通过溶解度研究优化的过饱和有机溶液中CsPbBr钙钛矿的单晶化
Single Crystallization of CsPbBr Perovskite from Supersaturated Organic Solutions Optimized Through Solubility Studies.
作者信息
Watanabe Satoshi, Hayashida Taiki, Iwai Masaru, Inomata Yusuke, Kunitake Masashi, Kida Tetsuya
机构信息
Faculty of Advanced Science and Technology, Kumamoto University, 2-39-1 Kurokami, Chuo-ku, Kumamoto City, Kumamoto 860-8555, Japan.
Institute of Industrial Nanomaterials, Kumamoto University, 2-39-1 Kurokami, Chuo-ku, Kumamoto City, Kumamoto 860-8555, Japan.
出版信息
ACS Omega. 2023 Jan 6;8(2):2455-2461. doi: 10.1021/acsomega.2c06945. eCollection 2023 Jan 17.
We demonstrate the fabrication of millimeter-sized single crystals of 0D-CsPbBr grown in a supersaturated solution consisting of organic solvents without HBr (aq). One of the precursors, CsBr, was dissolved in ethylene glycol (EG) mixed with dimethyl sulfoxide, which is a good solvent for the other precursor, PbBr. At a solvent ratio of 20 vol % EG, the solubility of cesium bromide decreased and the title compound, CsPbBr, was selectively formed, whereas, with an EG ratio of 80 vol %, 3D-CsPbBr was formed. A phase diagram (solubility curve) of CsPbBr in the mixed solvent containing 20 vol % EG was obtained by visually observing dissolution and crystal precipitation while changing the temperature. Because the solubility was proportional to the temperature, the solubility curve demonstrated an upper critical solution phenomenon. The solubility near the boiling point of the solution (150 °C) was approximately 0.14 M. A single crystal of CsPbBr was formed by growing a seed crystal in a supersaturated solution on the low-temperature side of the solubility curve. X-ray analysis established the crystal structure; a fluorescence emission at 520 nm with a full width at half maximum of 20 nm confirms the composition of the single crystal to be CsPbBr.
我们展示了在不含氢溴酸水溶液的有机溶剂组成的过饱和溶液中生长的毫米级零维 CsPbBr 单晶的制备过程。其中一种前驱体 CsBr 溶解于与二甲亚砜混合的乙二醇（EG）中，二甲亚砜是另一种前驱体 PbBr 的良溶剂。在乙二醇体积比为 20%的溶剂比例下，溴化铯的溶解度降低，选择性地形成了目标化合物 CsPbBr，而当乙二醇比例为 80%时，则形成了三维 CsPbBr。通过在改变温度的同时目视观察溶解和晶体沉淀，获得了 CsPbBr 在含 20%体积乙二醇的混合溶剂中的相图（溶解度曲线）。由于溶解度与温度成正比，溶解度曲线呈现出上临界溶液现象。溶液沸点（150°C）附近的溶解度约为 0.14 M。通过在溶解度曲线低温侧的过饱和溶液中生长籽晶形成了 CsPbBr 单晶。X 射线分析确定了晶体结构；在 520 nm 处的荧光发射，半高宽为 20 nm，证实了单晶的组成为 CsPbBr。
Zotero 插件