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Device and method for preparing titanium-boron-nitrogen compound powder
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A technology for preparing nitrogen compounds and powders, applied in boron compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of high cost, many impurities, long time, etc., and achieve high purity of synthetic powder, broad application prospects, and synthesis temperature. low effect
Active Publication Date: 2020-12-25
焦国豪 +1
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2.TiO2 2 Direct carbonization method, which is based on TiO 2 powder as raw material, need to be in H 2 In the atmosphere, react at a temperature of 1600-1950 ° C, high cost and many impurities
[0005] The existing preparation methods for synthesizing TiN powder are: 1, metal Ti powder or TiH 2 The direct nitriding method requires the H 2 ,N 2 In the atmosphere, 1000 ~ 1400 ℃, 30 hours of synthesis conditions, the synthesis time is long
2.TiO2 2 The carbon reduction method requires synthesis conditions of 1380-1800°C and 15 hours, and the synthesis time is long and the purity is not high
[0007] The above method of synthesizing TiC, TiN and Ti(C,N) has high temperature, long time and many impurities
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[0033] Prepare Ti powder, the particle size of the powder is -100 mesh, and the purity is above 95%. Put the Ti powder into the electric furnace, and the electric furnace is sealed and isolated from the outside air.
[0034] 2. Heating electric furnace
[0035] The compound synthesis temperature was set at 700°C, and the electric furnace was heated to 700°C.
[0036] 3. Introduce gas
[0037] When the vacuum degree in the furnace reaches 1x10-2Pa, N2 gas is introduced, and the flow rate is 100-150 liters / hour. When the temperature of the electric furnace reaches 700°C, H2 and BCl3 gases are introduced, and the ratio of N2 and H2 is 75vol%:25vol%. BCl The feed rate of gas is 5vol% of the sum of the above two gases. Keep warm for 3 hours.
[0039] Close each intake valve and vacuum valve, open the furnace door after the furnace temperature drops to room temperature, and take out the synthesized powder product....
[0042] Prepare Ti powder, the particle size of the powder is -150 mesh, and the purity is above 98%. Put the Ti powder into the electric furnace, and the electric furnace is sealed and isolated from the outside air.
[0043] 2. Heating electric furnace
[0044] The compound synthesis temperature was set at 860°C, and the electric furnace was heated to 860°C.
[0045] 3. Introduce gas
[0046] When the vacuum degree in the furnace reaches 1x10-2Pa, N2 gas is introduced, and the flow rate is 100-150 liters / hour. When the temperature of the electric furnace reaches 860°C, H2 and BCl3 gases are introduced, and the ratio of N2 and H2 is 60vol%:40vol%. BCl3 gas feed is the 3vol% of the sum of the above two gases. Keep warm for 3 hours.
[0048] Close each intake valve and vacuum valve, open the furnace door after the furnace temperature drops to room temperature, and take out the synthesized powder product. The che...
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Abstract
The invention relates to a titanium-boron-nitrogen compound powder preparation device and method. The titanium-boron-nitrogen compound powder preparation device consists of a BCl3 gas inlet valve, a H2 gas inlet valve, a N2 gas inlet valve, a vacuum electric furnace and an exhaust port, and precursor titaniumpowder is placed in the vacuum electric furnace. Titanium-boron-nitrogen compound powderis obtained by controlling a chemical reaction of three gases and the precursor titanium powder. Please see the specification for chemical equations involved in the titanium-boron-nitrogen compound powder preparation method, synthesized Ti-B-N is a non-stoichiometric compound, and the composition is variable, wherein x=0.01-2.6, and y=0.1-0.99. The synthesizing device has a simple structure, low manufacturing cost, a simple process, easy operation and high purity of the synthesized product, and is suitable for mass production.
Description
technical field [0001] The titanium-boron-nitrogen powder belongs to the inorganic non-metallic ceramic material and has the characteristics of high hardness and corrosion resistance. The invented device and method are used for synthesizing the titanium-boron-nitrogen powder material and belong to the field of material synthesis. [0002] technical background [0003] The device and method involved in the patent of the present invention are used for titanium-boron-nitrogen / Ti-B-N compound powder, and the powder materials close to Ti-B-N include TiC, TiN and TiCN (the same lattice structure); here, TiC, TiN And the synthesis method of TiCN is compared with the synthesis method we declared. TiCN is a ternary compound formed by the solid solution of C in TiN. It not only has the toughness of TiN, but also inherits the high hardness of TiC. These compounds have high hardness, good wear resistance and strong corrosion resistance. They can be divided into binary and ternary, amon...
Claims
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