CN110921639A - Preparation method of nano titanium carbonitride powder - Google Patents
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Abstract
The invention belongs to the field of metal ceramic powder, and particularly relates to a preparation method of nano titanium carbonitride powder. The method mainly comprises the following steps: (1) ball-milling titanium powder and graphite powder in an absolute ethyl alcohol environment by using a ball milling method to obtain uniformly mixed powder; (2) drying and taking out the powder obtained by ball milling to obtain a dry mixture; (3) putting the dried mixture into a self-propagating equipment reaction kettle, vacuumizing and introducing nitrogen; (4) igniting the mixture by utilizing high-pressure ignition of a tungsten wire and carrying out self-propagating reaction to obtain titanium carbonitride; (5) and ball-milling the titanium carbonitride generated by the reaction in an absolute ethyl alcohol environment by using a ball milling method and drying to finally obtain the high-purity titanium carbonitride nano powder. The method for preparing the titanium carbonitride has the advantages of simple process, high yield, low cost and high product purity.
Description
Technical Field
The invention belongs to the field of metal ceramic powder, and particularly relates to a preparation method of nano titanium carbonitride powder.
Background
WC-Co series hard alloy has high strength and good toughness, is widely used in modern manufacturing industry, but has slightly insufficient hardness and wear resistance, and is limited in certain applications. The titanium carbonitride-based cermet material has high hardness, high red hardness and high wear resistance, so that it may be used to replace WC-Co hard alloy. However, in order to prepare a titanium carbonitride cermet material having excellent overall properties, it is necessary to prepare a titanium carbonitride ceramic powder having high purity, fine particle size and stable sintering properties.
Titanium Carbonitride (TC)1-xNxX is more than or equal to 0 and less than or equal to 1) has excellent performances of high melting point, large hardness, good chemical stability and thermal stability and the like, has beautiful golden color, is used as a superhard material, a steelmaking additive, device surface decoration, an anti-corrosion and anti-wear material and the like, and has wide application. According to the different contents of carbon and nitrogen in titanium carbonitride, the material shows different hardness and toughness, when the content of nitrogen is high, the toughness is better, and when the content of carbon is high, the hardness is higher.
The preparation method of the titanium carbonitride powder comprises a carbothermal nitridation reduction method, a chemical vapor deposition method, a mechanical alloying method and a chemical synthesis method. The carbothermic nitridation reduction method has low cost, can be used for large-scale production, and has great advantages compared with other methods. The traditional carbothermal nitridation reduction method for synthesizing titanium carbonitride powder usually takes titanium dioxide and carbon black as raw materials, ball-milling and mixing the raw materials, and then carrying out carbothermal nitridation reduction reaction at high temperature. For example, chinese patent application CN108424147A discloses a method for producing titanium carbonitride and titanium nitride powder by rapid nitridation, which uses traditional titanium dioxide and carbon black raw materials, and high-energy ball milling and mixing, spray granulation and drying of slurry, and powder preparation by rapid nitridation device. The method realizes the mixing of the carbon and the titanium by a physical method, and the raw materials are difficult to be uniformly mixed due to the difference of the proportion and the polarity of the raw materials, so that incomplete reaction is easily caused.
Disclosure of Invention
The invention aims to overcome the defects of the existing method for preparing high-purity and high-crystallinity titanium carbonitride, and provides a method for preparing nano titanium carbonitride powder by a high-temperature self-propagating method.
The invention also protects the titanium carbonitride powder prepared according to the method and the application of the prepared titanium carbonitride powder to the preparation of titanium carbonitride-based ceramic materials which are widely applied to the machining field, such as cutting tool materials.
A method for preparing nano titanium carbonitride powder comprises the following steps:
(1) mixing materials: the mixing of a planetary ball mill is used, titanium powder and graphite powder are put into a ball milling tank, WC balls with the diameters of 10mm, 6mm and 8mm are matched for ball milling, and the proportion of the WC alloy balls adopted in the experiment is as follows: 10mm 14, 8mm 50 and 6mm 50, wherein the mass ratio of the WC balls to the alloy powder, namely the ball-material ratio, is 20:1, the rotating speed is 400r/min, the ball milling time is 9h, the ball mill operates in a forward rotation mode for 20min, a pause mode for 20min and a reverse rotation mode for 20min, and the circulation is carried out. Wet milling is carried out by taking absolute ethyl alcohol as a ball milling medium, and a ball milling tank is vacuumized and is filled with argon gas to prevent powder oxidation.
