高纯锗单晶的制备与位错密度分析

深圳大学物理与光电工程学院,广东深圳518060

半导体材料;晶体;高纯锗制备;高纯锗探测器;单晶生长;位错密度;直拉法

Preparation of high purity germanium single crystal and analysis of dislocation density
HAO Xin,GAN Lin,HU Shipeng,LUO Qi,WU Zhengxin,ZHONG Jian,ZHAO Haige,and SUN Huibin

College of Physics and Optoelectronic Engineering, ShenzhenUniversity, Shenzhen 518060, Guangdong Province, P. R. China

semiconductor material; crystal; high purity germanium preparation; high purity germanium detector;single crystal growth; dislocation density; Czochralski method

DOI: 10.3724/SP.J.1249.2022.05504

备注

高纯锗探测器在辐射探测领域具有重要地位.经过区熔提纯和单晶生长2个阶段,成功制备了纯度为13N、位错密度介于100~10000cm-2之间的高纯锗.其中,区熔实验使用自制水平区熔炉,在高纯氢气环境下,通过20~50次区熔以达到提纯要求.单晶生长采用直拉法,在高纯氢气环境下,沿[100]晶向生长,单晶有效长度>50mm,有效直径>30mm.采用浸蚀法测量位错密度,利用酸性腐蚀液腐蚀锗单晶片(100)晶面,读取位错腐蚀坑数量.结果显示,距单晶棒头部25、50和72mm处的位错密度分别为2537、3425和4075cm-2,表明在晶锭头部72mm前,位错密度满足高纯锗探测器制备的要求.研究可为高纯锗单晶的制备提供参考.
High purity germanium detector plays an important role in the field of radiation detection. High purity germanium with 13N purity and dislocation density between 100~ 10 000 cm-2 was successfully prepared through zone melting purification and single crystal growth. In the zone melting experiment, the self-made horizontal zone furnace is used to achieve the purification requirements through 20~50 times of zone melting in the environment of high-purity hydrogen. The single crystal is grown by Czochralski method along the [100] direction in high-purity hydrogen environment with effective length > 50 mm and effective diameter > 30 mm. The dislocation density measurement adopts the etching method. The acid etching solution is used to etch the crystal (100) surface and the number of the etch pits is counted. The results show that the dislocation densities at 25, 50 and 72 mm from the head of the single crystal are 2 537, 3 425 and 4 075 cm-2 respectively. These results indicate that the dislocation density before 72 mm meets the requirements for the preparation of high-purity germanium detectors. The research can provide reference for the preparation of high purity germanium single crystal.
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