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Controllable phase nickel phosphide powder material, and preparation method and formed electrode thereof

A powder material and powder technology are applied in the field of transition metal compound materials, which can solve the problems of difficult control of reaction conditions, easy aggregation of particles, expensive raw materials, etc., and achieve a favorable hydrogen evolution efficiency, good industrial application prospects, and environmental friendliness. Effect

Active Publication Date: 2019-08-06
SOUTHWEST JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solvothermal method has the advantages of low raw material price, high crystal purity, complete crystal growth, and avoiding the leakage of toxic substances, but the particles are easy to aggregate during the reaction.
Most of the products of the metal organic phosphating method are monodisperse and have more active sites, but the expensive raw materials lead to higher product costs
The solid-phase method has a simple process, but its reaction conditions are not easy to control, and the obtained crystals are large in size and easy to aggregate

Method used

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  • Controllable phase nickel phosphide powder material, and preparation method and formed electrode thereof
  • Controllable phase nickel phosphide powder material, and preparation method and formed electrode thereof
  • Controllable phase nickel phosphide powder material, and preparation method and formed electrode thereof

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Embodiment 1

[0059] This embodiment is basically the same as the controllable-phase nickel phosphide powder material of the comparative example three, the only difference is the nickel-phosphorus molar ratio of spherical porous metal nickel powder mixed with red phosphorus powder in step S3, the spherical porous metal nickel powder in step S3 of this example The nickel powder and the red phosphorus powder are mixed according to the molar ratio Ni:P=1 / 5.6.

[0060] This example also prepared an electrode. The specific method is: add carbon nanotube powder with a mass fraction of 33% to the controlled-phase nickel phosphide powder material prepared in this example, mix it evenly, pour it into a tablet machine mold, and press it. tablet to obtain a tableting sample, the pressure used for the tableting is 10MPa, the holding time is 30s, the tableting size is a disc with a diameter of 20mm, and then the obtained tableting sample is put into a vacuum drying oven, The vacuum degree is -0.1Mpa, an...

Embodiment 2

[0066] A preparation method of a controlled-phase nickel phosphide powder material, the steps are as follows:

[0067] S1. The average particle size range of preparation is 10-100μm, and the average specific surface area is 40-78m 2 / g, the average pore size distribution is 29.63 ~ 30.12nm spherical porous metal nickel powder, and the prepared spherical porous metal nickel powder is dried after repeated washing with distilled water;

[0068] S2, grinding the red phosphorus powder until fine and uniform;

[0069] S3. Mix the spherical porous metal nickel powder prepared in step S1 with the red phosphorus powder ground in step S2 according to the molar ratio Ni:P=1 / 5, grind and add absolute ethanol to mix evenly, and obtain nickel after fully vacuum drying Phosphorus mixed powder;

[0070] S4. Put the nickel-phosphorus mixed powder obtained in step S3 into a tube furnace, and under the protection of an inert gas atmosphere, the temperature was raised to 590°C at a heating rate...

Embodiment 3

[0080] A preparation method of a controlled-phase nickel phosphide powder material, the steps are as follows:

[0081] S1. The average particle size range of preparation is 10-100μm, and the average specific surface area is 40-78m 2 / g, the average pore size distribution is 29.63 ~ 30.12nm spherical porous metal nickel powder, and the prepared spherical porous metal nickel powder is dried after repeated washing with distilled water;

[0082] S2, grinding the red phosphorus powder until fine and uniform;

[0083] S3. Mix the spherical porous metal nickel powder prepared in step S1 with the ground red phosphorus powder in step S2 according to the molar ratio Ni:P=1 / 6, grind and add absolute ethanol to mix evenly, and obtain nickel after fully vacuum drying Phosphorus mixed powder;

[0084] S4. Put the nickel-phosphorus mixed powder obtained in step S3 into a tube furnace, and under the protection of an inert gas atmosphere, program the temperature to 610°C at a heating rate of...

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Abstract

The invention discloses a controllable phase nickel phosphide powder material, a preparation method thereof, and an electrode produced from the controllable phase nickel phosphide powder material. Thepreparation method comprises the following steps: S1, preparing spherical porous metal nickel powder; S2, uniformly grinding the red phosphorus powder; S3, mixing the spherical porous metal nickel powder with the red phosphorus powder according to a molar ratio of Ni:P of 1 / 5 to 1 / 6, grinding the obtained mixture, adding a dispersant, performing uniform mixing, and carrying out sufficient vacuumdrying treatment to obtain a nickel-phosphorus mixed powder; and S4, placing the nickel-phosphorus mixed powder in a tubular furnace, carrying out temperature programming to 590-610 DEG C at a heatingrate of 5-20 DEG C / min under the protection of an inert gas atmosphere, keeping the temperature for 30-120 min, and performing furnace cooling to room temperature in order to obtain the controllablephase nickel phosphide powder material. The preparation method has the advantages of mild reaction conditions, simplicity in operation, environmental friendliness, short reaction time, realization ofthe preparation of the biphasic Ni5P4 / Ni2P powder material with a good catalytic performance, and good industrial application prospect.

Description

technical field [0001] The invention relates to a controllable-phase nickel phosphide powder material, a preparation method thereof and an electrode formed thereof, belonging to the field of transition metal compound materials. Background technique [0002] Transition metal phosphides are a class of compounds that appear after transition metal carbides and transition metal nitrides. It is composed of transition metal elements (such as: W, Fe, Co, Ni, Cu, Mo, etc.) and phosphorus (P) Formed transition metal compound materials with multiphase states. Such compounds have good electrical conductivity and chemical stability. Therefore, it is widely used in hydrocarbon deoxygenation reaction, electrolysis water reaction, photocatalytic hydrogen evolution reaction, hydrodesulfurization reaction, etc. In the process of hydrogen production by electrolysis of water, the key to large-scale hydrogen production is efficient and cheap catalysts. Efficient hydrogen evolution electrode m...

Claims

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Application Information

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IPC IPC(8): C25B1/04C25B11/06B22F9/08C01B25/08
CPCB22F9/082C01B25/08C01P2002/72C01P2004/03C01P2004/61C01P2006/12C01P2006/17C01P2006/40C25B1/04C25B11/04Y02E60/36
Inventor 徐轶李丹兰伟
Owner SOUTHWEST JIAOTONG UNIV