碘化铟(InI)多晶的水平区熔提纯

doi:10.15541/jim20150121

无机材料学报 ›› 2015, Vol. 30 ›› Issue (10): 1063-1068.DOI: 10.15541/jim20150121 CSTR: 32189.14.10.15541/jim20150121

碘化铟(InI)多晶的水平区熔提纯

徐朝鹏, 张磊, 王倩, 纪亮亮, 李亚可

(燕山大学信息科学与工程学院, 河北省特种光纤与光纤传感重点实验室, 秦皇岛 066004)

收稿日期:2015-03-11 修回日期:2015-05-21 出版日期:2015-10-20 网络出版日期:2015-09-30
基金资助:
河北省应用基础研究计划重点基础研究项目(13961103D);中国电子科技集团公司第四十六研究所创新基金(CJ20120208);河北省高层次人才资助项目(C2013003040);燕山大学青年教师自主研究计划(13LGA011)

Horizontal Zone Refining of Indium Iodide (InI) Polycrystal

XU Zhao-Peng, ZHANG Lei, WANG Qian, JI Liang-Liang, LI Ya-Ke

(School of Information Science and Engineering, The Key Laboratory for Special Fiber and Fiber Sensor of Hebei Province, Yanshan University, Qinhuangdao 066004, China)

Received:2015-03-11 Revised:2015-05-21 Published:2015-10-20 Online:2015-09-30
Supported by:
Key Basic Research Program of Applied Basic Research Project of Hebei (13961103D);Innovation Fund of China Electronic Technology Group Corporation NO.46 Research Institute (CJ20120208);High Level Talent Funded Project of Hebei (C2013003040);Young Teachers Independent Research Project of Yanshan University (13LGA011)

摘要/Abstract

摘要：

采用水平区熔法对由两温区气相输运法制备的InI多晶进行提纯, 探索高纯、单相InI多晶的制备工艺。通过X射线粉末衍射仪、扫描电子显微镜以及电感耦合等离子体原子发射光谱仪对水平区熔提纯前后的InI多晶的晶格结构、形貌组分以及杂质浓度进行了表征。结果表明, 经过水平区熔提纯后的InI多晶晶格结构完整, 质量较高, 晶格参数为a=0.476 nm, b=1.278 nm, c=0.491 nm, 与理论值十分接近; In、I化学配比得到了有效调节, 其化学配比接近理论化学配比1: 1; 中间产物含量及杂质浓度显著降低。以提纯后InI多晶为原料, 用提拉法生长出的InI单晶电阻率达到10¹⁰ Ω·cm。

关键词: 碘化铟, 多晶合成, 气相输运, 区域熔融, 提纯

Abstract:

The indium iodide (InI) polycrystal which was synthesized by two-zone vapor transporting method was purified by using horizontal zone refining method. Preparation process on high quality and single phase InI polycrystal was successfully fixed. The lattice structure, morphology, component and impuritily concentration of InI crystal were investigated by X-Ray Diffraction (XRD), Scanning Electron Microscope-Energy Dispersive Spectrometer (SEM-EDS) and Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). The results indicate that the InI polycrystal after refinement has better lattice structure and higher quality than before. The lattice constants of a, b and c are 0.476 nm, 1.278 nm and 0.491 nm, respectively, which are very close to the theoretical values. The stoichiometric ratio of In to I is effectively modified and close to the theoretical stoichiometric ratio 1:1. The intermediate products and impurities concentrations decrease significantly. An InI single crystal with high resistivity (about 10¹⁰ Ω·cm) is grown by Czochralski (CZ) method with the purified InI polycrystal obtained in this work.

Key words: indium iodide, polycrystalline synthesis, vapor transporting, zone refining, purification

中图分类号:

徐朝鹏, 张磊, 王倩, 纪亮亮, 李亚可. 碘化铟(InI)多晶的水平区熔提纯[J]. 无机材料学报, 2015, 30(10): 1063-1068.

XU Zhao-Peng, ZHANG Lei, WANG Qian, JI Liang-Liang, LI Ya-Ke. Horizontal Zone Refining of Indium Iodide (InI) Polycrystal[J]. Journal of Inorganic Materials, 2015, 30(10): 1063-1068.

图/表 12

图1 InI多晶合成炉和温场曲线示意图

Fig. 1 Schematic diagram of synthesis furnace and temperature curve for InI polycrystal

图2 In-I化合物相图[4]

Fig. 2 Indium-Iodine compound phase diagram[4]

图3 InI多晶合成升温曲线图

Fig. 3 Temperature curve for InI polycrystal

图4 合成的InI多晶

Fig. 4 Synthesized InI polycrystal

表1 单质碘和单质铟所含的部分杂质及其分凝系数

Table 1 Segregation coefficient of elements in iodine and indium

Element	Mg	Ni	Ca	Cr	Fe
K₀	0.013	0.163	0.071	0.018	0.028

图5 区熔提纯过程(a)及提纯炉(b)示意图

Fig. 5 Schematic diagram of zone refining process (a) and zone refining furnace (b)

图6 提纯前后InI多晶样品的XRD图谱

Fig. 6 XRD patterns of InI polycrystalline sample before (a) and after (b) refinement

图7 提纯前(a)后(b)InI多晶的 SEM照片

Fig. 7 SEM images of InI polycrystal before (a) and after (b) refinement

表2 提纯前后InI多晶样品的EDS分析结果

Table 2 EDS analysis results of InI polycrystalline samples before and after refinement

Sample	In/at%	I/at%	Total/at%
Before refinement	47.13	52.87	100
After refinement	50.69	49.31	100

表3 提纯前后InI多晶样品的各元素浓度

Table 3 Concentrations of elements in InI polycrystalline before and after refinement

Elements	In/at%	I/at%	Li/ (μg·mL^-1)	Cr/ (μg·mL^-1)	Cu/ (μg·mL^-1)	Mg/ (μg·mL^-1)	Al/ (μg·mL^-1)	Zn/ (μg·mL^-1)	Fe/ (μg·mL^-1)	Ni/ (μg·mL^-1)
Before refinement	47.58	52.41	0.0504	0.0469	0.0790	0.1287	0.1256	0.2885	0.6436	0.8187
After refinement	50.74	49.25	--	--	0.0093	0.0107	0.0311	0.0291	0.0565	0.0740

图8 提拉法生长的InI单晶

Fig. 8 InI crystal grown by CZ method

图9 InI单晶的I-V曲线

Fig. 9 Current-voltage curve of InI crystal

参考文献 14

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碘化铟(InI)多晶的水平区熔提纯

Horizontal Zone Refining of Indium Iodide (InI) Polycrystal

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