了表征。结果表明,真空熔炼合成粉末和热压烧结块体材料的XRD图谱峰与Sb2Se3的标准衍射图谱(01-072-1184)相对应。Sb2Se3热压块体材料在平行于热压方向的断面上分布着大量的层片状结构,但少量片状结构变得粗大,层片状结构厚度约在1μm以下,并沿某一方向择优生长;垂直于热压方向的断面上微观形貌主要是层片状结构,并出现少量近似球形的结构,层片状结构短而薄,部分变得粗大,晶粒结构不均匀。热压烧结块体材料中Sb和Se的原子分数分别为40.68%,59.32%,接近2∶3。
High purity Sb and Se powders were vacuum-packed in quartz tube and smelted at 800 ℃ for 12 h. After cooling, Sb2Se3 powders were prepared and sintered under vacuum at 470 ℃ and 60 MPa for 0.5 h. Sb2Se3 bulk material. The phase, composition and morphology of the material were characterized by XRD, SEM and EDS. The results show that the XRD patterns of the vacuum melting powder and hot-pressed agglomerates correspond to the standard diffraction pattern of Sb2Se3 (01-072-1184). Sb2Se3 hot-pressed bulk material distributes a large number of lamellar structures in the section parallel to the hot pressing direction, but a small amount of lamellar structure becomes coarse, the thickness of the lamellar structure is less than 1μm and preferentially grows along a certain direction The micro-morphology on the cross-section perpendicular to the direction of hot pressing is mainly lamellar structure with a small amount of approximately spherical structure. The lamellar structure is short and thin, some become coarse, and the grain structure is not uniform. The atomic fraction of Sb and Se in the hot-pressed agglomerate was 40.68% and 59.32% respectively, close to 2: 3.