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采用石英管真空封装高纯度的Sb粉和Se粉,在800℃下熔炼8h,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,制备出Sb2Se3块体材料。运用XRD、SEM和EDS法对材料物相、形貌和成分进行了表征。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和垂直于热压方向的断面上都分布着大量的层片状结构,平行于热压方向的断面上层片状结构沿某一方向择优生长,而在垂直于热压方向的断面上层片状结构分布更均匀,结晶更充分;材料中Sb和Se的原子百分比分别为40.68%、59.32%,接近于2∶3。
Sb powder and Se powder were vacuum packed in quartz tube and smelted at 800 ℃ for 8h. After cooling, Sb2Se3 powder was prepared and sintered under vacuum at 470 ℃ and 60 MPa for 0.5 h to prepare Sb2Se3 Block material. The phase, morphology and composition of the material were characterized by XRD, SEM and EDS. The results show that the XRD patterns of vacuum smelting powder and hot-pressed agglomerate correspond to the standard diffraction pattern (01-072-1184) of Sb2Se3. The hot-pressed bulk material of Sb2Se3 is in parallel and perpendicular to the direction of hot pressing A large number of lamellar structures are distributed. The upper lamellar structure parallel to the direction of hot pressing preferentially grows in one direction, while the upper lamellar structure distributes more evenly in the section perpendicular to the hot pressing direction, and the crystal is more fully. The material The atomic percentages of Sb and Se are 40.68% and 59.32%, respectively, which are close to 2: 3.