CN109678168B - Titanium-boron-nitrogen compound powder preparation device and method - Google Patents

Titanium-boron-nitrogen compound powder preparation device and method Download PDF

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CN109678168B
CN109678168B CN201811431029.XA CN201811431029A CN109678168B CN 109678168 B CN109678168 B CN 109678168B CN 201811431029 A CN201811431029 A CN 201811431029A CN 109678168 B CN109678168 B CN 109678168B
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焦国豪
胡建东
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    • C01B35/00—Boron; Compounds thereof
    • C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
    • C01B35/14—Compounds containing boron and nitrogen, phosphorus, sulfur, selenium or tellurium
    • C01B35/146—Compounds containing boron and nitrogen, e.g. borazoles
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/58007—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on refractory metal nitrides
    • C04B35/58014—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on refractory metal nitrides based on titanium nitrides, e.g. TiAlON
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/583—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride
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    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
    • C04B35/6265—Thermal treatment of powders or mixtures thereof other than sintering involving reduction or oxidation
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40—Metallic constituents or additives not added as binding phase
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/46—Gases other than oxygen used as reactant, e.g. nitrogen used to make a nitride phase

Abstract

The invention relates to a device and a method for preparing titanium-boron-nitrogen compound powder. The device consists of BCl3、H2And N2Three gas inlet valves, a vacuum electric furnace and an exhaust port, wherein the precursor titanium powder is placed in the vacuum electric furnace. The titanium-boron-nitrogen compound powder is obtained by controlling the chemical reaction method of the three gases and the precursor titanium powder. The chemical reaction equation involved in the method is as follows: 2BCl3→2[B]+3Cl2，2BCl3+3H2→2[B]+6HCl，N2→2[N]，Ti+x[B]+y[N]→TiBxNyThe synthesized Ti-B-N is a non-stoichiometric compound with variable components, wherein x is 0.01-2.6; y is 0.1-0.99. The synthesis device has the advantages of simple structure, low manufacturing cost, simple process, easy operation and high purity of the synthesized product. Is suitable for batch production.