(2) And (3) drying: and (3) drying the wet material subjected to ball milling in a vacuum drying oven for 9 hours at the drying temperature of 60 ℃, grinding the dried powder, and then sieving, wherein a 200-mesh sieve is selected as the sieve.
(3) Self-propagating: uniformly placing the dried powder in a graphite tank, winding a tungsten wire with the diameter of 0.5mm into a coil with the diameter of 5mm, embedding the coil into the surface layer of the powder, fixing the graphite tank in a self-propagating reaction kettle, vacuumizing the self-propagating reaction kettle, introducing nitrogen into the self-propagating reaction kettle until the pressure in the kettle is 9MPa, igniting at high pressure, igniting the surface layer powder, carrying out self-propagating reaction until the reaction is completely finished, observing the temperature of a control console of the self-propagating instrument and a pressure display meter, rapidly increasing the temperature in the kettle to 2300 ℃ within 1 second when the reaction starts, instantly reaching 10MPa in the kettle, slowly decreasing the temperature and the pressure, reducing the pressure to below 7MPa after 10-15 minutes, completing the reaction after the temperature is reduced to room temperature, opening the reaction kettle, taking out a blocky sample obtained by the reaction, and obtaining a newly generated substance which is high-purity titanium carbonitride.
(4) Ball milling: the generated titanium carbonitride is crushed and ball-milled by a ball mill, WC balls with the diameters of 10mm, 6mm and 8mm are matched for ball milling, and the proportion of the WC alloy balls adopted in the experiment is as follows: 10mm 14, 8mm 50 and 6mm 50, wherein the mass ratio of the WC balls to the alloy powder, namely the ball-material ratio, is 20:1, the rotating speed is 400r/min, the ball milling time is 12h, the ball mill operates in a forward rotation mode for 20min, a pause mode for 20min and a reverse rotation mode for 20min, and the circulation is carried out. Wet milling is carried out by taking absolute ethyl alcohol as a ball milling medium, and a ball milling tank is vacuumized and is filled with argon gas to prevent powder oxidation.
(5) And (3) drying: and (3) drying the ball-milled titanium carbonitride powder in a vacuum drying oven for 12h at the drying temperature of 60 ℃, grinding and sieving the dried powder, and selecting a 200-mesh sieve for the sieve to obtain the high-purity and high-crystallinity nano titanium carbonitride powder.
In the step (1), the molar ratio of the titanium powder to the graphite powder is 10:3, 10:5 or 10: 7; the ball milling balls are WC hard alloy balls with the diameters of 10mm, 6mm and 8mm, and the ball material ratio is 20: 1; the rotating speed is 400r/min, the ball milling time is 9h, and the ball milling mode is wet milling by taking absolute ethyl alcohol as a medium.
And (3) in the drying step (2), a vacuum drying oven is selected, the drying time is 9 hours, and the drying temperature is 60 ℃.
In the step (3), the vertical self-propagating autoclave SHS3-20/200 of Dalianke metallocene equipment Limited company is selected for the self-propagating reaction; a tungsten wire with the diameter of 0.5mm is wound into a coil with the diameter of 5mm and is buried in the surface layer of the powder for ignition; introducing nitrogen into the reaction kettle until the pressure in the kettle reaches 9Mpa, wherein the reaction process needs to be in a sealed state; high-voltage ignition is adopted, and the ignition current is 30A.
In the ball milling process in the step (4), WC balls with the diameters of 10mm, 6mm and 8mm are matched for ball milling, the ball-material ratio is 20:1, the rotating speed is 400r/min, and the ball milling time is 12 h.
In the drying step (5), a vacuum drying oven is selected for the drying step, the drying time is 12 hours, and the drying temperature is 60 ℃.
The purity of the product prepared by the method is more than 99%, the crystallinity is high, the particle size of the product is 200-300 nm, and the preparation cost is low.
Drawings
Fig. 1 is a scanning electron microscope picture of the prepared titanium carbonitride nanoparticles.
