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 polycrystal material is a key problem in ZnGeP2 single crystal growth.The synthesis of ZnGeP2 polycrystal material is difficult due to the high vapor pressure of P and the volatilization of Zn and P.ZnGeP2 polycrystal material was synthesized by two-temperature synthesis technique.Some intermediate product was formed in the temperature gradient region in the furnace in the reaction process and a small amount of deposition product was formed on the quartz in the end side of the hot zone after all steps.Powder X-ray diffraction results show the intermediate product in the temperature gra-dient region is a mixture of 95.45%(volume fraction,the same below) ZnP2 and 4.55% Zn3P2.The deposition product on the quartz in the end side of the hot zone after all the steps is a mixture of 40% ZnP2 and 60% ZnGeP2.Some unreacted germanium was formed in the bottom of the ZnGeP2 polycrystal ingot due to the volatilization of Zn and P.High quality,stoichiometric ZnGeP2 polycrystal ma-terial can be prepared by the adjustment of temperature of hot zone and temperature reducing rate,and the control of volatilization of Zn and P.