Description

Titanium-boron-nitrogen compound powder preparation device and method
Technical Field
The invention relates to titanium-boron-nitrogen powder, which belongs to an inorganic non-metallic ceramic material and has the characteristics of high hardness and corrosion resistance.
Technical Field
The invention relates to a device and a method for preparing titanium-boron-nitrogen/Ti-B-N compound powder, wherein powder materials similar to Ti-B-N comprise TiC, TiN and TiCN (the lattice structures are the same); the synthesis of TiC, TiN and TiCN is compared to what we claim. TiCN is a ternary compound formed by dissolving C in TiN in a solid solution mode, has the toughness of TiN and inherits the high hardness characteristic of TiC. These compounds have high hardness, good wear resistance and strong corrosion resistance. They can be divided into binary and ternary, where TiC and TiN belong to the binary compounds and TiCN to the ternary compounds.
For synthesizing TiC powderThe existing methods at the end include: a direct carbonization method for producing high-purity H from Ti powder or TiH2 powder in graphite container and carbonizing induction furnace2And gas is heated at the temperature of 1500-1700 ℃, the required temperature is high, and powder particles are easy to sinter. 2, TiO2Direct carbonisation by TiO2The powder is used as raw material and needs to be in H2The reaction is carried out in the atmosphere at 1600-1950 ℃, the cost is high, and the impurities are more.
The existing preparation methods for synthesizing TiN powder are: 1, metal Ti powder or TiH2Direct nitridation method, requiring the use of H2,N2In the atmosphere, the synthesis time is long under the synthesis conditions of 1000-1400 ℃ and 30 hours. 2, TiO2The carbon reduction method needs 1380-1800 ℃ and 15 hours of synthesis conditions, and has long synthesis time and low purity.
The preparation method of the powder for synthesizing Ti (C, N) comprises the following steps: 1, a high-temperature diffusion method of TiC and TiN needs hot-pressing and solid solution at 1700-1800 ℃ in Ar. 2, high temperature nitriding method, which takes TiC + Ti as raw material in H2,N2In the atmosphere, the components are difficult to control because the solution is formed by hot pressing at high temperature.
The method for synthesizing TiC, TiN and Ti (C, N) has high temperature, long time and more impurities.
Disclosure of Invention
The Ti-B-N powder synthesis device and method provided by the inventor is a new method which is not available at home and abroad, and compared with the three existing similar powder materials, the method has the advantages of low synthesis temperature, short time and high purity of synthesized powder. The synthesized material is a new material which is not available in China.
The invention provides a titanium-boron-nitrogen compound powder preparation device, which comprises: BCl3、H2And N2Three gas inlet valves, an electric furnace and a vacuum pump; the electric stove is vacuum electric heater, and the electric stove is sealed isolated with the outside air, is equipped with furnace gate, gas outlet and air inlet on it, and titanium powder is put in the electric stove, three kinds of gas admission valves are established on the admission line, include: a boron trichloride gas control valve I, a hydrogen gas control valve II, a boron trichloride and hydrogen gas mixed gas control valve III and a nitrogen gas control valve IV, andand the boron trichloride gas and the hydrogen are respectively mixed through a valve I and a valve II and then enter the electric furnace through a valve III, the nitrogen enters the electric furnace through a valve IV, waste gas is discharged from a gas outlet of the electric furnace, the vacuum valve controls the vacuum in the electric furnace, and the air in the furnace is discharged through a vacuum pump to keep the vacuum.
The device is adopted to carry out a preparation method of the titanium-boron-nitrogen compound powder, a synthetic product, namely the titanium-boron-nitrogen compound powder, is obtained by controlling the chemical reaction of the three gases and the precursor titanium powder, and the synthetic process follows the following chemical reaction equation:
2BCl3→2[B]+3Cl2
2BCl3+3H2→2[B]+6HCl
N2→2[N]
Ti+x[B]+y[N]→TiBxNy
x in the synthetic compound is 0.01-2.6; y is 0.1-0.99, wherein x and y represent the chemical composition of the elements B and N, respectively.
Ti-B-N powder is synthesized through the chemical reaction. BCl3Decomposition into reactive B atoms and Cl2；BCl3And H2Reaction to generate activity [ B]Atoms and HCl; n is a radical of2Decomposition into active [ N ]]An atom; ti and active [ N ]]And [ B]Atoms form the final product Ti-B-N. [ B ]]And [ N]The active atoms diffuse into the Ti powder and combine with the Ti atoms to produce a Ti-B-N compound. Since Ti powder contains a large number of pores, these active atoms easily diffuse from the surface to the heart to achieve a complete reaction. The diffusion reaction can completely change all Ti powder into Ti-B-N powder material under the condition of high enough temperature and long enough holding time. This is an innovation over other powder preparation methods.
