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[求助]
鈣鈦礦合成
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看了一篇文獻(xiàn)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鈣鈦礦的反應(yīng)是在水溶液里進(jìn)行的，無比好奇這個(gè)到底是怎么合成出來的，鈣鈦礦不是見水就分解嗎？ 自己試了兩次，也都是呈現(xiàn)PbI2的的黃色溶液，沒有析出鈣鈦礦。 這個(gè)文獻(xiàn)引用率很高，一年160多次，工藝應(yīng)該不會(huì)有假的，但是為什么重復(fù)不出來呢？  不知道有沒有蟲子看過這個(gè)？歡迎大家討論一下~~~ 附合成工藝： 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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