A preparation process of transition metal carbide powder and transition metal carbide-nitride composite powder

A transition metal and composite powder technology, applied in the field of powder metallurgy, can solve the problems of coarse powder particles, high impurity content, and low output requirements of vapor deposition method.

Active Publication Date: 2021-12-28
LONGYAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods have their own limitations. The traditional reduction method and direct carbon / nitridation method usually need to be carried out at a higher temperature (1600-2200 ° C), and the prepared powder particles are coarse and uneven; the self-propagating combustion synthesis method It is difficult to control the preparation process and the uniformity of grains; the vapor deposition method is suitable for the situation with low output requirements; the mechanical alloying method is the method of using ball milling, through the contact between the ball and the ball and between the ball and the ball mill. The collision causes plastic deformation, work hardening and crushing of the powder particles. After the particles are refined, the surface activity increases. As the impact time of the grinding ball increases, diffusion reactions occur between atoms
In the invention patent application CN102249231A, carbon-containing organic solvents and transition metals are used as raw materials, and nano-transition metal carbides are prepared by ball milling. The average grain size is less than 20nm, but the impurity content is relatively high, and the performance is not ideal

Method used

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  • A preparation process of transition metal carbide powder and transition metal carbide-nitride composite powder
  • A preparation process of transition metal carbide powder and transition metal carbide-nitride composite powder
  • A preparation process of transition metal carbide powder and transition metal carbide-nitride composite powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Glove box (1) in an argon environment protection, material selection 200 mesh titanium metal powder, the quality of 50g, purity 99.9%, the carbon-containing organic solvent is toluene, 18ml volume, carbide ball 500g, raw materials and ball into a stainless steel ball mill jar, after packaging in a ball mill rotating at 350 rev / min, the milling time was 30 hours, the nano powder after milling in vacuum (degree of vacuum figure 1 , image 3 Indicated.

[0024] (2) the resulting milled titanium carbide, titanium hydride composite powder was placed in a high temperature vacuum furnace (the degree of vacuum figure 2 Indicated. Titanium hydride decomposition after heat treatment, thermal processing, decomposition of the hydride to give the pure titanium metal, titanium metal, after reaction with the titanium carbide titanium carbide solid solution of a non-stoichiometric, such as image 3 , The carbon to titanium carbide powder was 7:10 molar ratio of titanium, oxygen content of ...

Embodiment 2

[0031] Glove box (1) in an argon environment protection, material selection 200 mesh titanium metal powder, the quality of 50g, purity 99.9%, containing carbon, the organic solvent is ethylene diamine N, a volume of 15ml, carbide ball 500g, raw materials and stainless steel ball mill pot was charged, after packaging in a ball mill, a rotational speed of 300 revolutions / minute 30 hours milling, milled powder was removed in vacuo (vacuum Figure 4 , Figure 5 Indicated.

[0032] (2) The ball-milled titanium carbide, titanium carbonitride, titanium hydride, titanium nitride in the composite powder is placed in a high temperature vacuum furnace (the degree of vacuum Figure 6 Shown), the carbon composite powder, the molar ratio of nitrogen to titanium of 6: 2: 10, an oxygen content of 0.40%. The preparation of ultrafine titanium carbide, titanium nitride powder and 10% mass fraction of 20% of molybdenum metal and nickel ball mill mixing, the mixed powder was placed in a graphite compos...

Embodiment 3

[0034] (1) Among the metal-resistant glove boxes, the raw materials were selected from 200 mesh metal titanium powder and metal zirconium powder, titanium and zirconium atomic ratio of 8: 2, with a total mass of 50 g, and the purity was 99.9%, including The carbon or organic solvent is toluene, the volume is 16mL, the carbonide mill is 500g, the raw material and the grinding ball are loaded into the stainless steel ball grinding, and the ball mill is loaded into the ball mill. After 20 hours of rotation of 300 rpm, the powder is removed from the powder. 2 hours were dried in vacuum (vacuum Figure 7 , Figure 8 Indicated.

[0035] (2) Titanium carbide, carbonized zirconium, hydrogenide, and hydrogenide, and hydrogenated, and hydrogenated, and the vacuum is set to 10 ° C / min, and the temperature is 900 ° C, the temperature is 5 min. . The prepared composite powder average grain size 300 nm (eg Figure 9 The standard PDF card, which compares titanium carbide and carbon zirconium, the...

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Abstract

The invention discloses a preparation process of transition metal carbide powder and transition metal carbide-nitride composite powder. The present invention uses a ball milling method to mix a transition metal with a certain amount of organic solvent containing carbon or carbon and nitrogen at the same time. After ball milling for a certain period of time, transition metal carbides or transition metal carbides with an average grain size of less than 50nm are obtained. The nitride composite powder contains a certain amount of transition metal hydride nano powder. The prepared powder is heat-treated under vacuum (<1Pa) or argon environment to obtain transition metal carbide or carbide-nitride composite powder, and the transition metal grain size distribution of 50-900nm is prepared by controlling the heating rate and heat treatment time. For metal carbide powders and transition metal carbide-nitride composite powders, the carbon and nitrogen contents varied with the ball milling time and the amount of organic solvent. The invention has simple process and is easy to produce, and can be used for preparing high-performance metal ceramics.

Description

Technical field [0001] The present invention is in the field of powder metallurgy, in particular to a transition metal carbide and transition metal carbide powder - Preparation of a composite nitride powder. Background technique [0002] Transition metal carbides, nitrides having high strength and hardness, as a binder metal can be used to prepare the cermet, widely used in metal cutting, mineral extraction, producing wear member. Transition metal compounds such as carbon TaC, ZrC, HfC, NbC, TiC and the like more than a melting point of 3000 deg.] C, and are ultra high temperature structural materials comprising a high temperature oxidation resistance, can accommodate a long time hypersonic flight, atmospheric re-entry, and rocket propulsion systems extreme environments, for aircraft nose cone, wing leading edge, and a nuclear reactor and other critical engine components. [0003] Transition metal carbides, nitrides synthetic preparation include reduction, direct carbon / nitridi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/921C01B21/076C01B32/914C22C1/05C22C29/10
CPCC22C1/051C22C29/10C01B21/0761C01B32/914C01B32/921C01P2004/62C01P2004/64C01P2004/80C01P2004/82
Inventor 刘少存向建勇柳忠元廖娟秀
Owner LONGYAN UNIV
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