Microwave synthesis process for nanometer level titaniuym carbide

A microwave synthesis and nano-scale technology, applied in the field of inorganic materials, can solve the problems of difficult process control, complex preparation process and high reaction temperature, and achieve the effects of easy control, simple process and difficult agglomeration

Inactive Publication Date: 2002-05-15
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Looking at these existing technologies for preparing TiC, there are some shortcomings: the reaction temperature is high, all above 1400 °C; the preparation process is complicated, and the process is difficult to control; TiC prepared by the SHS method is a block and needs ball milling , can only reach the micron level after processing, and may also be mixed with various impurities during processing

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In the first step, titanium dioxide (15nm, rutile type, content > 91%) and acetylene carbon black (specific surface area 58.866m 2 / g) Dry in an oven at 105°C to constant weight, weigh 87.7 grams of titanium dioxide and 36 grams of acetylene carbon black;

[0020] The second step is to get 450 grams of zirconia balls, 500 ml of 95% ethanol, add materials, and carry out ball milling and mixing in an alumina ball mill tank (or rubber tank) for 12 hours until uniform;

[0021] The third step is to dry the slurry at 100°C to constant weight;

[0022] The fourth step weighs 75 grams of the mixture and puts it into the MFM-863 microwave sintering furnace, then evacuates for 20 minutes, passes in argon as a protective gas, and the pressure is 1 atm, microwave heating to 1200 ° C, and constant temperature for 30 minutes.

Embodiment 2

[0024] The first step is to combine titanium dioxide (15nm, rutile type, content > 91%) and acetylene carbon black (specific surface area 58.866m 2 / g) Dry in an oven at 80°C to constant weight, weigh 87.7 grams of titanium dioxide and 36 grams of acetylene carbon black;

[0025] The second step is to take 125 grams of zirconia balls, 300 ml of 95% ethanol, add materials, and carry out ball milling and mixing in an alumina ball mill tank (or rubber tank) for 24 hours until uniform;

[0026] The third step is to dry the slurry at 80°C to constant weight;

[0027] The fourth step weighs 75 grams of the mixture and puts it into the MFM-863 microwave sintering furnace, then evacuates for 20 minutes, passes in argon as a protective gas, and the pressure is 1 atm, microwave heating to 1300 ° C, and constant temperature for 20 minutes.

Embodiment 3

[0029] The first step is to combine titanium dioxide (15nm, rutile type, content > 91%) and acetylene carbon black (specific surface area 58.866m 2 / g) Dry in an oven at 90°C to constant weight, weigh 87.7 grams of titanium dioxide and 36 grams of acetylene carbon black;

[0030] The second step is to take 620 grams of zirconia balls, 600 ml of 95% ethanol, add materials, and carry out ball milling and mixing in an alumina ball mill tank (or rubber tank) for 18 hours until uniform;

[0031] The third step is to dry the slurry at 90°C to constant weight;

[0032] Step 4 Weigh 75 grams of the mixture and put it into the MFM-863 microwave sintering furnace, then vacuumize for 20 minutes, pass in argon as a protective gas, the pressure is 1 atm, microwave heating to 1400 ° C, and keep the temperature for 10 minutes.

[0033] Synthesis rate%

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Abstract

The present invention relates to method of synthesizing nano grade titanium carbide by using microwave, it is proceeded as follows: titanium dioxide and acetylene carbon black are over dried to form raw material, then the raw material: zirconium pellet: absolute ethyl alcohol are mixed in ratio 1:1-5:3-6, and ground in ball mill to unifom, over dried microwave heating and synthesizing to obtain product, advantages include: low reaction temperature, simple technological process, easy to control, the obtained TiC powder is not easy to agglomerate, no impurity etc.

Description

(1) Technical field [0001] The invention relates to the technical field of inorganic materials, in particular to a method for synthesizing nanoscale titanium carbide by microwave. (2) Background technology [0002] At present, the general methods for synthesizing titanium carbide (TiC) can be divided into three categories: (1) directly carbonizing TiC with metal titanium or titanium halide; (2) using gaseous titanium halide (such as TiCl 4 ) Synthesize TiC by pyrolysis in a carbon-containing atmosphere; (3) In a controlled atmosphere, reduce TiO by carbothermal reduction at high temperature 2 Synthesis of TiC. The cheaper way to synthesize TiC is to use TiO 2 Prepared by reacting with carbon black at 1700-2100°C. The reaction formula is: [0003] <chemistry num="001"> <chem file="01129991_cml001.xml" / > < / chemistry> But this method has certain limitations. Because the progress of the reaction is affected by the TiO 2 Influenced by the particle size...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/12C01B31/30
Inventor 胡晓力刘阳张伟南陈楷尹虹曾令可陈志雄赵宗亮
Owner SOUTH CHINA UNIV OF TECH
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