Fig. 2 is an X-ray diffraction pattern of the prepared titanium carbonitride nanoparticles.
Detailed Description
Example 1:
(1) mixing materials: mixing materials by using a planetary ball mill, putting 18.6g of titanium powder and 1.4g of graphite powder into a ball milling tank, and performing ball milling by matching WC balls with the diameters of 10mm, 6mm and 8mm respectively, wherein the ball-material ratio is 20:1, namely the mass of the balls is 400g in total, the rotating speed is 400r/min, the ball milling time is 9h, the ball mill is operated in a forward rotation mode for 20min, a pause mode for 20min and a reverse rotation mode for 20min, and the steps are repeated. Wet milling is carried out by taking absolute ethyl alcohol as a ball milling medium, and a ball milling tank is vacuumized and is filled with argon gas to prevent powder oxidation.
(2) And (3) drying: and (3) drying the wet material subjected to ball milling in a vacuum drying oven for 9 hours at the drying temperature of 60 ℃, grinding the dried powder, and then sieving, wherein a 200-mesh sieve is selected as the sieve.
(3) Self-propagating: uniformly placing the dried powder in a graphite tank, winding a tungsten wire with the diameter of 0.5mm into a coil with the diameter of 5mm, embedding the coil into the surface layer of the powder, fixing the graphite tank in a self-propagating reaction kettle, vacuumizing the self-propagating reaction kettle, introducing nitrogen into the self-propagating reaction kettle until the pressure in the kettle is 9Mpa, igniting at high pressure, igniting the surface layer powder, and then performing self-propagating reaction until the reaction is completely finished, wherein the newly generated substance is high-purity titanium carbonitride.
(4) Ball milling: and (2) crushing titanium carbonitride, ball-milling by using a ball mill, performing ball-milling by matching WC balls with the diameters of 10mm, 6mm and 8mm respectively, wherein the ball-material ratio is 20:1, the rotating speed is 400r/min, the ball-milling time is 12h, the ball mill operates in a forward rotation mode for 20min, a pause mode for 20min and a reverse rotation mode for 20min, and the steps are repeated. Wet milling is carried out by taking absolute ethyl alcohol as a ball milling medium, and a ball milling tank is vacuumized and is filled with argon gas to prevent powder oxidation.
(5) And (3) drying: and (3) drying the ball-milled titanium carbonitride powder in a vacuum drying oven for 12h at the drying temperature of 60 ℃, grinding and sieving the dried powder, and selecting a 200-mesh sieve for the sieve to obtain the high-purity and high-crystallinity nano titanium carbonitride powder.
Example 2:
(1) mixing materials: mixing materials by using a planetary ball mill, putting 17.77g of titanium powder and 2.23g of graphite powder into a ball milling tank, and performing ball milling by matching WC balls with the diameters of 10mm, 6mm and 8mm respectively, wherein the ball-material ratio is 20:1, namely the mass of the balls is 400g in total, the rotating speed is 400r/min, the ball milling time is 9h, the ball mill is operated in a forward rotation mode for 20min, a pause mode for 20min and a reverse rotation mode for 20min, and the steps are repeated. Wet milling is carried out by taking absolute ethyl alcohol as a ball milling medium, and a ball milling tank is vacuumized and is filled with argon gas to prevent powder oxidation.
(2) And (3) drying: and (3) drying the wet material subjected to ball milling in a vacuum drying oven for 9 hours at the drying temperature of 60 ℃, grinding the dried powder, and then sieving, wherein a 200-mesh sieve is selected as the sieve.
(3) Self-propagating: uniformly placing the dried powder in a graphite tank, winding a tungsten wire with the diameter of 0.5mm into a coil with the diameter of 5mm, embedding the coil into the surface layer of the powder, fixing the graphite tank in a self-propagating reaction kettle, vacuumizing the self-propagating reaction kettle, introducing nitrogen into the self-propagating reaction kettle until the pressure in the kettle is 9Mpa, igniting at high pressure, igniting the surface layer powder, and then performing self-propagating reaction until the reaction is completely finished, wherein the newly generated substance is high-purity titanium carbonitride.
