于 颖, 曹丙强

（济南大学材料科学与工程学院, 山东济南250022）

引用格式：于颖, 曹丙强. 无铅双钙钛矿纳米粉体Cs₂AgBiBr₆的球磨法制备工艺与性能[J]. 中国粉体技术, 2023, 29(6): 91-100.

YU Y, CAO B Q. Preparation process and property of lead-free double perovskite nano-powder Cs₂AgBiBr₆ by ball milling [J]. China Powder Science and Technology, 2023, 29(6): 91-100.

DOI：10.13732/j.issn.1008-5548.2023.06.009

收稿日期：2023-07-06,修回日期：2023-09-11,在线出版时间：2023-10-09 11:51。

基金项目：国家自然科学基金项目,编号:51872161;国家重点研发计划项目,编号:2022YFC3700801。

第一作者简介：于颖(1998—),女,硕士研究生,研究方向为无铅双钙钛Cs₂AgBiBr₆制备技术。E-mali: 614349800@qq.com。

通信作者简介：曹丙强(1978—),男,博士,教授,博士生导师,研究方向为新能源材料与器件。E-mali: mse_caobq@ujn.edu.cn。

摘要：以溴化铯、溴化银和溴化铋为原料,采用机械球磨工艺制备无铅双钙钛矿Cs₂AgBiBr₆纳米粉体;在一定的球磨转速、 研磨球与物料的质量比条件下,利用X射线衍射仪、 拉曼光谱仪、 激光粒度分析仪、 扫描电子显微镜、 紫外可见分光光度计、 稳态荧光光谱和热重分析仪等手段对制得的Cs₂AgBiBr₆纳米粉体进行测试和表征,研究球磨时间对纳米粉体Cs₂AgBiBr₆的纯度、 粒径和形貌的影响,并对Cs₂AgBiBr₆纳米粉体进行光学性质分析和热重分析。结果表明,随着球磨时间的增加,Cs₂AgBiBr₆纳米粉体最终达到纯相,粒径逐渐减小至约100 nm,颗粒形状由棒状变为圆形颗粒;在球磨转速为500 r/min、研磨球与物料的质量比为4.5∶1时,最佳球磨时间为12 h;Cs₂AgBiBr₆粉体禁带宽度为1.97 eV,发光峰位的波长为630 nm,属可见光发光波段;Cs₂AgBiBr₆粉体在温度为430 ℃时发生分解,在室温下可长久保存。

关键词：球磨工艺; 无铅双钙钛矿; 球磨时间; 纳米粉体; 光学性质

Abstract：Cesium bromide, silver bromide and bismuth bromide used as raw materials, a mechanical ball milling process using a planetary ball mill was employed to prepare lead-free double perovskite Cs₂AgBiBr₆ nano-powder. Under fixed ball milling speed and ball-to-material mass ratio, the nano powder was characterized using X-ray diffraction, Raman spectroscopy, laser particle size analyzer, scanning electron microscope, UV-visible spectrophotometer, steady-state fluorescence spectroscopy, and thermogravimetric analysis. To investigate the influence of ball milling time on the purity, particle size, and morphology of the Cs₂AgBiBr₆ nano-powder, the optical properties and thermogravimetric analysis of Cs₂AgBiBr₆ nano powder were also carried out. The results show that Cs₂AgBiBr₆ nano-powder finally reach pure phase, the particle size of Cs₂AgBiBr₆ nano-powder gradually decrease to about 100 nm, and the particle shape changes from rod to round with the increase of milling time. When the grinding speed is 500 r/min, the mass ratio of between grinding ball and raw material is 4.5∶1, the optimal grinding time is 12 h. The band gap of Cs₂AgBiBr₆ powder is 1.97 eV, and the wavelength of the luminescence peak is 630 nm, which belongs to the visible light band. Cs₂AgBiBr₆ powder is decomposed at 430 ℃ and can be stored for a long time at room temperature.

Keywords：ball milling process; lead-free double perovskite; milling time; nano-powder; optical property

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