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Preparation method of polyhedral transition metal carbide particles for catalytic material

A technology of carbide particles and transition metals, which is applied in the field of preparation of polyhedral transition metal carbide particles, can solve the problem that particle size, morphology and specific crystal plane cannot be well controlled, and transition metal carbides cannot achieve large-scale controllable preparation , the preparation process cannot be controlled, etc., to achieve the effect of regular shape, uniform size and sufficient reaction

Active Publication Date: 2021-03-26
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The preparation method of transition metal carbides in the prior art is a self-propagating high-temperature preparation technology. However, in the process of preparing transition metal carbides in this method, due to the fast combustion reaction speed, the release of a large amount of heat and the uneven temperature field, resulting in The preparation process cannot be controlled, making the prepared particle size uneven, and may even lead to irregular shapes
[0004] The current problem is that the large-scale controllable preparation of transition metal carbides cannot be achieved, and the particle size, morphology and specific crystal planes cannot be well controlled, which limits the practical application of transition metal carbides in catalysis. Therefore, It is urgent to develop a carbide particle with regular shape, uniform size and high catalytic activity.

Method used

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  • Preparation method of polyhedral transition metal carbide particles for catalytic material
  • Preparation method of polyhedral transition metal carbide particles for catalytic material
  • Preparation method of polyhedral transition metal carbide particles for catalytic material

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preparation example Construction

[0039] The invention provides a method for preparing polyhedral transition metal carbide particles for catalytic materials, comprising the following steps:

[0040] Step 1. Mix aluminum powder, transition metal powder and carbon source evenly in a ball mill, the mass ratio of ball to material in the ball mill is 5:1-20:1, the speed of the ball mill is 50-100r / min, and the ball milling time is 8-24h; The evenly mixed powder is taken out and wrapped in aluminum foil, and pressed into a cylindrical preparation block, and then placed in a graphite grinding tool;

[0041] Wherein, the transition metal powder includes titanium powder, tantalum powder, niobium powder, zirconium powder, tungsten powder and or vanadium powder; the carbon source is carbon black or CNTs.

[0042] The content of the aluminum powder is 40-70wt.%, the molar ratio of the carbon source to the transition metal powder is 0.5-0.8; the purity of the aluminum powder is greater than 99.9%, and the purity of the tra...

Embodiment 1

[0050] Preparation of nano-polyhedral TiC particles with uniform size and regular shape at low temperature: First, weigh Al powder (purity ≥ 99.9%), Ti powder (purity ≥ 99.9%) and CNTs, wherein the Al content is 40wt.%, C / Ti The molar ratio is 0.6, the weighed powder is poured into a ball mill tank, and mixed by a ball mill, wherein the ball mass ratio in the ball mill tank is 15:1, the ball mill speed is 50r / min, and the ball mill time is 24h.

[0051] Then, sieve the uniformly mixed powder from the ball mill jar, weigh 30g of the uniformly mixed powder and wrap it with aluminum foil, and use a metal compressor to press it in a self-made grinding tool to form a cylindrical block with a diameter of 30mm and a height of 10mm.

[0052] After that, put the pressed cylindrical block into a self-made graphite mold, put them together into a vacuum hot-pressing sintering furnace, and start heating after the vacuum is exhausted, wherein the vacuum degree is kept below 10Pa, and the hea...

Embodiment 2

[0055] Preparation of nano-polyhedral TiC particles with uniform size and regular shape at low temperature: first, weigh Al powder (purity ≥ 99.9%), Ti powder (purity ≥ 99.9%) and CNTs, wherein the Al content is 60wt.%, C / Ti The molar ratio is 0.6, the weighed powder is poured into a ball mill tank, and mixed by a ball mill, wherein the ball mass ratio in the ball mill tank is 15:1, the ball mill speed is 50r / min, and the ball mill time is 24h.

[0056] Then, sieve the uniformly mixed powder from the ball mill jar, weigh 30g of the uniformly mixed powder and wrap it with aluminum foil, and use a metal compressor to press it in a self-made grinding tool to form a cylindrical block with a diameter of 30mm and a height of 10mm.

[0057] After that, put the pressed cylindrical block into a self-made graphite mold, put them together into a vacuum hot-pressing sintering furnace, and start heating after the vacuum is exhausted, wherein the vacuum degree is kept below 10Pa, and the hea...

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Abstract

The invention discloses a preparation method of polyhedral transition metal carbide particles for a catalytic material, wherein the preparation method comprises the following steps: step 1, ball-milling and uniformly mixing aluminum powder, transition metal powder and a carbon source, and pressing into a preparation block, wherein the transition metal powder comprises titanium powder, tantalum powder, niobium powder, zirconium powder, tungsten powder and / or vanadium powder, the content of the aluminum powder is 40-70 wt.%, and the molar ratio of the carbon source to the transition metal powderis 0.5-0.8; step 2, heating the preparation block in a vacuum or argon protection state, and cooling to room temperature; and step 3, soaking with hydrochloric acid to remove an aluminum matrix to obtain the polyhedral transition metal carbide particles. According to the method provided by the invention, the nano polyhedral transition metal carbide particles are prepared through medium-low temperature and high temperature combined rapid cooling, and the submicron and micron polyhedral transition metal carbide particles are prepared through secondary heating.

Description

technical field [0001] The invention relates to the technical field of ultra-high temperature ceramic materials, and more specifically, the invention relates to a method for preparing polyhedral transition metal carbide particles used for catalytic materials. Background technique [0002] Transition metal carbides have the advantages of high melting point, high hardness, good electrical conductivity and chemical stability, and are widely used as coating materials, mechanical parts and reinforcing phases in composite materials. Transition metal carbides have attracted extensive attention in catalytic applications since the first report by Levy and Boudart in 1973 that WC possessed Pt-group metal-like catalytic properties in neopentane isomerization. When transition metal carbide particles are used as the reinforcing phase of composite materials, it is generally desired that the particle shape is nearly spherical or spherical. When the particle shape is a regular polyhedron, i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/921C01B32/907B82Y40/00B82Y30/00C25B1/02C25B11/075B01J27/22C01B3/02
CPCC01B32/921C01B32/907B82Y40/00B82Y30/00C25B1/02C25B11/04B01J27/22C01B3/02C01P2004/61C01P2004/64C01P2004/41C01P2004/30B01J35/23Y02E60/50
Inventor 赵庆龙金伟姜启川
Owner JILIN UNIV
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