A carbon-coated tungsten-doped metal phosphide and its preparation method

A metal phosphide and tungsten doping technology, which is applied in the preparation/purification of carbon, phosphide, phosphorus compounds, etc., can solve the problems of easy agglomeration and instability, and achieve the effect of small particle size and controllable structural units

Active Publication Date: 2022-01-04
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are disadvantages such as active chemical properties, instability, and easy reunion.

Method used

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  • A carbon-coated tungsten-doped metal phosphide and its preparation method
  • A carbon-coated tungsten-doped metal phosphide and its preparation method
  • A carbon-coated tungsten-doped metal phosphide and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1) Weigh 0.016g WCl 6 , 1.412g C 15 h 21 FeO 6 and 3g NaH 2 PO 2 Pour it into a ball mill jar, add 100ml of absolute ethanol, wherein the molar ratio of W element to Fe element is 0.1:1.

[0028] 2) Place the ball mill jar on a planetary ball mill, and mill for 5 hours at a revolution speed of 300r / min and an autorotation speed of 400r / min.

[0029] 3) Put the ball mill jar into an oven at 60°C to obtain uniformly mixed precursor powder.

[0030] 4) Perform high-temperature phosphating heat treatment on the precursor powder. The heat treatment process is: in N 2 In the atmosphere, the temperature was raised to 300°C at a rate of 2°C / min, kept for 3 hours, and then naturally cooled to room temperature. After taking it out, you get W 0.1 - FeP / C nanoparticles.

[0031] The phase of the carbon-coated tungsten-doped iron phosphide particles prepared in this example is FeP, image 3 It is a scanning electron microscope picture of the iron-cobalt phosphide nano-part...

Embodiment 2

[0033] 1) Weigh 0.008g WCl 6 , 1.412g C 15 h 21 FeO 6 and 3g NaH 2 PO 2 Pour it into a ball mill jar and add 100ml of absolute ethanol, wherein the molar ratio of W element to Fe element is 0.05:1.

[0034] 2) Place the ball mill jar on a planetary ball mill, and mill for 5 hours at a revolution speed of 300r / min and an autorotation speed of 400r / min.

[0035] 3) Put the ball mill jar into an oven at 60°C to obtain uniformly mixed precursor powder.

[0036] 4) Perform high-temperature phosphating heat treatment on the precursor powder. The heat treatment process is: in N 2 In the atmosphere, the temperature was raised to 300°C at a rate of 2°C / min, kept for 3 hours, and then naturally cooled to room temperature. After taking it out, you get W 0.05 - FeP / C nanoparticles.

[0037] The phase of the carbon-coated tungsten-doped iron phosphide particles prepared in this example is FeP, and the size of the nanoparticles is about 17 nm.

Embodiment 3

[0039] 1) Weigh 0.024g WCl 6 , 1.412g C 15 h 21 FeO 6 and 3g NaH 2 PO 2Pour it into a ball mill jar, add 100ml of absolute ethanol, wherein the molar ratio of W element to Fe element is 0.15:1.

[0040] 2) Place the ball mill jar on a planetary ball mill, and perform ball milling for 6 hours at a revolution speed of 400r / min and an autorotation speed of 500r / min.

[0041] 3) Put the ball mill jar into an oven at 60°C to obtain uniformly mixed precursor powder.

[0042] 4) Perform high-temperature phosphating heat treatment on the precursor powder. The heat treatment process is: in N 2 In the atmosphere, the temperature was raised to 300°C at a rate of 2°C / min, kept for 3 hours, and then naturally cooled to room temperature. After taking it out, you get W 0.15 - FeP / C nanoparticles.

[0043] The phase of the carbon-coated tungsten-doped iron phosphide particles prepared in this example is FeP, and the size of the nanoparticles is about 20 nm.

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Abstract

The invention discloses a preparation method of a carbon-coated tungsten-doped metal phosphide material. The preparation method comprises: 1) using tungsten chloride, metal organic salt, and sodium hypophosphite as raw materials, adding absolute ethanol, and obtaining a precursor powder by ball milling; 2) heat-treating the precursor powder under an inert atmosphere to obtain A carbon-coated tungsten atom-doped metal phosphide material is obtained. The chemical composition general formula of the material prepared by this method is W x ‑MP y / C, where W is tungsten element, x is the molar ratio of tungsten atom to M metal element, ranging from 0.05 to 0.15, and M can be any one of Co, Ni, Fe or any combination of several kinds in any ratio. The tungsten-doped metal phosphide prepared by the method is composed of nanoparticles with a size of about 10-20nm, and the surface is coated with a carbon layer of 2-3nm. The preparation method of the invention has the characteristics of simple preparation process and uniform size of the obtained nano particles, and the prepared material can be applied to catalysts, supercapacitors, lithium ion batteries and the like.

Description

technical field [0001] The invention belongs to the technical field of nanoparticle and carbon composite material preparation, and in particular relates to a carbon-coated tungsten-doped metal phosphide and a preparation method thereof. Background technique [0002] The composite material of carbon and nanoparticles can not only retain the chemical activity of the nanoparticles, but also increase the chemical stability of the overall material due to the existence of the carbon layer. Common forms of carbon and particle composites are as follows: carbon fiber composite with nanoparticles; carbon layer or carbon nanosheet composite with nanoparticles; three-dimensional network porous carbon coated nanoparticles. Because its size is close to the coherence length of electrons, the properties of nanoparticles have changed greatly due to the self-organization brought about by strong coherence, which can provide larger specific surface area and higher chemical activity. However, t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/08C01B32/05B82Y40/00
CPCC01B25/08C01B25/088C01B32/05B82Y40/00C01P2004/64C01P2004/80C01P2004/03C01P2002/72
Inventor 洪樟连全鑫瑶支明佳
Owner ZHEJIANG UNIV
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