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High-temperature carbonitriding preparation method of nano crystal titanium carbonitride ceramic ultrafine powder

A technology for crystalline nitrogen carbide and high temperature carbon is applied in the field of high temperature carbonitriding reaction preparation, which can solve the problems of restricting large-scale production, impure synthetic products, and high cost of raw materials, and achieve industrial-scale production, high purity, and low cost. The effect of grain growth

Active Publication Date: 2007-03-28
SICHUAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Analyzing the above methods, it will be found that they generally have one or several disadvantages such as high raw material cost, cumbersome process, low yield, impure synthetic product, expensive equipment, etc., thus limiting their industrial scale production

Method used

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  • High-temperature carbonitriding preparation method of nano crystal titanium carbonitride ceramic ultrafine powder

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] In the present embodiment, raw material is nano-titanium dioxide and nano-carbon black, has the following process steps by process flow chart 1:

[0035] (1) Ingredients

[0036] The mol ratio of nano carbon black and titanium dioxide is 2.5;

[0037] (2) Mixing

[0038] The prepared raw materials are mixed by rolling wet milling, the weight ratio of balls to materials is 5:1, the medium is absolute ethanol, the speed of the ball mill is 60 rpm, and the milling time is 8 hours;

[0039] (3) dry

[0040] Dry the material after wet grinding at 70°C for 24 hours;

[0041] (4) Loading

[0042] Weigh 100g of the mixed raw materials and put them into the graphite crucible of carbon tube furnace and compact them;

[0043] (5) High temperature carbonitriding

[0044] Evacuate the carbon tube furnace to a vacuum of 1.5×10 -2 At MPa, start heating at 20°C / min, keep warm at 400°C for 30min, and pass nitrogen to the pressure of 0.005MPa at the end of the heat preservation. ...

Embodiment 2

[0050] In the present embodiment, raw material is nano-titanium dioxide and nano-carbon black, has the following process steps by process flow chart 1:

[0051] (1) Ingredients

[0052] The mol ratio of nano carbon black and titanium dioxide is 2.7;

[0053] (2) Mixing

[0054] The prepared raw materials are mixed by rolling wet milling, the weight ratio of balls to materials is 5:1, the medium is absolute ethanol, the speed of the ball mill is 60 rpm, and the milling time is 8 hours;

[0055] (3) dry

[0056] The material after wet grinding is dried in an oven at 80°C for 24 hours;

[0057] (4) Loading

[0058] Weigh 200g of the mixed raw materials and put them into the graphite crucible of carbon tube furnace and compact them;

[0059] (5) High temperature carbonitriding

[0060] Fill the carbon tube furnace with nitrogen to slightly greater than 1 standard atmospheric pressure, then flow nitrogen and heat at the same time at 15°C / min, and keep warm for 3 hours after r...

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Abstract

The invention is a method for preparing nano-crystalline titanium carbonitride ceramic superfine powder by high temperature carbonitriding reaction, using nano titanium oxide and nano carbon black, and comprising the steps of batching, mixing, drying, charging, high temperature carbonitriding, ball-milling, and screening. And it has simple process, lower cost, saves energy sources as compared with common carbon reduction, and easily implements scale industrialized production. By controlling reaction temperature, heat preserving time, nitrogen gas pressure (or flow), C-Ti ratio and other process factors, it can synthesize titanium carbonitride nano-crystalline superfine powders of various N contents. And the prepared powder is ball-shaped, has good dispersivity, and average grain size of 100-200nm, average crystal grain size of 20-50 nm and purity up to above 99%.

Description

1. Technical field [0001] The invention relates to a high-temperature carbonitriding reaction preparation method of nanocrystalline titanium nitride carbide ceramic superfine powder. 2. Background technology [0002] At present, known methods for preparing titanium nitride carbide ultrafine and nanopowders include plasma methods, such as: "Synthesis of ultrafine titanium carbonitride solid solution micropowder by plasma method" by Zeng Daquan et al. , 1991, 1103-1106); high-energy mechanical ball milling method, for example: the paper "Low temperature mechanochemical formation of titanium carbonitride" by Kerr.A et al. (see NanoStructured Materials, 1999, 11(2), 233-239)); sol -Gel method, for example, the paper "Synthesis of Ti(C,N) ultrafine powders by carbothermal reduction of TiO 2 derived from sol-gel process" (see Journal of the European Ceramic Society, 20(2000), 933-938); low-temperature chemical method, for example: the paper "A simple route to prepare nanocrystal...

Claims

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Application Information

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IPC IPC(8): C04B35/58C04B35/56C04B35/622
Inventor 向道平刘颖赵志伟曹泓高升吉涂铭旌
Owner SICHUAN UNIV
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