CN115385697A - Production process of high-nitrogen titanium carbonitride - Google Patents
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- CN115385697A CN115385697A CN202211018072.XA CN202211018072A CN115385697A CN 115385697 A CN115385697 A CN 115385697A CN 202211018072 A CN202211018072 A CN 202211018072A CN 115385697 A CN115385697 A CN 115385697A
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Abstract
The invention provides a production process of high-nitrogen titanium carbonitride, which comprises the following steps: compounding, high temperature carbonization, secondary carbonization, analysis adjustment, add nitrogen, abrasive material process, through high temperature carbonization, secondary carbonization then the adjustment ratio compounding again, can the content of greatly reduced free carbon, advance again in the vacuum hot pressing stove with nitrogen gas and carry out the nitrogenize, can produce the titanium carbonitride product of high nitrogen, the nitrogen content is high, simple process, production efficiency is high.
Description
Technical Field
The invention relates to the technical field of metal materials, in particular to a production process of high-nitrogen titanium carbonitride.
Background
Titanium carbide is a steel gray crystal with metallic luster, the crystal structure belongs to a typical NaCl structure, and the lattice constant a =0.4320nm. The density of the titanium carbide at 20 ℃ is 4.91g/cm 3 The melting point is 3150 seconds 10 ℃, the boiling point is 4300 ℃, the Mohs hardness is 9.5, and the hardness is second to that of diamond. The titanium carbide has good heat transfer performance and electric conductivity, and the electric conductivity is reduced along with the increase of temperature, which shows that the titanium carbide has the property of metal. Titanium carbide also has excellent oxidation resistance, chemical stability and thermal stability, and can be widely applied to the electronic, chemical and microelectronic industries.
Titanium carbonitrideIs a single compound formed by continuously solid-dissolving titanium carbide and titanium nitride, the crystal structure of the titanium carbonitride is similar to that of the titanium carbide, and part of C atoms in the titanium carbide are replaced by N atoms. The lattice constant of titanium carbonitride is intermediate between that of titanium carbide and titanium nitride, and as the C content decreases, the lattice constant decreases accordingly. The C atoms in the titanium carbide can be replaced by N atoms in any proportion to form a continuous solid solution Ti (C) 1-x N x ) (0 < x < l), the property changes with the change of x, and the hardness of the material decreases and the toughness improves with the increase of the value of x. Titanium carbonitride is a non-oxide ceramic material with excellent performance as a continuous solid solution of titanium carbide and titanium nitride, and has the characteristics of high melting point, high hardness, corrosion resistance and good oxidation resistance, so the titanium carbonitride is widely applied to the fields of mechanical chemistry, automobile manufacturing, aerospace and the like. The titanium carbonitride-based hard alloy cutter has high strength, high hardness, good oxidation resistance and good heat conduction performance, so that the adopted titanium carbonitride-based hard alloy cutter has better wear resistance, size precision and surface quality of the processed workpiece than the workpiece processed by the WC or TiC-based hard alloy cutter.
The application number of 201010534952.3 discloses a method for manufacturing a titanium carbonitride hard alloy material, titanium dioxide (TiO 2) is used as a raw material, and TiO is used as 2 Mixed with carbon (C) (about 1 kg TiO) 2 Mixing with 0.2-0.5 kg of carbon (C) to ensure that the added carbon (C) can not completely reduce the titanium dioxide (TiO) 2 ) The excess oxygen (O) in the reaction mixture is excessive, so that the excessive carbon (C) and part of the titanium (Ti) form titanium carbide (TiC), and the other part of the titanium (Ti) and the nitrogen (N) form titanium nitride (TiN). In the process, the temperature of two stages in one furnace is adopted and the temperature is automatically controlled. The first-stage temperature control is 1220-1240 ℃. The secondary temperature control is 1630-1670 ℃. In the feeding process, the raw materials need to be compacted and then sent into a sintering furnace, so that incomplete oxygen reaction is easily caused, and the oxygen content of the product is high. In addition, the conventional titanium carbonitride generally has the problem of low nitrogen content, and the problem needs to be solved.
