不同硫化温度下铜锌锡硫薄膜的微观组织结构表征  

Microstructure Characterization of Cu2ZnSnS4 Thin Films Fabricated by Sulfurization at Different Temperatures

作　　者：赵新奇[1] 范亮亮 韩俊峰[2] 明文全[1] 杨修波 李石勇 洪悦[1] 茶丽梅[1,4] ZHAO Xinqi;FAN Liangliang;HAN Junfeng;MING Wenquan;YANG Xiubo;LI Shiyong;HONG Yue;CHA Limei(College of Materials Science and Engineering,Hunan University,Changsha 410082,China;School of Physics,Beijing Institute of Technology,Beijing 100081,China;Analytical&Testing Center,Northwestern Polytechnical University,Xi′an 710072,China;Guangdong Technion Israel Institute of Technology,Shantou 515063,China)

机构地区：[1]湖南大学材料科学与工程学院,湖南长沙410082 [2]北京理工大学物理学院,北京100081 [3]西北工业大学分析测试中心,陕西西安710072 [4]广东以色列理工学院,广东汕头515063

出　　处：《湖南大学学报（自然科学版）》2019年第12期85-89,共5页Journal of Hunan University:Natural Sciences

基　　金：国家自然科学基金资助项目(51402103)~~

摘　　要：在覆盖Mo层的钠钙玻璃上采用磁控溅射沉积后续硫化处理方式制备铜锌锡硫(CZTS)薄膜.利用X射线衍射仪、扫描电子显微镜、透射电子显微镜、高角环形暗场像和X射线能谱仪等表征技术,研究不同硫化温度下CZTS薄膜形成过程中微观组织结构的变化.结果表明:硫化温度升高到400℃以上形成CZTS四元结晶相组成的薄膜,在400~550℃之间,随硫化温度的升高CZTS相增多且尺寸增大,600℃硫化时,CZTS相出现分解现象.硫化温度对薄膜影响显著,近钼层颗粒尺寸较小,表层颗粒尺寸较大.温度较低时薄膜的表层中Cu和S富集形成CuS,近钼层中Zn和Sn含量较多.随着温度升高,Cu、Zn、Sn和S不断扩散,分布更加均匀,形成的CZTS相结晶性愈好,晶粒不断长大成等轴晶,且CZTS晶粒出现孪晶.Cu2ZnSnS4(CZTS)thin films were deposited on Mo-coated soda lime glass substrates by magnetron sputtering and sulfurization treatment.The microstructure of thin films sulfurized at different temperatures was studied using different microstructural charaterizations such as X-ray diffraction(XRD),scanning electron microscopy(SEM),transmission electron microscopy(TEM),high angle annular dark field(HAADF)imaging and X-ray energy dispersive spectrum(EDS)analysis.The results showed that crystallization of CZTS films synthesized at above 400℃was enhanced with the increase of annealing temperature from 400~550℃,but decomposition reaction of CZTS films occurred at 600℃.Films morphology was influenced by the temperatures greatly,the size of grains close to the surface of the thin films was large and the size of grains close to the Mo substrate was small.The CuS phase was observed on the surface of the thin films based on the rich of Cu and S,while the contents of Zn and Sn were richclose to the Mo substrate at relatively low temperatures.With the increase of temperatures,crystallization of CZTS films was enhanced with Cu,Zn,Sn and S gradual diffusion,and the grains of CZTS grew up as equiaxial crystals.Twins were formed in grains of CZTS.

关 键 词：Cu2ZnSnS4薄膜 硫化 微观组织结构 电子显微镜 孪晶 

分 类 号：TM914.4[电气工程—电力电子与电力传动] O484.1[理学—固体物理]