Issue 44, 2015

Novel synthesis of dispersed molybdenum and nickel phosphides from thermal carbonization of metal- and phosphorus-containing resins

Abstract

Dispersed pure phases of MoP and Ni2P nanoparticles supported by carbon were synthesized by carbonization of metal- and phosphorus-containing resins under an inert atmosphere. The solid products and the evolution of gases during the carbonization process were investigated by various techniques, including X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), inductively coupled plasma-atomic emission spectroscopy (ICP-AES), N2 adsorption–desorption analysis, and mass spectrometry (MS). The resins underwent two carbonization stages: the low-temperature carbonization stage (<650 °C) and the high-temperature carbonization stage (≥650 °C). There was an initial reduction of Mo and Ni precursors in the low-temperature region. However, the formation of phosphides was observed in the high-temperature carbonization stage, in which Mo(Ni) and POx species were further reacted with the carbonization products (C, H2 and CH4) to yield Mo(Ni) phosphide. Note that compared with the traditional H2-temperature-programmed reduction (H2-TPR) method, this novel synthesis route produced a large amount of COx besides H2O, leading to a lower water vapor pressure. In addition, the residual carbon produced from resin can play a role in bonding of nanoparticle aggregation. Therefore, the better dispersions and higher surface areas of the as-prepared phosphide nanoparticles were attributed to the mitigation of hydrothermal sintering and the intimate contact between phosphide nanoparticles and carbon species.

Graphical abstract: Novel synthesis of dispersed molybdenum and nickel phosphides from thermal carbonization of metal- and phosphorus-containing resins

Supplementary files

Article information

Article type
Paper
Submitted
30 Jun 2015
Accepted
12 Oct 2015
First published
13 Oct 2015

Dalton Trans., 2015,44, 19383-19391

Novel synthesis of dispersed molybdenum and nickel phosphides from thermal carbonization of metal- and phosphorus-containing resins

Z. Yao, J. Tong, X. Qiao, J. Jiang, Y. Zhao, D. Liu, Y. Zhang and H. Wang, Dalton Trans., 2015, 44, 19383 DOI: 10.1039/C5DT02464A

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