CN109437132B - Production method of titanium nitride powder - Google Patents
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/076—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with titanium or zirconium or hafnium
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Abstract
A titanium nitride powder production method comprises the steps of putting a titanium-containing raw material into a crucible, introducing high-purity hydrogen into a hydrogenation reactor to carry out hydrogenation reaction to obtain titanium hydride, and carrying out ball milling and dehydrogenation reaction to obtain a titanium hydride material; after crushing, performing primary nitridation in a resistance furnace at 800-900 ℃ to obtain primary nitrided titanium nitride; after ball milling and crushing, performing secondary nitridation h in a resistance furnace at 1000-1200 ℃ to obtain secondarily nitrided titanium nitride; and (3) filling titanium nitride powder obtained by secondary nitridation into a ball milling tank for crushing to obtain titanium nitride powder. The advantages are that: the titanium sponge is used as a raw material, the raw material is easy to obtain, the nitrogen content of the titanium nitride product is high, the whole process is stable, and the titanium sponge is suitable for industrial production.
Description
Technical Field
The invention belongs to the field of metallurgy, and particularly relates to a production method of titanium nitride powder.
Background
The titanium nitride powder has excellent performances of high temperature resistance, corrosion resistance, wear resistance, thermal shock resistance, low density, high hardness and the like, and can be used for hard alloys, high-temperature ceramic conductive materials, heat-resistant wear-resistant materials, dispersion strengthening materials and the like. In addition, the material has good conductivity, can be used as a conductive material such as an electrode, an electrical contact and the like for molten salt electrolysis, is widely applied to the aerospace industry and other industrial fields, and has very wide application.
Research shows that the sintering performance of titanium nitride powder affects mechanical properties such as bending strength, fracture toughness and the like of a sintered body, while micron-sized titanium nitride has poor sintering performance, and the sintering temperature can be reduced and the sintering performance of titanium nitride can be improved by replacing the micron-sized titanium nitride with nano-sized titanium nitride.
At present, the method for preparing the nano titanium nitride powder takes titanium sponge as a raw material and nitrogen as a nitrogen source, and the titanium nitride powder is produced by a direct nitriding method. The method has high requirements on process conditions, the titanium sponge is not easy to be nitrided, the nitrogen content is low, and the product does not reach the standard.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for producing titanium nitride powder which has easily obtained raw materials, stable process and high nitrogen content and takes titanium sponge as the raw material.
The technical scheme of the invention is as follows:
a production method of titanium nitride powder comprises the following steps:
(1) loading titanium-containing raw materials into a crucible, loading the raw materials into a hydrogenation reactor together, vacuumizing, when the vacuum degree is less than or equal to 4Pa, transmitting power to heat, when the temperature reaches 550 ℃, closing a valve of a vacuum system, and introducing high-purity hydrogen to carry out hydrogenation reaction for 5-10 h to obtain titanium hydride;
(2) filling hydrogenated titanium hydride obtained by hydrogenation into a ball milling tank, adding a ball milling medium, and carrying out ball milling crushing by using a roller ball mill, wherein the ball milling revolution is 96 r/min, and the ball milling time is 2-6 h;
(3) charging crushed titanium hydride powder into a furnace according to the charging amount of 5 kg/furnace-8 kg/furnace, vacuumizing, and when the vacuum degree is less than or equal to 4Pa, performing dehydrogenation after gradient temperature rise, wherein the gradient temperature rise is that the temperature is respectively kept for 1h at 500 ℃, 600 ℃, 700 ℃ and 800 ℃, the temperature of dehydrogenation reaction is 800-900 ℃, the change of the vacuum degree in the furnace is monitored at any time, when the vacuum degree in the furnace is less than or equal to 4Pa, a heating power supply is closed, water is sprayed for cooling, and the temperature is reduced for 4-5 h, and then discharging is performed to obtain a dehydrogenated titanium material;
(4) loading the dehydrogenated titanium powder obtained by dehydrogenation into a ball milling tank, adding a ball milling medium, and carrying out ball milling and crushing by using a roller ball mill, wherein the ball milling revolution is 96 r/min, and the crushing time is 5-10 h;
(5) feeding the crushed dehydrotitanium powder into a resistance furnace, vacuumizing, when the vacuum degree is less than or equal to 4Pa, transmitting power, heating, when the temperature reaches 800 ℃, closing the vacuum, introducing nitrogen, and performing primary nitridation reaction for 5-10 h at 800-900 ℃ to obtain titanium nitride;
(6) filling the primarily nitrided titanium nitride powder into a ball milling tank, adding a ball milling medium, and carrying out ball milling crushing by using a roller ball mill with the ball milling revolution of 96 r/min for 10-20 h
(7) Loading the crushed titanium nitride powder into a resistance furnace, vacuumizing, when the vacuum degree is less than or equal to 4Pa, transmitting power to heat the titanium nitride powder, when the temperature reaches 1000 ℃, closing the vacuum, introducing nitrogen, and performing secondary nitridation reaction for 5-10 h at 1000-1200 ℃ to obtain titanium nitride;
(8) and (3) filling titanium nitride powder obtained by secondary nitridation into a ball milling tank, adding a ball milling medium, and carrying out ball milling and crushing by using a ball mill to obtain the titanium nitride powder.
