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合成高纯及化学计量比的ZnGeP2多晶材料是生长高质量ZnGeP2单晶的关键。但由于P在高温下蒸气压高,Zn和P易挥发等因素,使合成化学计量比ZnGeP2多晶材料存在一定困难。采用双温区合成法制备了ZnGeP2多晶材料,用X射线粉末衍射分析了反应过程中在炉内温度梯度区间生成的中间产物和在高温区末端石英管壁上的少量沉淀。结果表明:温度梯度区间生成的中间产物中ZnP2含量为95.45%(体积分数,下同),Zn3P2含量为4.55%。高温区末端石英管壁上的沉淀中ZnP2含量为40%,ZnGeP2含量为60%,Zn和P的挥发导致合成的ZnGeP2多晶体中富含Ge。通过调节高温区的温度和降温速率,可有效地控制组分挥发,得到化学计量比的ZnGeP2多晶材料。
Synthesis of high purity and stoichiometric ZnGeP2 polycrystalline material is the key to the growth of high quality ZnGeP2 single crystal. However, due to P high vapor pressure at high temperatures, volatile Zn and P and other factors, the synthesis of stoichiometric ZnGeP2 polycrystalline material there are some difficulties. The ZnGeP2 polycrystalline material was prepared by the dual temperature zone synthesis method. The intermediate products formed during the reaction in the temperature gradient zone and the small amount of precipitate on the quartz tube wall at the end of the high temperature zone were analyzed by X-ray powder diffraction. The results show that the content of ZnP2 in the intermediate product produced by temperature gradient is 95.45% (volume fraction), and the content of Zn3P2 is 4.55%. ZnP2 content is 40% and ZnGeP2 content is 60% in the precipitation of the quartz tube wall at the end of the high temperature region. The volatilization of Zn and P results in the enrichment of Ge in the synthesized ZnGeP2 polycrystal. By adjusting the temperature in the high temperature zone and cooling rate, the components can be effectively volatilized to obtain the stoichiometric ZnGeP2 polycrystalline material.