Disclosure of Invention
Aiming at the technical defects in the background art, the invention provides a production process of high-nitrogen titanium carbonitride, which solves the technical problems and meets the actual requirements, and the specific technical scheme is as follows:
a production process of high-nitrogen titanium carbonitride comprises the following steps:
s1, mixing materials: mixing titanium dioxide and carbon black, and then grinding to obtain a mixture;
s2, high-temperature carbonization: after being loaded in a boat, the mixture is transferred to a high-temperature carbon tube furnace for sintering, and after being cooled, the mixture is fed;
s3, secondary carbonization: loading the mixture obtained in the step S2 into a boat again, transferring the boat into a high-temperature carbon tube furnace for sintering, cooling and then discharging;
s4, analysis and adjustment: analyzing the oxygen content and the free carbon content in the semi-finished product obtained in the step S3, and then adjusting the ratio of titanium dioxide to carbon black;
s5, adding nitrogen: transferring the mixture to a vacuum hot pressing furnace, introducing nitrogen, and keeping the temperature and the pressure at 1500 ℃ under the positive pressure condition for 15 to 20 hours;
s6, grinding materials: grinding under nitrogen atmosphere, and sieving to obtain high-nitrogen titanium carbonitride.
Specifically, in step S1, the mass ratio of titanium dioxide to carbon black is 100:25 to 50.
Specifically, in step S1, grinding is performed by a ball mill, an alloy ball is used as a medium, the grinding time is 8 hours, and the Fsss of a mixture obtained after grinding is 1 to 3 μm.
Specifically, in the step S3, the temperature set in the high-temperature carbon tube furnace is 1650 to 1700 ℃, and the sintering time is 1 to 3h.
Specifically, in the step S4, the temperature in the high-temperature carbon tube furnace is 1680 to 1720 ℃, and the sintering time is 4 to 5h.
Specifically, the boat loading state of the mixture in the steps S2 and S3 is loose loading, and the mixture enters the high-temperature carbon tube furnace according to 30 min/boat after the loose loading is finished.
Specifically, in step S4, the pressure in the vacuum hot-pressing furnace is not lower than 1.2MPa.
Specifically, in the titanium carbonitride obtained in step S6, the nitrogen content is higher than 17%, the oxygen content is not higher than 0.40%, and the free carbon content is lower than 0.30%.
The invention has the beneficial effects that:
1. the production process comprises the working procedures of material mixing, high-temperature carbonization, secondary carbonization, analysis and adjustment, nitrogen adding and material grinding, wherein the materials are subjected to high-temperature carbonization and secondary carbonization and then mixed again by adjusting the proportion, so that the content of free carbon can be greatly reduced, and then the materials are fed into a vacuum hot-pressing furnace and nitrogen is added for nitridation, so that a high-nitrogen titanium carbonitride product can be produced, and the production process has the advantages of high nitrogen content, simple process and high production efficiency;
2. through high-temperature carbonization, secondary carbonization is carried out after loose packing, so that the oxygen reaction is more complete, and titanium nitrogen carbon is better compounded to ensure the purity of subsequent products.
Detailed Description
Embodiments of the present invention will be described with reference to the following examples, which are not limited to the following examples, and the present invention relates to relevant essential parts in the technical field, and it should be considered that the known technology in the technical field can be known and grasped by those skilled in the art.
Example 1: the embodiment discloses a production process of high-nitrogen titanium carbonitride, which comprises the following steps: weighing 100kg of titanium dioxide and 45kg of carbon black as raw materials for later use, mixing the titanium dioxide and the carbon black, transferring the mixture into a ball mill for grinding, and taking an alloy ball as a medium, wherein the grinding time is 8 hours, and a mixture with the Fsss of 1.50 mu m is obtained after grinding; loading the mixture into a boat, wherein the loading state is loose, i.e. compaction is not needed, transferring the mixture into a high-temperature carbon tube furnace for sintering, the temperature in the high-temperature carbon tube furnace is 1650 ℃, the sintering time is 2 hours, cooling to normal temperature, and then discharging; the mixture is packaged again, the charging state is loose packaging, namely compaction is not needed, the loose packaging is carried out, the mixture enters a high-temperature carbon tube furnace for sintering according to 30 min/boat, the temperature set in the high-temperature carbon tube furnace is 1700 ℃, the sintering time is 4h, the mixture is cooled to normal temperature, and then blanking is carried out, so that a semi-finished product is obtained; if the oxygen content is higher than 0.5 percent, the proportion of the titanium dioxide and the carbon black is reduced until the oxygen content in the semi-finished product is not higher than 0.5 percent; transferring the semi-finished product into a vacuum hot-pressing furnace, introducing nitrogen, and controllingThe pressure for preparing nitrogen is 1.2MPa, the heat preservation and the pressure maintenance are carried out for 15 hours under the conditions of 1500 ℃ and positive pressure, and the reaction in the process is as follows: 2TiO 2 2 +6C+N 2 =2TiCN +4CO ═; grinding in nitrogen atmosphere, and sieving to obtain high-nitrogen titanium carbonitride; and (3) taking the obtained titanium carbonitride part sample to perform total carbon content, free carbon content detection, oxygen content detection, nitrogen content detection and Fisher's particle size (Fsss) detection, recording the detection result as shown in the following table 1, mixing titanium carbonitride powder obtained in different batches of production processes after the detection is qualified, and packaging and storing.