(4) Ball milling: and (2) crushing titanium carbonitride, ball-milling by using a ball mill, performing ball-milling by matching WC balls with the diameters of 10mm, 6mm and 8mm respectively, wherein the ball-material ratio is 20:1, the rotating speed is 400r/min, the ball-milling time is 12h, the ball mill operates in a forward rotation mode for 20min, a pause mode for 20min and a reverse rotation mode for 20min, and the steps are repeated. Wet milling is carried out by taking absolute ethyl alcohol as a ball milling medium, and a ball milling tank is vacuumized and is filled with argon gas to prevent powder oxidation.
(5) And (3) drying: and (3) drying the ball-milled titanium carbonitride powder in a vacuum drying oven for 12h at the drying temperature of 60 ℃, grinding and sieving the dried powder, and selecting a 200-mesh sieve for the sieve to obtain the high-purity and high-crystallinity nano titanium carbonitride powder.
Example 3:
(1) mixing materials: mixing materials by using a planetary ball mill, putting 17.01g of titanium powder and 2.99g of graphite powder into a ball milling tank, and performing ball milling by matching WC balls with the diameters of 10mm, 6mm and 8mm respectively, wherein the ball-material ratio is 20:1, namely the mass of the balls is 400g in total, the rotating speed is 400r/min, the ball milling time is 9h, the ball mill is operated in a forward rotation mode for 20min, a pause mode for 20min and a reverse rotation mode for 20min, and the steps are repeated. Wet milling is carried out by taking absolute ethyl alcohol as a ball milling medium, and a ball milling tank is vacuumized and is filled with argon gas to prevent powder oxidation.
(2) And (3) drying: and (3) drying the wet material subjected to ball milling in a vacuum drying oven for 9 hours at the drying temperature of 60 ℃, grinding the dried powder, and then sieving, wherein a 200-mesh sieve is selected as the sieve.
(3) Self-propagating: uniformly placing the dried powder in a graphite tank, winding a tungsten wire with the diameter of 0.5mm into a coil with the diameter of 5mm, embedding the coil into the surface layer of the powder, fixing the graphite tank in a self-propagating reaction kettle, vacuumizing the self-propagating reaction kettle, introducing nitrogen into the self-propagating reaction kettle until the pressure in the kettle is 9Mpa, igniting at high pressure, igniting the surface layer powder, and then performing self-propagating reaction until the reaction is completely finished, wherein the newly generated substance is high-purity titanium carbonitride.
(4) Ball milling: and (2) crushing titanium carbonitride, ball-milling by using a ball mill, performing ball-milling by matching WC balls with the diameters of 10mm, 6mm and 8mm respectively, wherein the ball-material ratio is 20:1, the rotating speed is 400r/min, the ball-milling time is 12h, the ball mill operates in a forward rotation mode for 20min, a pause mode for 20min and a reverse rotation mode for 20min, and the steps are repeated. Wet milling is carried out by taking absolute ethyl alcohol as a ball milling medium, and a ball milling tank is vacuumized and is filled with argon gas to prevent powder oxidation.
(5) And (3) drying: and (3) drying the ball-milled titanium carbonitride powder in a vacuum drying oven for 12h at the drying temperature of 60 ℃, grinding and sieving the dried powder, and selecting a 200-mesh sieve for the sieve to obtain the high-purity and high-crystallinity nano titanium carbonitride powder.
As can be seen from the SEM of FIG. 1, the TiC is produced0.7N0.3The particle size of the powder is between 0.2 μm and 0.3. mu.m.
