ZnGeP_2多晶合成工艺改进及其X射线衍射分析  

Process improvement of polycrystalline synthesis and X-ray diffraction analysis on ZnGeP_2

作　　者：王志超[1] 朱世富[1] 赵北君[1] 陈宝军[1] 何知宇[1] 张建强[1] 杨登辉[1] 曹新玲[1] 

机构地区：[1]四川大学材料科学系,成都610064

出　　处：《四川大学学报（自然科学版）》2013年第4期829-833,共5页Journal of Sichuan University(Natural Science Edition)

基　　金：国家自然科学基金重点项目(50732005);高等学校博士学科点专项科研基金(20090181120001)

摘　　要：两温区气相输运合成ZnGeP2多晶,易发生化学计量比偏离,产生Ge、Zn3P2等杂相,在合成坩埚(石英安瓿)内壁凝聚一层ZnP2和P的沉积物.通过对合成设备、安瓿尺寸和工艺的改进,采用机械振荡炉体和竖直梯度降温相结合的新工艺,成功地合成出ZnGeP2多晶材料.合成的ZnGeP2多晶,经XRD分析测试,并采用Rietveld法进行全谱拟合精修、计算出各物相的相对含量.结果表明,改进工艺合成的ZnGeP2多晶是高纯单相材料,可用于单晶生长.采用改进工艺合成的ZnGeP2多晶为原料,生长出完整性好的ZnGeP2单晶体,在2.5～8.2μm范围的透过率达60%左右,光学质量较高.The stoichiometry of ZnGeP2 polycrystals synthesized by two-temperature vapor transport method deviates easily. The impurity phases of Ge and Zn3 P2 and condensed layer of ZnP2 and P precipi- tates often occur in the inner wall of the synthesis crucible （quartz ampoule）. We used a new synthesis process that combines the mechanically oscillated furnace and vertical gradient cooling technique, the modified synthesis equipment, and chooses appropriate size of the quartz ampoule. Based on this, we successfully synthesized the ZnGeP2 polycrystalline materials. The phase analysts was carried out using X-ray diffraction （XRD） on synthesized ZnGeP2 polycrystals. Whole pattern fitting refinement by Ri- etveld method was adopted, and then the relative contents of each phase were calculated by quantitative analysis. The results show that the synthesized ZnGeP2 using the improved process is of high-purity and single-phase, and that it can be used to grow ZnGeP2 crystals. We have grown the integral ZnGeP2 crys- tal using the synthesized ZnGeP2 polycrystals as raw material. Its infrared transimittance in the range of 2.5-8.2μm is close to 60%, suggesting that the optical quality of the grown crystal is good.

关 键 词：磷锗锌 多晶合成 工艺改进 竖直梯度降温 X射线衍射 

分 类 号：O722[理学—晶体学] O734