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对球磨时间不同的Cu2Se、In2Se3和Ga2Se3混合粉末进行热压烧结制备CIGS靶材,发现在球磨时间较短时靶材出现分层,随着球磨时间延长分层缺陷消失。由此考察了粉末在球磨过程中发生的物理化学变化及其对分层的影响。结果表明:Cu2Se、In2Se3和Ga2Se3三种硒化物粉末在球磨过程中发生机械合金化反应形成黄铜矿相Cu(In,Ga)Se2(CIGS)。随着球磨时间的延长,黄铜矿相结构Cu In Se2(CIS)首先在Cu-Se二元化合物表面产生,并随着Ga原子的扩散逐步形成CIGS四元相。当球磨时间达到48 h时,粉末由黄铜矿相CIGS和少量Ga2Se3组成。由于Cu2-xSe与CIGS晶体结构相近,因此通过外延反应的方式有效促进了CIGS的合成。球磨过程中Cu-Se二元相的消失和CIGS相的形成有助于抑制烧结过程中分层缺陷的产生。
The CuZSe, In2Se3 and Ga2Se3 mixed powders with different ball milling time were prepared by hot pressing sintering. The results showed that when the milling time was short, the target layer delaminated, and the delamination defects disappeared with the milling time extended. In this way, the physical and chemical changes of the powders during ball milling and their effects on the delamination were investigated. The results show that the chalcopyrite phase Cu (In, Ga) Se2 (CIGS) is formed by the mechanical alloying reaction of Cu2Se, In2Se3 and Ga2Se3 powders. With the extension of ball milling time, the chalcopyrite phase Cu In Se2 (CIS) is firstly produced on the surface of Cu-Se binary compound and gradually forms the CIGS quaternary phase with the diffusion of Ga atoms. When ball milling time reaches 48 h, the powder consists of chalcopyrite phase CIGS and a small amount of Ga2Se3. Due to the similar crystal structure of Cu2-xSe and CIGS, the synthesis of CIGS is effectively promoted by the epitaxial reaction. The disappearance of Cu-Se binary phase and the formation of CIGS phase during ball milling help to restrain the delamination defects during sintering.