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<p>This investigation presents the solvothermal synthesis of black phosphorus (BP) nanosheets derived from a slurry of red phosphorus and ethylenediamine, conducted under standard laboratory conditions. The synthesised BP nanosheets underwent comprehensive characterisation using techniques such as X-ray diffraction (XRD), Raman spectroscopy, transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), ultraviolet–visible (UV–Vis) spectroscopy, and cyclic voltammetry (CV). XRD analysis confirms the orthorhombic crystal structure of BP, with lattice parameters of a = 3.311&#xa0;Å, b = 10.421&#xa0;Å, and c = 4.373&#xa0;Å. The Scherrer equation estimates the average crystallite size to be 13.6&#xa0;nm. Raman spectroscopy further verifies the structural integrity of BP, highlighting characteristic vibrational peaks corresponding to the A<sup>1</sup><sub>g</sub>, B<sub>2 g</sub>, and A<sup>2</sup><sub>g</sub> modes, confirming the preservation of its layered structure. TEM imaging reveals well-exfoliated nanosheets with distinct lattice fringes and interlayer spacings of 0.33&#xa0;nm and 0.26&#xa0;nm, corresponding to the (021) and (040) crystal planes, respectively. Electrochemical characterisation through CV and EIS measurements of the BP working electrode in an electrolytic solution of Na₂SO₄ using a three-electrode system demonstrates electric double-layer capacitance behaviour with well-defined, nearly rectangular voltammograms with high current response, suggesting efficient charge storage and rapid ion diffusion at the electrode–electrolyte interface. Furthermore, FESEM-EDX confirms the nanosheet morphology and expected elemental composition, while UV–Vis spectroscopy reveals a semiconducting optical bandgap of 1.40&#xa0;eV, supporting its applicability in optoelectronics.</p>

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Black phosphorus nanosheets synthesised by solvothermal method: structural integrity, optical properties, and EDLC behaviour

  • 期刊论文

  • 发表日期：

    2025年6月18日

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  • Shahbaz Ahmad,
  • Roomul Mushtaq,
  • Towseef Ahmad,
  • Mohd Zubair Ansari

摘要

This investigation presents the solvothermal synthesis of black phosphorus (BP) nanosheets derived from a slurry of red phosphorus and ethylenediamine, conducted under standard laboratory conditions. The synthesised BP nanosheets underwent comprehensive characterisation using techniques such as X-ray diffraction (XRD), Raman spectroscopy, transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), ultraviolet–visible (UV–Vis) spectroscopy, and cyclic voltammetry (CV). XRD analysis confirms the orthorhombic crystal structure of BP, with lattice parameters of a = 3.311 Å, b = 10.421 Å, and c = 4.373 Å. The Scherrer equation estimates the average crystallite size to be 13.6 nm. Raman spectroscopy further verifies the structural integrity of BP, highlighting characteristic vibrational peaks corresponding to the A1g, B2 g, and A2g modes, confirming the preservation of its layered structure. TEM imaging reveals well-exfoliated nanosheets with distinct lattice fringes and interlayer spacings of 0.33 nm and 0.26 nm, corresponding to the (021) and (040) crystal planes, respectively. Electrochemical characterisation through CV and EIS measurements of the BP working electrode in an electrolytic solution of Na₂SO₄ using a three-electrode system demonstrates electric double-layer capacitance behaviour with well-defined, nearly rectangular voltammograms with high current response, suggesting efficient charge storage and rapid ion diffusion at the electrode–electrolyte interface. Furthermore, FESEM-EDX confirms the nanosheet morphology and expected elemental composition, while UV–Vis spectroscopy reveals a semiconducting optical bandgap of 1.40 eV, supporting its applicability in optoelectronics.