Furthermore, the titanium-containing raw material is sponge titanium, and the purity of the sponge titanium is more than or equal to 99%.
Further, in the steps (2), (4), (6) and (8), the ball milling medium has the size ratio of
Furthermore, the model of the ball milling tank in the step (2) is phi 500 multiplied by 700mm, the ball milling medium is agate balls, the addition amount of the agate balls is 7.0 kg-8.0 kg, and the amount of titanium hydride material filled in each tank is 10 kg-16 kg.
Furthermore, the type of the ball milling tank in the step (4) is phi 500 multiplied by 700mm, the ball milling medium is agate balls, the addition amount of the agate balls is 7.0-8.0 kg, and the amount of the titanium hydride material filled in each tank is 5.0-8.0 kg.
Further, the introduction flow rate of hydrogen in the step (1) is 1Nm3/h～2Nm3/h。
Further, the flow rate of nitrogen introduced in the step (5) and the step (7) was 1Nm3/h～2Nm3/h。
Further, the fineness of the titanium nitride powder in the step (8) is 200 meshes.
The invention has the beneficial effects that:
the titanium sponge is used as a raw material, the raw material is easy to obtain, hydrogenation reaction is firstly carried out, after dehydrogenation treatment, nitridation reaction is carried out twice, the nitrogen content of the titanium nitride product is high, no other impurities are introduced, the nitrogen content in the titanium nitride powder is more than 19%, the whole process is stable, and the titanium nitride powder is suitable for industrial production.
Detailed Description
The specific technical solution of the present invention will be described with reference to the following embodiments, which are merely illustrative of the effective implementation of the technical solution of the present invention, but the technical solution of the present invention is not limited to the following embodiments.
Example 1
(1) Loading 10kg of sponge titanium with the purity of 99.5 percent into a crucible, loading the sponge titanium into a hydrogenation reactor together, vacuumizing, when the vacuum degree is less than or equal to 4Pa, transmitting power to heat, when the temperature reaches 550 ℃, closing a valve of a vacuum system, introducing high-purity hydrogen, wherein the introduction flow rate of the hydrogen is 1Nm3Performing hydrogenation reaction for 5 hours to obtain titanium hydride;
(2) loading the hydrogenated material into a ball milling tank, adding agate balls, wherein the model of the ball milling tank is phi 500 multiplied by 700mm, and the size ratio of the agate balls is
7.0kg of agate balls are added, the amount of titanium hydride material in each can is 10kg, and the materials are ball-milled and crushed by a roller-bar ball mill, the ball-milling revolution is 96 r/min, and the ball-milling time is 2 h;
(3) charging the crushed titanium hydride powder into a furnace according to the charging amount of 5 kg/furnace, vacuumizing, and dehydrogenating after gradient temperature rise when the vacuum degree is less than or equal to 4Pa, wherein the gradient temperature rise is that the temperature is respectively kept for 1h at 500 ℃, 600 ℃, 700 ℃ and 800 ℃, the dehydrogenation reaction temperature is 800 ℃, the change of the vacuum degree in the furnace is monitored at any time, when the vacuum degree in the furnace is less than or equal to 4Pa, a heating power supply is closed, water is sprayed for cooling, and the temperature is reduced for 4h, and then the titanium hydride powder is discharged out of the furnace to obtain a titanium hydride material;
(4) placing the dehydrogenated titanium powder obtained by dehydrogenation into a ball-milling tank, adding agate balls, wherein the model of the ball-milling tank is phi 500 multiplied by 700mm, and the size ratio of the agate balls is
7.0 of agate ball, 5.0kg of dehydrotitanium material per can, and performing ball milling and crushing by using a roller-bar ball mill, wherein the ball milling revolution is 96 r/min, and the crushing time is 5 hours;
(5) charging the crushed dehydrotitanium powder into a resistance furnace, vacuumizing, feeding power and heating when the vacuum degree is less than or equal to 4Pa,when the temperature reaches 800 ℃, the vacuum is closed, nitrogen is introduced, and the flow rate of the nitrogen is 1Nm3Performing primary nitridation reaction for 10 hours at 800 ℃ to obtain titanium nitride;
