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采用石英管真空封装高纯度的Sb和Te粉末,在800℃熔炼12h,炉冷后研磨制备Sb2Te3粉末,真空热压烧结(480℃,20MPa,保温1h),制备出Sb2Te3块体材料。用XRD、SEM和EDS对材料的物相、形貌和成分进行表征。XRD分析表明,真空熔炼合成粉末和热压烧结块体材料的XRD图谱峰与Sb2Te3的标准衍射图谱相对应。Sb2Te3热压块体材料在平行于热压方向的断面上分布有大量层片状结构,层片厚度均小于1μm,在层片状结构之间均匀分布着短的片状结构。与热压方向垂直的断面上也是层片状结构,层片状较短且分布较均匀,层片厚度大多在1μm左右。材料中Sb和Te的原子百分数分别为38.2%、61.8%,接近2∶3的原子百分比。
The Sb2Te3 bulk material was prepared by vacuum packaging of Sb and Te powders with high purity in quartz tube, smelting at 800 ℃ for 12h, furnace cooling and then grinding to prepare Sb2Te3 powder and vacuum hot pressing sintering (480 ℃, 20MPa, 1h). The phase, morphology and composition of the material were characterized by XRD, SEM and EDS. XRD analysis showed that the XRD patterns of vacuum melting powder and hot-pressed agglomerates corresponded to the standard diffraction patterns of Sb2Te3. The Sb2Te3 hot-pressed bulk material has a large number of lamellar structures distributed in the section parallel to the hot pressing direction. The lamellar thickness is less than 1μm, and the short lamellar structure is uniformly distributed between the lamellar structures. The cross section perpendicular to the direction of hot pressing is also a lamellar structure, the lamellar shape is short and the distribution is relatively uniform, and the lamellar thickness is mostly about 1 μm. The atomic percentages of Sb and Te in the material were 38.2% and 61.8% respectively, close to the atomic percentage of 2: 3.