The formation of Ti-B-N powder particles undergoes nucleation and growth processes, the final size of which depends on the original Ti powder size and the synthesis temperature. The smaller the original size, the lower the synthesis temperature, the smaller the particle size of the powder produced.
The preparation of the Ti-B-N powder material is realized by the following operation steps:
step one, preparing Ti powder
Preparing Ti powder with granularity of-100 to-500 meshes and purity of more than 95 percent, and putting the Ti powder into an electric furnace which is sealed and isolated from the outside air.
Step two, heating the electric furnace
The electric furnace is heated to a set temperature, and the temperature can be set within the range of 700-1100 ℃. The specific temperature depends on the desired particle size, and the higher the synthesis temperature, the larger the powder particles.
Step three, introducing gas
When the vacuum degree in the furnace reaches 1x10-2Introducing N at Pa2The flow rate of the gas was 100-150 l/h. After reaching the set temperature, the temperature is switched on H2And BCl3Gas, N2And H2The proportion of (A) is 50-75 vol% to 25-50 vol%. BCl3The amount of the gas introduced is 1 to 5 vol% of the total amount of the two gases. And (3) preserving heat for 2-5 hours, wherein when the quantity of Ti powder is large, the heat preservation time needs to be properly prolonged to 6-8 hours.
Step four, discharging
After the time comes, H is closed2、BCl3Gas valves and electric furnace power supply. Closing N when the furnace temperature is reduced to 300-500 DEG C2An air valve. Keeping the vacuum in the furnace not lower than 1x10 in the temperature reduction process-2Pa. And when the temperature is reduced to the room temperature, closing the vacuum valve, opening the furnace door, and taking out the Ti-B-N powder.
The particle size distribution of the synthesized Ti-B-N powder material is from nanometer to micron. The chemical formula of the Ti-B-N compound is TiBxNyWherein x is 0.01-2.6; y is 0.1-0.99.
The synthesized powder has wide application prospect and is suitable for being used as an additive for laser 3D printing and metal composite materials to prepare various composite materials; is suitable for being used as a high-pressure oxygen explosion spraying and plasma spraying raw material to prepare various surface coatings; bulk ceramic materials can be prepared by high temperature sintering of powders.
Drawings
FIG. 1 shows the principle and apparatus for preparing Ti-B-N powder.
Wherein: 1. valves I, 2, II, 3, III, 4, IV, 5, 6, hydrogen, 7, nitrogen, 8, 9, 10, electric furnace, 11, Ti powder, 12, vacuum valve, 13, vacuum pump
Detailed Description
Example 1:
1, preparing Ti powder
Preparing Ti powder with granularity of-100 meshes and purity of more than 95%, charging the Ti powder into an electric furnace, and sealing the electric furnace to isolate the Ti powder from the outside air.
2, heating electric furnace
The compound synthesis temperature was set at 700 ℃ and the electric furnace was heated to 700 ℃.
3, introducing gas
When the vacuum degree in the furnace reaches 1x10-2Pa, N2 gas is introduced, and the flow rate is 100-150 l/h. When the temperature of the electric furnace reaches 700 ℃, H2 and BCl3 gases are introduced, and the proportion of N2 and H2 is 75 vol% to 25 vol%. The amount of BCl3 gas introduced was 5 vol% based on the sum of the above two gases. The temperature was maintained for 3 hours.
Step four, discharging
Closing each air inlet valve and vacuum valve, opening the furnace door after the furnace temperature is reduced to room temperature, taking out the synthesized powder product, wherein the chemical formula of the product is TiB0.04N0.96, and the average particle size is D5035 microns.
Example 2:
1, preparing Ti powder
Preparing Ti powder with granularity of-150 meshes and purity of over 98 percent, charging the Ti powder into an electric furnace, and sealing the electric furnace to isolate the Ti powder from the outside air.
2, heating electric furnace
The compound synthesis temperature was set at 860 ℃ and the electric furnace was heated to 860 ℃.
3, introducing gas
When the vacuum degree in the furnace reaches 1x10-2Pa, N2 gas is introduced, and the flow rate is 100-150 l/h. When the temperature of the electric furnace reaches 860 ℃, H2 and BCl3 gases are introduced, and the proportion of N2 and H2 is 60 vol% to 40 vol%. The amount of BCl3 gas introduced was 3 vol% based on the sum of the above two gases. The temperature was maintained for 3 hours.
Step four, discharging
Closing each air inlet valve and vacuum valve, opening the furnace door after the furnace temperature is reduced to room temperature, taking out the synthesized powder product, wherein the chemical formula of the product is TiB0.02N0.98, and the average particle size is D5038 microns.