(6) filling the titanium nitride powder subjected to primary nitridation into a ball milling tank, and adding agate balls with the size ratio of the agate balls
Performing ball milling crushing by using a roller ball mill, wherein the ball milling revolution is 96 r/min, and the ball milling lasts for 10 hours;
(7) charging the crushed titanium nitride powder into a resistance furnace, vacuumizing, when the vacuum degree is less than or equal to 4Pa, transmitting power, heating, when the temperature reaches 1000 ℃, closing the vacuum, introducing nitrogen gas with the flow rate of 1Nm3Performing secondary nitridation reaction for 510 hours at 1000 ℃ to obtain titanium nitride;
(8) titanium nitride powder obtained by secondary nitridation is filled into a ball milling tank, and agate balls with the size ratio of
And ball-milling and crushing by using a roller bar type ball mill, and sieving by using a standard sieve of 200 meshes to obtain the titanium nitride powder with the nitrogen content of 19.16 percent.
Example 2
(1) Loading 12kg of sponge titanium with the purity of 99.5 percent into a crucible, loading the crucible and the sponge titanium into a hydrogenation reactor together, vacuumizing, when the vacuum degree is less than or equal to 4Pa, transmitting power to heat, when the temperature reaches 550 ℃, closing a valve of a vacuum system, introducing high-purity hydrogen, wherein the introduction flow of the hydrogen is 1.5Nm3Performing hydrogenation reaction for 8 hours to obtain titanium hydride;
(2) loading hydrogenated titanium into a ball milling tank, adding agate balls, wherein the ball milling tank is phi 500 mm by 700mm, and the agate balls have the size ratio of
7.5kg of agate balls are added, the amount of titanium hydride material in each can is 12kg, and the materials are ball-milled and crushed by a roller-bar ball mill, the ball-milling revolution is 96 r/min, and the ball-milling time is 4 hours;
(3) loading the crushed titanium hydride powder into a furnace according to the charging amount of 6 kg/furnace, vacuumizing, and dehydrogenating after gradient temperature rise when the vacuum degree is less than or equal to 4Pa, wherein the gradient temperature rise is that the temperature is respectively kept at 500 ℃, 600 ℃, 700 ℃ and 800 ℃ for 1h, the dehydrogenation reaction temperature is 850 ℃, the change of the vacuum degree in the furnace is monitored at any time, when the vacuum degree in the furnace is less than or equal to 4Pa, a heating power supply is closed, water is sprayed for cooling, and the temperature is reduced for 4.5h, and then the titanium hydride powder is discharged from the furnace to obtain a titanium hydride material;
(4) placing the dehydrogenated titanium powder obtained by dehydrogenation into a ball-milling tank, adding agate balls, wherein the model of the ball-milling tank is phi 500 multiplied by 700mm, and the size ratio of the agate balls is
7.5kg of agate balls are added, the amount of the dehydrotitanium material in each can is 6kg, and the ball milling and crushing are carried out by a roller ball mill, wherein the ball milling revolution is 96 r/min, and the crushing time is 8 h;
(5) charging the crushed dehydrotitanium powder into a resistance furnace, vacuumizing, when the vacuum degree is less than or equal to 4Pa, transmitting power, heating, when the temperature reaches 800 ℃, closing the vacuum, introducing nitrogen gas with the flow rate of 1.5Nm3Performing primary nitridation reaction for 8 hours at 850 ℃ to obtain titanium nitride;
(6) filling the titanium nitride powder subjected to primary nitridation into a ball milling tank, and adding agate balls with the size ratio of the agate balls
Ball milling and crushing by using a roller ball mill, wherein the ball milling revolution is 96 r/min, and the ball milling lasts for 15 hours
(7) Charging the crushed titanium nitride powder into a resistance furnace, vacuumizing, when the vacuum degree is less than or equal to 4Pa, transmitting power to heat, and when the temperature reaches 1000 ℃, closing the vacuumIntroducing nitrogen at a flow rate of 1.5Nm3Performing secondary nitridation reaction for 8 hours at 1100 ℃ to obtain titanium nitride;
(8) titanium nitride powder obtained by secondary nitridation is filled into a ball milling tank, and agate balls with the size ratio of
And ball-milling and crushing by using a ball mill, and sieving by using a standard sieve of 200 meshes to obtain the titanium nitride powder with the nitrogen content of 19.21 percent.