Example 2: the embodiment discloses a production process of high-nitrogen titanium carbonitride, which comprises the following steps: weighing 100kg of titanium dioxide and 30kg of carbon black as raw materials for later use, mixing the titanium dioxide and the carbon black, transferring the mixture into a ball mill for grinding, taking an alloy ball as a medium, wherein the grinding time is 8 hours, and obtaining a mixture with the Fsss of 2.80 mu m after grinding; loading the mixture into a boat, wherein the loading state is loose, i.e. compaction is not needed, transferring the mixture into a high-temperature carbon tube furnace for sintering, the temperature in the high-temperature carbon tube furnace is 1650 ℃, the sintering time is 2 hours, cooling to normal temperature, and then discharging; the mixture is packaged again, the charging state is loose packaging, namely compaction is not needed, the loose packaging is carried out, the mixture enters a high-temperature carbon tube furnace for sintering according to 30 min/boat, the temperature set in the high-temperature carbon tube furnace is 1700 ℃, the sintering time is 4h, the mixture is cooled to normal temperature, and then blanking is carried out, so that a semi-finished product is obtained; if the oxygen content is higher than 0.5 percent, the proportion of the titanium dioxide and the carbon black is reduced until the oxygen content in the semi-finished product is not higher than 0.5 percent; transferring the semi-finished product to a vacuum hot pressing furnace, introducing nitrogen, controlling the pressure of the nitrogen to be 1.8MPa, and keeping the temperature and the pressure for 15 hours at 1500 ℃ under the condition of positive pressure, wherein the reaction in the process is as follows: 2TiO 2 2 +6C+N 2 =2TiCN +4CO ═; grinding in a nitrogen atmosphere, and sieving to obtain high-nitrogen titanium carbonitride; and (2) carrying out total carbon content detection, free carbon content detection, oxygen content detection, nitrogen content detection and Fisher's particle size (Fsss) detection on the obtained titanium carbonitride partial sample, recording detection results as shown in the following table 1, mixing titanium carbonitride powder obtained in different batches of production processes after the detection is qualified, and packaging and storing the mixed titanium carbonitride powder.
Comparative example 1: this comparative example discloses a method for producing a titanium carbonitride hard alloy material using titanium dioxide (TiO 2) as a raw material and TiO 2 Mixed with carbon (C) (about 1 kg TiO titanium dioxide) 2 Mixing with 0.2 kg of carbon (C) to ensure that the added carbon (C) can completely reduce oxygen (O) in titanium dioxide (TiO 2) and needs to be excessive, so that the excessive carbon (C) and part of titanium (Ti) form titanium carbide (TiC), and the other part of titanium (Ti) and nitrogen (N) form titanium nitride (TiN). Wherein, tiO 2 130kg C, 26.3kg, mixing TiO 2 Mixing the mixture with the C, uniformly stirring the mixture into a mixed material, putting the uniformly mixed material into a sintering container, compacting the mixed material, sending the compacted mixed material into a sintering furnace, and sintering the mixture by adopting a double temperature control mode to prepare TiCN; wherein the primary temperature control is 1220-1240 ℃ and the sintering time is 50-55 minutes. The secondary temperature control is 1630-1670 ℃, and the sintering time is 70-75 minutes. The whole manufacturing time is only 2 hours per boat; and (3) taking the obtained titanium carbonitride part sample to perform total carbon content, free carbon content detection, oxygen content detection, nitrogen content detection and Fisher's particle size (Fsss) detection, recording the detection result as shown in the following table 1, mixing titanium carbonitride powder obtained in different batches of production processes after the detection is qualified, and packaging and storing.
