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[求助]
钙钛矿合成
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看了一篇文献Semiconducting Tin and Lead Iodide Perovskites with Organic Cations：Phase Transitions, High Mobilities, and Near-Infrared Photoluminescent Properties，里面提到合成CH3NH3PbI3钙钛矿的反应是在水溶液里进行的，无比好奇这个到底是怎么合成出来的，钙钛矿不是见水就分解吗？ 自己试了两次，也都是呈现PbI2的的黄色溶液，没有析出钙钛矿。 这个文献引用率很高，一年160多次，工艺应该不会有假的，但是为什么重复不出来呢？  不知道有没有虫子看过这个？欢迎大家讨论一下~~~ 附合成工艺： 1. A 100 ml 2-necked round bottom flask was charged with a mixture of aqueous HI (6.8 ml, 7.58M) and aqueous H3PO2 (1.7 ml, 9.14M). The liquid was degassed by passing a stream of nitrogen through it for 1 min and keeping it under a nitrogen atmosphere throughout the experiment. 2. PbI2 (462 mg, 1 mmol) was dissolved in the mixture upon heating the flask to 120oC using an oil bath, under constant magnetic stirring, forming a bright yellow solution. 3. To the hot yellow solution was added solid CH3NH3I (159 mg, 1 mmol) dissolving immediately. 4. The solution was evaporated to approximately half its original volume by heating at 120oC. The stirring was discontinued and the solution was left to cool back to room temperature. 5. Upon cooling, black, rhombic dodecahedral crystals (12 faces) of the title compound precipitated. 6. The crystals were left to grow inside the mother liquor for a further 24 h under a nitrogen atmosphere before being filtered and washed copiously with anhydrous EtOH. Yield 70-90%. |
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