Example 3
(1) Loading 16kg of sponge titanium with the purity of 99.5 percent into a crucible, loading the sponge titanium into a hydrogenation reactor together, vacuumizing, when the vacuum degree is less than or equal to 4Pa, transmitting power, heating, when the temperature reaches 550 ℃, closing a valve of a vacuum system, introducing high-purity hydrogen, wherein the introduction flow of the hydrogen is 2Nm3Performing hydrogenation reaction for 10 hours to obtain titanium hydride;
(2) loading hydrogenated titanium into a ball milling tank, adding agate balls, wherein the ball milling tank is phi 500 mm by 700mm, and the agate balls have the size ratio of
The adding amount of agate balls is 8.0kg, the amount of titanium hydride material filled in each tank is 16kg, and the ball milling and crushing are carried out by a roller-bar ball mill, the ball milling revolution is 96 r/min, and the ball milling time is 6 h;
(3) loading the crushed titanium hydride powder into a furnace according to the charging amount of 8 kg/furnace, vacuumizing, and dehydrogenating after gradient temperature rise when the vacuum degree is less than or equal to 4Pa, wherein the gradient temperature rise is that the temperature is respectively kept at 500 ℃, 600 ℃, 700 ℃ and 800 ℃ for 1h, the dehydrogenation reaction temperature is 900 ℃, the change of the vacuum degree in the furnace is monitored at any time, when the vacuum degree in the furnace is less than or equal to 4Pa, a heating power supply is closed, water is sprayed for cooling, and the temperature is reduced for 5h and then discharged to obtain a dehydrogenated titanium material;
(4) placing the dehydrogenated titanium powder obtained by dehydrogenation into a ball-milling tank, adding agate balls, wherein the model of the ball-milling tank is phi 500 multiplied by 700mm, and the size ratio of the agate balls isIs composed of
8.0kg of agate balls are added, the amount of the titanium hydride material in each can is 8.0kg, and the ball milling and crushing are carried out by a roller-bar ball mill, the ball milling revolution is 96 r/min, and the crushing time is 10 h;
(5) charging the crushed dehydrotitanium powder into a resistance furnace, vacuumizing, when the vacuum degree is less than or equal to 4Pa, transmitting power, heating, when the temperature reaches 800 ℃, closing the vacuum, introducing nitrogen gas with the flow rate of 2Nm3Performing primary nitridation reaction for 5 hours at 900 ℃ to obtain titanium nitride;
(6) filling the titanium nitride powder subjected to primary nitridation into a ball milling tank, and adding agate balls with the size ratio of the agate balls
Ball milling and crushing by using a roller ball mill, wherein the ball milling revolution is 96 r/min, and the ball milling lasts for 20 hours
(7) Charging the crushed titanium nitride powder into a resistance furnace, vacuumizing, when the vacuum degree is less than or equal to 4Pa, transmitting power, heating, when the temperature reaches 1000 ℃, closing the vacuum, introducing nitrogen gas with the flow rate of 2Nm3Performing secondary nitridation reaction for 5 hours at 1200 ℃ to obtain titanium nitride;
(8) titanium nitride powder obtained by secondary nitridation is filled into a ball milling tank, and agate balls with the size ratio of
And ball-milling and crushing by using a ball mill, and sieving by using a standard sieve of 200 meshes to obtain the titanium nitride powder with the nitrogen content of 19.25 percent.