TABLE 1 test results
| Item | Total carbon content (μm) | Free carbon content (%) | Oxygen content (%) | Nitrogen content (%) | Fsss（μm） |
| Example 1 | 4.96 | 0.11 | 0.27 | 17.3 | 1.30 |
| Example 2 | 4.85 | 0.05 | 0.29 | 17.1 | 2.30 |
| Comparative example 1 | 6.32 | 0.52 | 1.01 | 14.6 | 1.80 |
Compared with the titanium carbonitride prepared by the conventional preparation method in the comparative example 1, the titanium carbonitride prepared by the preparation method in the embodiment 1-2 has the advantages of obviously improved nitrogen content, obviously reduced oxygen content and free carbon content, and high product purity.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A production process of high-nitrogen titanium carbonitride is characterized by comprising the following steps:
s1, mixing materials: mixing titanium dioxide and carbon black, and then grinding to obtain a mixture;
s2, high-temperature carbonization: after being loaded in a boat, the mixture is transferred to a high-temperature carbon tube furnace for sintering, and after being cooled, the mixture is fed;
s3, secondary carbonization: re-loading the mixture obtained in the step S2 into a boat, transferring the boat into a high-temperature carbon tube furnace for sintering, cooling and then discharging;
s4, analysis and adjustment: analyzing the oxygen content and the free carbon content in the semi-finished product obtained in the step S3, and then adjusting the ratio of titanium dioxide to carbon black;
s5, adding nitrogen: transferring the mixture into a vacuum hot pressing furnace, introducing nitrogen, and keeping the temperature and the pressure for 15 to 20 hours at 1500 ℃ under the positive pressure condition;
s6, grinding materials: grinding the materials in the nitrogen atmosphere, and sieving the materials to obtain the high-nitrogen titanium carbonitride.
2. The process for producing titanium carbonitride containing high nitrogen content as claimed in claim 1, wherein in the step S1, the mass ratio of titanium dioxide to carbon black is 100:25 to 50.
3. The process for producing titanium carbonitride containing high nitrogen as claimed in claim 1, wherein in step S1, the grinding is performed by a ball mill, an alloy ball is used as a medium, the grinding time is 8 hours, and the Fsss of the mixture obtained after grinding is 1 to 3 μm.
4. The process for producing high-nitrogen titanium carbonitride according to claim 1, wherein in the step S3, the temperature in the high-temperature carbon tube furnace is 1650 to 1700 ℃, and the sintering time is 1 to 3h.
5. The process for producing high-nitrogen titanium carbonitride according to claim 1, wherein in the step S4, the temperature in the high-temperature carbon tube furnace is set to be 1680 to 1720 ℃ and the sintering time is 4 to 5h.
6. The process for producing high-nitrogen titanium carbonitride as claimed in claim 1, wherein the loading state of the mixture in steps S2 and S3 is loose loading, and the mixture is fed into the high-temperature carbon tube furnace at 30 min/boat after the loose loading is completed.
7. The process for producing titanium carbonitride containing high nitrogen as claimed in claim 1, wherein in step S4, the pressure in the vacuum hot pressing furnace is not lower than 1.2MPa.
8. The process for producing titanium carbonitride of high nitrogen content according to claim 1, characterized in that the titanium carbonitride obtained through step S6 has a nitrogen content higher than 17%, an oxygen content not higher than 0.40% and a free carbon content lower than 0.30%.
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| JPH08333107A (en) * | 1995-06-07 | 1996-12-17 | Tokyo Tungsten Co Ltd | Production of powder of titanium carbide nitride |
| JP2000327423A (en) * | 1999-05-14 | 2000-11-28 | Toshiba Ceramics Co Ltd | Bolt and nut made of titanium carbonitride sintered body |
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| US20210061660A1 (en) * | 2016-08-22 | 2021-03-04 | Sumitomo Electric Industries, Ltd. | Titanium carbonitride powder and method for manufacturing titanium carbonitride powder |
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