A vanadium nitride nanocluster loaded on a 3D carbon foam skeleton and its preparation method

A technology of vanadium nitride nano and carbon foam, which is applied in the direction of carbon preparation/purification, chemical instruments and methods, nitrogen compounds, etc., can solve the problems of large energy consumption, high cost, and complicated operation, and achieve uniform distribution and stable structure , solve the effect of easy reunion

Active Publication Date: 2022-03-11
西安天牛材料科技有限公司
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Problems solved by technology

[0004] The purpose of the present invention is to provide a vanadium nitride nanocluster loaded on a 3D carbon foam skeleton and its preparation method, which solves the problems of high cost, large energy consumption and complicated operation when preparing vanadium nitride, and at the same time prevents nitrogen The vanadium oxide particles agglomerate and keep their shape stable

Method used

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  • A vanadium nitride nanocluster loaded on a 3D carbon foam skeleton and its preparation method
  • A vanadium nitride nanocluster loaded on a 3D carbon foam skeleton and its preparation method

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preparation example Construction

[0022] A method for preparing vanadium nitride nanoclusters loaded on a 3D carbon foam skeleton provided by the invention comprises the following steps:

[0023] In the first step, the melamine foam was placed in a tube furnace and heated at 5 °C min under an argon or nitrogen atmosphere. -1 After calcining at 800°C for 1 hour, and cooling to room temperature, a 3D carbon foam is obtained;

[0024] The second step is to configure an aqueous oxalic acid solution with a pH of 1 to 4;

[0025] The 3rd step, the concentration is the ammonium metavanadate of 10~30mol / L and the hexamethylenetetramine of 1~10mol / L and above-mentioned oxalic acid aqueous solution with (1~3):(1~4):(1 ~5) volume ratio mixed, fully stirred to obtain solution A;

[0026] The fourth step is to vacuum-impregnate the carbon foam in the first step in solution A and transfer it to a polytetrafluoroethylene reactor, and seal it, and at the same time, hydrothermally react at a temperature of 100°C to 150°C for...

Embodiment 1

[0029] In the first step, the melamine foam was placed in a tube furnace and heated at 5 °C min under an argon or nitrogen atmosphere. -1 After calcining at 800°C for 1 hour, and cooling to room temperature, a 3D carbon foam is obtained;

[0030] The second step is to configure an aqueous oxalic acid solution with a pH of 1;

[0031] In the third step, mix the ammonium metavanadate with a concentration of 10 mol / L, the hexamethylenetetramine of 1 mol / L and the above-mentioned oxalic acid aqueous solution in a volume ratio of 1:1:1, and stir fully to obtain solution A;

[0032] The fourth step is to vacuum impregnate the carbon foam in solution A and transfer it to a polytetrafluoroethylene reactor, and seal it. At the same time, it is hydrothermally reacted at a temperature of 100°C for 0.5h, and then it is washed and freeze-dried. get intermediate products;

[0033] The fifth step is to put the intermediate product obtained above into a tube furnace, and under an ammonia at...

Embodiment 2

[0037] In the first step, the melamine foam was placed in a tube furnace and heated at 5 °C min under an argon or nitrogen atmosphere. -1 After calcining at 800°C for 1 hour, and cooling to room temperature, a 3D carbon foam is obtained;

[0038] The second step is to configure an aqueous oxalic acid solution with a pH of 2;

[0039] The third step is to mix the ammonium metavanadate with a concentration of 20mol / L, the hexamethylenetetramine of 5mol / L and the above-mentioned oxalic acid aqueous solution in a volume ratio of 2:3:3, and stir fully to obtain solution A;

[0040] The fourth step is to vacuum impregnate the carbon foam in solution A and transfer it to a polytetrafluoroethylene reactor, and seal it. At the same time, it is hydrothermally reacted at a temperature of 150 ° C for 8 hours, and then it is washed and freeze-dried to obtain mid product;

[0041] The fifth step is to put the intermediate product obtained above into a tube furnace, and under an ammonia at...

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Abstract

The invention provides a vanadium nitride nanocluster loaded on a 3D carbon foam skeleton and a preparation method thereof, comprising the following steps: the first step, carbonizing melamine foam to obtain a 3D carbon foam; the second step, converting the first step The 3D carbon foam body is immersed in solution A, and undergoes hydrothermal reaction; after the reaction is completed and cooled to room temperature, the 3D carbon foam body is washed alternately with water and absolute ethanol, and freeze-dried to obtain an intermediate product; in the third step, the The intermediate product obtained above is calcined, cooled to room temperature after the reaction, and vanadium nitride nanoclusters supported on the 3D carbon skeleton are obtained; the reaction raw material ammonium metavanadate used in the present invention is cheap and easy to obtain, and the hydrothermal method adopted is simple and convenient to operate. It is easy to control, and the finally prepared vanadium nitride nanoclusters loaded on the 3D carbon skeleton are evenly distributed and stable in structure.

Description

technical field [0001] The invention belongs to the field of preparation of inorganic micro-nano materials, and in particular relates to a vanadium nitride nano-cluster loaded on a 3D carbon foam skeleton and a preparation method thereof. Background technique [0002] Transition metal nitrides (M X N Y , M = Ti, V, M O ) is widely used in optical, electrical, magnetic and other fields due to its special crystal structure, and has a broad market prospect, so it has attracted the attention of many researchers, especially vanadium nitride has become a research hotspot. Vanadium nitride has both good electrical conductivity and multivalent states of vanadium, which makes vanadium nitride have good application prospects in lithium-sulfur batteries and supercapacitors. In particular, endowing vanadium nitride with different nano-morphological structures greatly expands its application fields and effectively improves its performance. [0003] At present, the preparation of vana...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/05C01B21/06
CPCC01B21/0617C01B32/05
Inventor 原晓艳王瑞琴黄文瑞郭守武
Owner 西安天牛材料科技有限公司
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