The above description is only exemplary of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A production method of titanium nitride powder is characterized by comprising the following steps: the method comprises the following steps:
(1) loading titanium-containing raw materials into a crucible, loading the raw materials into a hydrogenation reactor together, vacuumizing, when the vacuum degree is less than or equal to 4Pa, transmitting power to heat, when the temperature reaches 550 ℃, closing a valve of a vacuum system, and introducing high-purity hydrogen to carry out hydrogenation reaction for 5-10 h to obtain titanium hydride;
(2) filling hydrogenated titanium hydride obtained by hydrogenation into a ball milling tank, adding a ball milling medium, and carrying out ball milling crushing by using a ball mill, wherein the ball milling revolution is 96 r/min, and the ball milling time is 2-6 h;
(3) charging crushed titanium hydride powder into a furnace according to the charging amount of 5 kg/furnace-8 kg/furnace, vacuumizing, and when the vacuum degree is less than 4Pa, performing gradient temperature rise and then performing dehydrogenation, wherein the gradient temperature rise is that the temperature is respectively kept for 1h at 500 ℃, 600 ℃, 700 ℃ and 800 ℃, the temperature of dehydrogenation reaction is 800-900 ℃, the change of the vacuum degree in the furnace is monitored at any time, when the vacuum degree in the furnace is 4Pa, a heating power supply is closed, water is sprayed for cooling, and the temperature is reduced for 4-5 h and then discharged, so that the titanium hydride powder is obtained;
(4) loading the dehydrogenated titanium powder obtained by dehydrogenation into a ball milling tank, adding a ball milling medium, and carrying out ball milling and crushing by using a ball mill, wherein the ball milling revolution is 96 revolutions per minute, and the crushing time is 5-10 hours;
(5) loading the crushed dehydrotitanium powder into a resistance furnace, vacuumizing, when the vacuum degree is less than or equal to 4Pa, transmitting power to heat the dehydrotitanium powder, when the temperature reaches 800 ℃, closing the vacuum, introducing nitrogen, and performing primary nitridation reaction at 800-900 ℃ for 5-10 h to obtain primary nitrided titanium nitride powder;
(6) filling the primarily nitrided titanium nitride powder into a ball milling tank, adding a ball milling medium, and carrying out ball milling crushing by using a ball mill, wherein the ball milling revolution is 96 r/min, and the ball milling lasts for 10-20 h
(7) Loading the crushed titanium nitride powder into a resistance furnace, vacuumizing, when the vacuum degree is less than or equal to 4Pa, transmitting power to heat the titanium nitride powder, when the temperature reaches 1000 ℃, closing the vacuum, introducing nitrogen, and performing secondary nitridation reaction for 5-10 h at 1000-1200 ℃ to obtain secondary nitrided titanium nitride powder;
(8) and (3) filling titanium nitride powder obtained by secondary nitridation into a ball milling tank, adding a ball milling medium, and carrying out ball milling and crushing by using a ball mill to obtain the titanium nitride powder.
2. The method for producing titanium nitride powder according to claim 1, wherein: the titanium-containing raw material is sponge titanium, and the purity of the sponge titanium is more than or equal to 99%.
3. The method for producing titanium nitride powder according to claim 1, wherein: in the steps (2), (4), (6) and (8), the ball milling medium has the size ratio of
4. The method for producing titanium nitride powder according to claim 1, wherein: the ball milling tank in the step (2) has the model diameter of 500 x 700mm, the ball milling medium is agate balls, the addition amount of the agate balls is 7.0 kg-8.0 kg, and the amount of titanium hydride material filled in each tank is 10 kg-16 kg.
5. The method for producing titanium nitride powder according to claim 1, wherein: the ball milling tank in the step (4) has the model diameter of 500 x 700mm, the ball milling medium is agate balls, the addition amount of the agate balls is 7.0-8.0 kg, and the amount of the dehydrotitanium material filled in each tank is 5.0-8.0 kg.
6. The method for producing titanium nitride powder according to claim 1, wherein: the introduction flow rate of hydrogen in the step (1) is 1Nm3/h～2Nm3/h。
7. The method for producing titanium nitride powder according to claim 1, wherein: the flow rate of nitrogen introduced in the step (5) and the step (7) is 1Nm3/h～2Nm3/h。
8. The method for producing titanium nitride powder according to claim 1, wherein: the fineness of the titanium nitride powder subjected to ball milling in the step (8) is 200 meshes.
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| CN113387337A (en) * | 2021-05-25 | 2021-09-14 | 宝鸡泉兴钛业股份有限公司 | Equipment and process method for preparing high-titanium-nitride powder by titanium powder nitriding method |
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| KR950013068B1 (en) * | 1992-08-26 | 1995-10-24 | 김용택 | Process for the preparation of titanium nitride powders |
| JP5257381B2 (en) * | 2010-03-05 | 2013-08-07 | 住友金属鉱山株式会社 | Near-infrared shielding polyester resin composition, molded article thereof, and laminate thereof |
| CN104511595B (en) * | 2014-12-30 | 2016-08-24 | 中南大学 | A kind of preparation method of high-purity titanium valve |
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