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A Stage-by-Stage Phase-induction and Nucleation of Black Phosphorus from Red Phosphorus Under Low-pressure Mineralization

Abstract

In the preparation of black Phosphorene (BP) by means of low-pressure mineralization, the complex temperature program makes its synthesis mechanism complicated and confusing. Herein, orthorhombic BP crystal was successfully synthesized by way of low-pressure mineralization and the phase transition at every stage was revealed systematically, which was accurately confirmed via a series of interference experiments and supported by structure characterization. Besides, the nucleation agents and nucleation sites were of systematic demonstration. Based on this, we found that the synthesis of BP is a process of stage-by-stage phase-induction. At first, red phosphorus (RP) is transformed to Hittorf's phosphorus (HP) without the assistance of mineralizers. Subsequently, HP is transformed into BP at the cooling stage. Moreover, Sn24P19.3I8 should work as the sole nucleation agent, which leads to BP crystal nucleating and growing large in the heat preservation stage subsequently. And the nucleation site lies in the product region opposite to the source region. In addition, the radial morphology of BP crystal bunches under RP/SnI4/Sn (granule) system were revealed firstly, the straps taken out from the BP bunches is convenient for exfoliating.

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Publication details

The article was received on 16 Aug 2017, accepted on 09 Nov 2017 and first published on 09 Nov 2017


Article type: Paper
DOI: 10.1039/C7CE01492A
Citation: CrystEngComm, 2017, Accepted Manuscript
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    A Stage-by-Stage Phase-induction and Nucleation of Black Phosphorus from Red Phosphorus Under Low-pressure Mineralization

    Z. Chen, Y. Zhu, J. Lei, W. Liu, Y. Xu and P. Feng, CrystEngComm, 2017, Accepted Manuscript , DOI: 10.1039/C7CE01492A

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