A Novel Route to the Preparation of Carbon Supported Nickel Phosphide Catalysts by a Microwave Heating Process

Abstract

A simple and efficient approach based on microwave heating process was developed to prepare carbon supported nickel phosphide. In this approach, red phosphorus was used as a P source and carbon acted as both the support and the microwave absorbent. The red phosphorus was homogeneously mixed with Ni-impregnated carbon by milling, and then subjected to microwave heating. After several minutes by microwave heating in Ar or H 2 atmosphere, the nickel phosphide, Ni 2 P, was produced on the carbon support, while the temperature of the sample bed was only 473 K or even lower during the reaction. It was also found that the preparation atmosphere had significant effects on the phosphide formation. Compared to the preparation in Ar, the nickel phosphides prepared in H 2 were more readily formed and more highly dispersed on the carbon support due to PH 3 formation during the reduction process. The as-prepared nickel phosphide catalysts exhibited much higher activities in selective hydrogenation of 1,3-butadiene compared to that prepared by the conventional heating method, which was attributed to the high dispersion of Ni 2 P prepared by the microwave heating method.

Rapid, High‐Temperature, In Situ Microwave Synthesis of Bulk Nanocatalysts

“…c) Comparison of the peak temperatures among various masses of carbon black (20, 200, and 800 mg) during microwave irradiation. d) Comparison of the heating times and temperatures demonstrated in this work with previous carbon‐black‐based microwave syntheses …”

“…d) Comparison of the heating times and temperatures demonstrated in this work with previous carbon-black-based microwave syntheses. [18][19][20][21][22][23][24][25][26][27] synthesis. Figure 2e compares the heating and cooling rates of the proposed microwave heating method to those of a conventional tube furnace heating.…”

“…Recently, microwave‐assisted synthesis has been extensively studied in carbon‐based composites . By using liquid‐phase microwave heating strategy, carbon‐supported metal, alloy and metal chalcogenide nanoparticles have been successfully fabricated, resulting in homogeneous and well‐defined nanoparticle catalysts that demonstrated enhanced performance for fuel cell applications. However, these liquid‐phase synthetic processes suffer many of the same pitfalls as that of conventional wet chemistry methods.…”

“…Therefore, a facile and scalable synthetic strategy for preparing CNPs with small size and uniform distribution is desired for their future development and application as high-performance electrocatalysts.Recently, microwave-assisted synthesis has been extensively studied in carbon-based composites. [14][15][16][17] By using liquid-phase microwave heating strategy, carbon-supported metal, [18][19][20] alloy [21][22][23] and metal chalcogenide [24] nanoparticles have been successfully fabricated, resulting in homogeneous and welldefined nanoparticle catalysts that demonstrated enhanced performance for fuel cell applications. However, these liquid-phase synthetic processes suffer many of the same pitfalls as that of conventional wet chemistry methods.…”

Direct synthesis and growth mechanism of 3D dendritic Mg3P2 microstructures

“…So far, phosphides have been prepared by the reduction of phosphates, the reaction of metal oxides and phosphine, the decomposition of phosphite, solvothermal method, plasma method, etc. [10][11][12][13][14][15][16].…”