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Method for preparing transition metal phosphide through chemical vapor deposition by using microwave plasmas

A chemical vapor deposition, microwave plasma technology, applied in phosphide and other directions, can solve the problems of low crystallinity, restricting catalytic performance, and improving reliability.

Inactive Publication Date: 2019-01-08
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

With the continuous development of the field of catalysis, transition metal phosphides have gradually attracted people's attention due to their stable and efficient hydrogen production performance, and have become the focus of research in the field of new material catalysis, but currently prepared transition metal phosphides generally contain nanoparticles. The problem of large particle size and low crystallinity restricts its catalytic performance, and its reliability needs to be improved.

Method used

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  • Method for preparing transition metal phosphide through chemical vapor deposition by using microwave plasmas
  • Method for preparing transition metal phosphide through chemical vapor deposition by using microwave plasmas
  • Method for preparing transition metal phosphide through chemical vapor deposition by using microwave plasmas

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Embodiment 1

[0024] The method for preparing cobalt phosphide by microwave plasma chemical vapor deposition in this embodiment comprises the following steps:

[0025] 1) Put the ceramic boat filled with sodium hypophosphite solid and the cobalt hydroxide precursor nanosheets (grown on the carbon cloth substrate) together in the center of the graphite platform in the cavity, and vacuum the cavity to a vacuum degree of 0.5torr .

[0026] 2) Feed nitrogen gas into the cavity, and when the cavity reaches a certain pressure, adjust the microwave power, and the nitrogen gas inside the cavity absorbs microwaves to generate nitrogen plasma and phosphine plasma. Process parameters: Microwave power is 400W, working air pressure is 17torr.

[0027] 3) Adjust the flow of nitrogen gas to keep the air pressure in the chamber within a certain range, so that the plasma state is stable and wraps the sample for a period of time. Process parameters: The nitrogen flow rate is 30sccm, the chamber pressure is...

Embodiment 2

[0031] In this embodiment, the method for preparing cobalt phosphide and cobalt nickel phosphide by microwave plasma chemical vapor deposition comprises the following steps:

[0032] 1) Put the ceramic boat filled with solid sodium hypophosphite and cobalt-nickel hydroxide precursor nanosheets (grown on the carbon cloth substrate) into the center of the graphite platform in the cavity, and vacuum the cavity to a vacuum degree of 0.5 torr.

[0033] 2) Feed nitrogen gas into the cavity, and when the cavity reaches a certain pressure, adjust the microwave power, and the nitrogen gas inside the cavity absorbs microwaves to generate nitrogen plasma and phosphine plasma. Process parameters: Microwave power is 400W, working air pressure is 17torr.

[0034] 3) Adjust the flow of nitrogen gas to keep the air pressure in the chamber within a certain range, so that the plasma state is stable and wraps the sample for a period of time. Process parameters: The nitrogen flow rate is 30sccm...

Embodiment 3

[0038] The present embodiment prepares the method for iron phosphide by microwave plasma chemical vapor deposition, comprises the following steps:

[0039] 1) Put the ceramic boat filled with sodium hypophosphite and the iron hydroxide precursor nanorods (grown on the carbon cloth substrate) together in the center of the graphite platform in the cavity, and vacuum the cavity to a vacuum degree of 0.5 torr.

[0040] 2) Introduce nitrogen gas into the cavity, when the cavity reaches a certain pressure, adjust the microwave power, nitrogen and phosphine gas inside the cavity absorb microwaves to generate nitrogen plasma and phosphine plasma. Process parameters: The heating temperature is 300°C, the microwave power is 400W, and the working pressure is 17torr.

[0041] 3) Adjust the flow of nitrogen gas to keep the air pressure in the chamber within a certain range, so that the plasma state is stable and wraps the sample for a period of time. Process parameters: The nitrogen flow ...

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Abstract

The invention discloses a method for preparing transition metal phosphide through chemical vapor deposition by using microwave plasmas. The method comprises the following steps: (1) putting a ceramicboat with sodium hypophosphite and a hydroxide precursor nano piece of a transition metal onto a graphite table in a cavity together, closing the cavity, and vacuumizing the cavity; (2) feeding nitrogen into the cavity, and adjusting microwave power to generate nitrogen plasmas and phosphine plasmas; (3) adjusting the flow rate of the nitrogen to maintain the gas pressure in the cavity within a range of 15 to 23 torr, ending the reaction after the state of the plasmas is stable and the plasmas cover the sample for reaction for 0.5 to 3 min, and shutting off a microwave source; (4) after the cavity is cooled, taking out the sample, thereby obtaining the transition metal phosphide. Nano particles of the transition metal phosphide prepared by the method are small in particle size and high incrystallinity, so that the catalysis performance and the reliability of the transition metal phosphide are improved; test and characterization of the catalysis field are facilitated, and the electrocatalytic characteristic of the transition metal phosphide can be researched favorably.

Description

technical field [0001] The invention relates to the field of nanometer material preparation, in particular to a method for preparing transition metal phosphide by microwave plasma chemical vapor deposition. Background technique [0002] Due to the rapid decline of petroleum fuels, hydrogen energy has attracted widespread attention as a clean and sustainable energy source. However, today's high-performance hydrogen production catalysts are generally noble metal materials represented by rare Pt, so it is very important to develop non-precious metal hydrogen production catalyst substitutes. With the continuous development of the field of catalysis, transition metal phosphides have gradually attracted people's attention due to their stable and efficient hydrogen production performance, and have become the focus of research in the field of new material catalysis, but currently prepared transition metal phosphides generally contain nanoparticles. The problem of large particle siz...

Claims

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Application Information

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IPC IPC(8): C01B25/08
CPCC01B25/08C01P2002/72C01P2004/03
Inventor 王加瑞金秋焱崔浩吴俊凤
Owner SUN YAT SEN UNIV
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