Claims (3)

1. A titanium-boron-nitrogen compound powder production apparatus characterized by comprising: BCl3、H2And N2Three gas inlet valves, an electric furnace and a vacuum pump; the electric stove is vacuum electric heater, and the electric stove is sealed isolated with the outside air, is equipped with furnace gate, gas outlet and air inlet on it, and titanium powder is put in the electric stove, three kinds of gas admission valves are established on the admission line, include: boron trichloride gas control valve I, hydrogen control valve II, boron trichloride and hydrogen gas mixture control valve III and nitrogen gas control valve IV, boron trichloride gas and hydrogen mix through valve I and valve II respectively, then get into the electric stove through valve III, nitrogen gas passes through valve IV and gets into the electric stove, and waste gas is discharged from the gas outlet of electric stove, vacuum valve control vacuum in the electric stove, through the interior air of vacuum pump discharge stove, keep vacuum.
2. The method for preparing titanium-boron-nitrogen compound powder using the apparatus of claim 1, wherein the synthesized product, i.e., titanium-boron-nitrogen compound powder, is obtained by controlling the chemical reaction of the three gases with the precursor titanium powder, the synthesis process following the following chemical reaction equation:
2BCl3→2[B]+3Cl2
2BCl3+3H2→2[B]+6HCl
N2→2[N]
Ti+x[B]+y[N]→TiBxNy
x in the synthetic compound is 0.01-2.6; y is 0.1-0.99, wherein x and y represent the chemical composition of the elements B and N, respectively.
3. The method of producing a titanium-boron-nitrogen compound powder according to claim 2, wherein the synthesis of the titanium-boron-nitrogen compound powder is carried out by the steps of:
step one, preparing Ti powder
Preparing Ti powder with the granularity of-100 to-500 meshes and the purity of more than 95 percent, putting the Ti powder into an electric furnace, and sealing the electric furnace to isolate the electric furnace from the outside air;
step two, heating the electric furnace
Heating an electric furnace to a set temperature, wherein the temperature is set within the range of 700-1100 ℃, the specific temperature is determined according to the required particle size, and the higher the synthesis temperature is, the larger the powder particles are;
step three, introducing gas
When the vacuum degree in the furnace reaches 1x10-2Introducing N at Pa2The flow rate of the gas is 100-150 l/H, and H is introduced after the set temperature is reached2And BCl3Gas, N2And H2The proportion of the BCl is 50-75 vol% to 25-50 vol%, BCl3The gas is introduced in an amount which is 1-5 vol% of the total amount of the two gases, the heat is preserved for 2-5 hours, and when the amount of Ti powder is large, the heat preservation time is prolonged to 6-8 hours;
step four, discharging
After the time comes, H is closed2、BCl3A gas valve and an electric furnace power supply, and N is closed when the furnace temperature is reduced to 300-500 DEG C2A gas valve for maintaining the vacuum in the furnace not lower than 1x10 in the temperature reduction process-2And Pa, opening the furnace door when the temperature is reduced to the room temperature, and taking out the titanium-boron-nitrogen powder.
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US5851680A (en) * 1996-02-01 1998-12-22 Tecmachine Boron-doped titanium nitride coatings and coated parts
US6746952B2 (en) * 2001-08-29 2004-06-08 Micron Technology, Inc. Diffusion barrier layer for semiconductor wafer fabrication
CN101250716A (en) * 2008-03-31 2008-08-27 太原理工大学 Acid-fast anode
CN101358308A (en) * 2008-09-19 2009-02-04 山东大学 Aluminium-titan-carbon-boron-nitrogen intermediate alloy and preparation method thereof
CN101460649A (en) * 2006-06-02 2009-06-17 株式会社丰田中央研究所 Conductive corrosion-resistant material, and method for producing the same
CN102197162A (en) * 2008-10-30 2011-09-21 山特维克知识产权股份有限公司 A coated tool and a method of making thereof

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Publication number Priority date Publication date Assignee Title
US5851680A (en) * 1996-02-01 1998-12-22 Tecmachine Boron-doped titanium nitride coatings and coated parts
US6746952B2 (en) * 2001-08-29 2004-06-08 Micron Technology, Inc. Diffusion barrier layer for semiconductor wafer fabrication
CN101460649A (en) * 2006-06-02 2009-06-17 株式会社丰田中央研究所 Conductive corrosion-resistant material, and method for producing the same
CN101250716A (en) * 2008-03-31 2008-08-27 太原理工大学 Acid-fast anode
CN101358308A (en) * 2008-09-19 2009-02-04 山东大学 Aluminium-titan-carbon-boron-nitrogen intermediate alloy and preparation method thereof
CN102197162A (en) * 2008-10-30 2011-09-21 山特维克知识产权股份有限公司 A coated tool and a method of making thereof

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