As can be seen from the X-ray diffraction pattern of the attached figure 2, the TiC is prepared0.7N0.3The main peak of the powder is clear and has no impurity peak, and the sample is known to have high crystallinity and high purity.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (7)
1. A preparation method of nano titanium carbonitride powder is characterized by comprising the following steps:
(1) mixing materials: mixing materials by using a planetary ball mill, putting titanium powder and graphite powder into a ball milling tank, carrying out wet milling by using absolute ethyl alcohol as a ball milling medium, vacuumizing the ball milling tank, and introducing argon to prevent the powder from being oxidized;
(2) and (3) drying: putting the wet material subjected to ball milling into a vacuum drying oven for drying, grinding the dried powder and then sieving;
(3) self-propagating: uniformly placing the dried and sieved powder in a graphite tank, embedding a coil made by winding a tungsten wire into the surface layer of the powder, fixing the graphite tank in a self-propagating reaction kettle, vacuumizing the self-propagating reaction kettle, introducing nitrogen into the self-propagating reaction kettle until the pressure in the kettle is 9Mpa, igniting at high pressure, igniting the powder on the surface layer, and then carrying out self-propagating reaction until the reaction is completely finished to obtain a newly generated substance, namely titanium carbonitride;
(4) ball milling: crushing the generated titanium carbonitride, ball-milling the titanium carbonitride by using a ball mill, wet-milling the titanium carbonitride by using absolute ethyl alcohol as a ball-milling medium, vacuumizing a ball-milling tank, and introducing argon to prevent powder from being oxidized;
(5) and (3) drying: and (3) putting the ball-milled titanium carbonitride powder into a vacuum drying oven for drying and sieving to obtain the high-purity and high-crystallinity nano titanium carbonitride powder.
2. The method for preparing nano titanium carbonitride powder according to claim 1 characterized in that the ratio of the titanium powder to the graphite powder in the step (1) is 10:3, 10:5 or 10:7 in molar ratio; the adopted WC alloy balls are prepared in the following proportion: 10mm 14, 8mm 50 and 6mm 50, wherein the mass ratio of the WC alloy balls to the alloy powder, namely the ball-material ratio, is 20:1, the rotating speed is 400r/min, the ball milling time is 9h, the ball mill operates in a forward rotation mode for 20min, a pause mode for 20min and a reverse rotation mode for 20min, and the circulation is carried out.
3. The method of claim 1, wherein in the step (2), the drying time is 9 hours, the drying temperature is 60 ℃, and a 200-mesh screen is selected for the screen.
4. The method for preparing nano titanium carbonitride powder according to claim 1 characterized in that in the step (3), the self-propagating reaction is performed by using a vertical self-propagating autoclave SHS3-20/200 of Daliankomao equipment Co., Ltd; a tungsten wire with the diameter of 0.5mm is wound into a coil with the diameter of 5mm and is buried in the surface layer of the powder for ignition; the reaction process needs to be in a sealed state; high-voltage ignition is adopted, and the ignition current is 30A.
5. The method of claim 1, wherein in the step (3), the temperature of the reaction vessel is rapidly increased to 2300 ℃ within 1 second by observing the temperature and pressure indicator of the control console of the self-propagating apparatus, the pressure in the reaction vessel is instantaneously increased to 10Mpa, the temperature and pressure are then slowly decreased, and the pressure is decreased to 7Mpa or less after 10-15 minutes, and the reaction is completed when the temperature is decreased to room temperature.
6. The method for preparing nano titanium carbonitride powder according to claim 1, wherein in the step (4), WC alloy balls with diameters of 10mm, 6mm and 8mm are matched for ball milling, and the proportion of the WC alloy balls is as follows: 10mm 14, 8mm 50 and 6mm 50, wherein the mass ratio of the WC balls to the alloy powder, namely the ball-material ratio, is 20:1, the rotating speed is 400r/min, the ball milling time is 12h, the ball mill operates in a forward rotation mode for 20min, a pause mode for 20min and a reverse rotation mode for 20min, and the circulation is carried out.
7. The method for preparing nano titanium carbonitride powder according to claim 1 wherein in the step (5), the drying time is 12 hours, the drying temperature is 60 ℃, and a 200-mesh screen is selected for the screen.
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| CN112010308A (en) * | 2020-08-26 | 2020-12-01 | 盐城工学院 | Preparation method of surface modified carbon titanium sulfide battery negative electrode material |
| CN115196606A (en) * | 2022-07-29 | 2022-10-18 | 株洲托普硬质合金材料有限公司 | Preparation method and equipment of high-performance titanium carbonitride |
| CN115448727A (en) * | 2022-09-13 | 2022-12-09 | 苏州科技大学 | Preparation method of spherical titanium carbonitride ceramic powder |
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| CN112010308A (en) * | 2020-08-26 | 2020-12-01 | 盐城工学院 | Preparation method of surface modified carbon titanium sulfide battery negative electrode material |
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| CN115448727A (en) * | 2022-09-13 | 2022-12-09 | 苏州科技大学 | Preparation method of spherical titanium carbonitride ceramic powder |
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