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System and method for producing TiN, TiC and TiCN powder

A powder and inert gas technology is applied in the field of powder preparation, TiN, TiC, TiCN powder preparation technology. , the effect of raw material economy

Active Publication Date: 2019-08-23
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, although the Mg thermal or Na thermal reduction method improves the nitriding or (and) carbonization efficiency of TiCl4 raw materials, the prepared powder has a high impurity content (Na or Mg), and the metal element needs to be gasified at high temperature. , there is serious corrosion, which leads to complicated process, and has not yet achieved industrial production
[0008] In summary, although there are many methods to prepare TiN, TiC, and TiCN powders, there is a lack of new processes that can meet the low-cost and high-efficiency preparation of TiN, TiC, and TiCN powders in the industry.

Method used

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  • System and method for producing TiN, TiC and TiCN powder
  • System and method for producing TiN, TiC and TiCN powder
  • System and method for producing TiN, TiC and TiCN powder

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Experimental program
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Effect test

Embodiment 1

[0046] combine figure 1 , the system used in this embodiment to produce TiN, TiC, TiCN powders includes powder feeding device 1, TiCl 4 Evaporation device 2, heating device 2-1, deposition reaction fluidized bed 3, cyclone separation device 4, high temperature dust removal device 5, first water cooling device 6, fine powder collection device 7, second water cooling device 8, TiCl 4 Recovery device 9, tail gas treatment device 10, powder collection device 11;

[0047] The air inlet at the bottom of the powder feeding device 1 is connected to the inert gas pipeline through an air valve and the pipeline; The valve is connected to the pipeline;

[0048] The TiCl 4 The evaporation device 2 is equipped with the heating device 2-1; the TiCl 4 The gas inlet of evaporation device 2 is connected with inert gas pipeline and hydrogen pipeline through gas valve and pipeline; 4 The exhaust port of the evaporating device 2 is connected with the gas inlet at the bottom of the deposition ...

Embodiment 2

[0056] In this embodiment, the method for producing TiN, TiC, and TiCN powders using the system in the above-mentioned embodiment 1 specifically includes the following steps:

[0057] The target seed powder is cleaned with an inert gas in the powder feeding device 1 to remove physically or chemically adsorbed air impurities, and is transported into the deposition reaction fluidized bed 3 through material valves and pipelines; inert gas and / or h 2 Through the TiCl 4 Evaporation device 2 TiCl 4 Loaded into the deposition reaction fluidized bed 3; inert gas, nitrogen source gas, carbon source gas, and hydrogen enter the deposition reaction fluidized bed 3 through gas valves and pipelines, and the target seed powder is in a fluidized state in an inert atmosphere. oxidized state, while the TiCl 4 React with nitrogen source gas, carbon source gas, and hydrogen to synthesize TiN, TiC, and TiCN powders, and the synthesized powders are attached to the target seed powder to form new ...

Embodiment 3

[0060] In this embodiment, on the basis of the above-mentioned embodiment 2, TiC is the target seed powder with a particle size of 5 μm. The TiCl 4 The temperature of the evaporator 2 was 25°C. The temperature of the deposition reaction fluidized bed 3 is 900°C, the average residence time of the powder is 30min, and the carbon source gas is CH 4 , C content in carbon source gas and TiCl 4 The ratio of the Ti content in the medium is 1. The powder in the fine powder collection device 7 is submicron TiC powder, and the powder in the powder collection device 11 is micron TiC powder. figure 2 is the XRD pattern of the obtained powder. It can be seen from the figure that the powder is a single-phase TiC powder, and Ti / C≈1.

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Abstract

The invention discloses a system and a method for producing TiN, TiC and TiCN powder. Target seed powder is added in a fluidized bed in advance and fluidized by an inert gas, and then the TiN, TiC andTiCN powder are synthesized in the fluidized bed by gaseous TiCl 4 and a nitrogen source or (and) carbon source gas under a certain temperature range. The method solves the problems of low efficiency, easy coating formation and difficult powder formation in a chemical vapor deposition process based on TiCl 4 raw materials, improves the efficiency of preparing the TiN, TiC and TiCN powder, has simple process flow, does not need expensive equipment, can realize continuous batch production of the TiN, TiC and TiCN powder, and has good economic and social benefits.

Description

technical field [0001] The invention belongs to the field of materials and chemical industry, and relates to a preparation method of powder, in particular to a preparation process of TiN, TiC and TiCN powder. Background technique [0002] TiN, TiC, and TiCN are widely used in mechanical processing, aerospace, petrochemical, electronic information, bioelectrochemistry, etc. field has a wide range of applications. For example, TiN, TiC, and TiCN can be used as tool materials, mold materials, anti-corrosion materials, conductive ceramic materials, electrode materials, decorative materials, energy-saving materials, wear-resistant materials or biocompatible materials. TiN, TiC, TiCN powder is the basis for preparing these high-performance TiN, TiC, TiCN materials. After decades of continuous research and development, there are currently the following major categories of preparation methods: [0003] (1) Direct nitriding or (and) carbonization method, that is, directly nitridin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/076
CPCC01B21/0763C01B32/90C01B32/921C01P2002/72C01P2004/03C01P2004/60C01P2004/61
Inventor 向茂乔朱庆山宋淼
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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