Volume 5, Issue 11 p. 3266-3271
Full Paper

Scalable Synthesis of Micron Size Crystals of CH3NH3PbI3 at Room Temperature in Acetonitrile via Rapid Reactive Crystallization

Dr. Taame A. Berhe

Dr. Taame A. Berhe

NanoElectrochemistry Laboratory, Graduate Institute of Applied Science and Technology, National Taiwan University of Science and Technology, Taipei, 106 Taiwan

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Prof. Wei-Nien Su

Corresponding Author

Prof. Wei-Nien Su

NanoElectrochemistry Laboratory, Graduate Institute of Applied Science and Technology, National Taiwan University of Science and Technology, Taipei, 106 Taiwan

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Dr. Ju-Hsiang Cheng

Dr. Ju-Hsiang Cheng

NanoElectrochemistry Laboratory, Department of Chemical Engineering, National Taiwan University of Science and Technology, Taipei, 106 Taiwan

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Prof. Ming-Hsien Lin

Prof. Ming-Hsien Lin

NanoElectrochemistry Laboratory, Department of Chemical Engineering, National Taiwan University of Science and Technology, Taipei, 106 Taiwan

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Dr. Kassa B. Ibrahim

Dr. Kassa B. Ibrahim

NanoElectrochemistry Laboratory, Graduate Institute of Applied Science and Technology, National Taiwan University of Science and Technology, Taipei, 106 Taiwan

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Dr. Amaha W. Kahsay

Dr. Amaha W. Kahsay

NanoElectrochemistry Laboratory, Department of Chemical Engineering, National Taiwan University of Science and Technology, Taipei, 106 Taiwan

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Chia Lin Li

Chia Lin Li

Department of Material Science and Engineering, National Taiwan University of Science and Technology, Taipei 106, Taiwan

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Dr. Alok M. Tripathi

Dr. Alok M. Tripathi

NanoElectrochemistry Laboratory, Department of Chemical Engineering, National Taiwan University of Science and Technology, Taipei, 106 Taiwan

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Dr. Mau-Tsu Tang

Dr. Mau-Tsu Tang

National Synchrotron Radiation Research Center, Hsin-Chu, 30076 Taiwan

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Prof. Bing-Joe Hwang

Corresponding Author

Prof. Bing-Joe Hwang

NanoElectrochemistry Laboratory, Department of Chemical Engineering, National Taiwan University of Science and Technology, Taipei, 106 Taiwan

National Synchrotron Radiation Research Center, Hsin-Chu, 30076 Taiwan

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First published: 17 March 2020
Citations: 1

Graphical Abstract

The synthesis of highly crystalline CH3NH3PbI3 pure chemical substance is feasible by reactive crystallization of PbI2 and CH3NH3I in acetonitrile at room temperature. The nucleation and growth steps involve Ostwald ripened iodide ions moving into PbI2 to form PbI3-octahedrons. It is then followed by the intercalation of CH3NH3+, as the key step for this reactive crystallization. This reactive crystallization method is expected to be suitable for mass production of larger crystals of perovskites

Abstract

From application point of view, scalable, facile and rapid synthesis method for mass production of a homogeneous and phase pure CH3NH3PbI3 micron size crystal at the industry level is still highly required, although it has been claimed that the CH3NH3PbI3 crystals can be prepared by solution-annealing the precursors at elevated temperature or prolonged reaction time. Herein, polycrystalline CH3NH3PbI3 micron size crystals can be prepared by reactive crystallization of PbI2 and CH3NH3I in a stoichiometric ratio at room temperature. TXM (Transmission X-ray Microscopy), optical microscope, TEM and TEM-EDX analysis were used to confirm the nature of the CH3NH3PbI3 product. Moreover, Ostwald ripening of iodide ion into PbI2 is proposed as the key step to form 3D PbI3, followed by the intercalation of CH3NH3+ for this reactive crystallization. Interestingly, this result suggests that industry level mass production of micron CH3NH3PbI3 crystals is possible with this novel synthesis method.

Conflict of interest

The authors declare no conflict of interest.