CN115198157B - Grain growth induced pressureless sintering ultra-fine grain Ti (C, N) -based cermet densification method - Google Patents
Grain growth induced pressureless sintering ultra-fine grain Ti (C, N) -based cermet densification method Download PDFInfo
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- CN115198157B CN115198157B CN202210792474.9A CN202210792474A CN115198157B CN 115198157 B CN115198157 B CN 115198157B CN 202210792474 A CN202210792474 A CN 202210792474A CN 115198157 B CN115198157 B CN 115198157B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/04—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbonitrides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
A grain growth induced pressureless sintering ultra-fine grain Ti (C, N) -based cermet densification method relates to a cermet densification method. The invention aims to solve the problems that the densification of ultra-fine grain Ti (C, N) -based cermet prepared by pressureless sintering is difficult and the manufacturing cost is increased by means of gas pressure sintering. The method comprises the following steps: 1. weighing 50-60 parts of Ti (C, N), 10-30 parts of WC, 5-10 parts of TaC, 1-5 parts of VC, 10-20 parts of metal binder phase, 0.5-3 parts of carbon black and 1-4 parts of polyvinyl alcohol according to parts by weight; 2. ball milling and mixing; 3. drying and granulating; 4. compression molding; 5. and (5) sintering. The density of the densified ultrafine-grained Ti (C, N) -based cermet prepared by the method is 96.67-99%. The invention can obtain ultra-fine grain Ti (C, N) -based cermet.
Description
Technical Field
The invention relates to a method for densifying metal ceramics.
Background
Ti (C, N) -based cermet usually uses Ti (C, N) as a hard phase, ni, co and other metals as a bonding phase, and transition metal carbide as an additive phase, and has hardness, wear resistance and oxidation resistance at high temperature (700-1100 ℃) obviously superior to WC-Co hard alloy, fracture toughness obviously superior to superhard material and ceramic tool material, and the manufactured tool has the characteristics of high cutting speed, good quality of processed surface, long service life of the tool and the like, makes up the blank between WC-Co hard alloy and ceramic tool in the range of processing materials, and becomes a potential substitute material of WC-Co hard alloy.
The further improvement of the performance of the cutter material through grain refinement is a hot point direction and a main trend of the development of the cutter material. The superfine powder has high specific surface area and high surface activity, usually has higher sintering activity, and plays an obvious role in promoting the densification of solid-phase sintering. However, in the liquid phase sintering process, the liquid phase filling the pores is the basic process of densification, and plays an important role even in the early stage of the liquid phase sintering. The critical condition for the liquid phase to fill the pores depends on the radius of curvature of the liquid-gas meniscus between the particles, which in turn is positively correlated with the particle size. Therefore, the densification process and the grain size show a negative correlation relationship, which also causes difficulty in densification of pressureless sintered ultrafine-grained Ti (C, N) -based cermet, and finally results in insufficient mechanical properties and poor reliability. Therefore, to prepare highly dense, high-toughness, ultra-fine grain Ti (C, N) -based cermets, it is usually accomplished by gas pressure sintering, which undoubtedly increases the manufacturing cost.
Disclosure of Invention
The invention aims to solve the problems that the preparation of ultra-fine grain Ti (C, N) -based cermet by pressureless sintering is difficult to densify and the manufacturing cost is increased by means of the pressureless sintering, and provides a method for densifying ultra-fine grain Ti (C, N) -based cermet by grain growth induction pressureless sintering.
A method for densifying grain growth induced pressureless sintering ultra-fine grain Ti (C, N) -based cermet is specifically completed according to the following steps:
1. weighing:
(1) weighing 50-60 parts of Ti (C, N), 10-30 parts of WC, 5-10 parts of TaC, 1-5 parts of VC, 10-20 parts of metal bonding phase, 0.5-3 parts of carbon black and 1-4 parts of polyvinyl alcohol according to parts by weight to obtain a raw material;
the metal bonding phase in the step one (1) is one or two of Ni and Co;
(2) adding water and absolute ethyl alcohol into the raw materials to obtain slurry;
2. ball-milling and mixing:
ball-milling the slurry to obtain ball-milled slurry;
3. drying and granulating:
drying the ball-milled slurry under a vacuum condition to obtain metal ceramic mixed powder;
4. compression molding:
filling the metal ceramic mixed powder into a powder pressing mold, applying pressure to perform press forming, and maintaining the pressure to obtain a pressed blank;
5. and (3) sintering:
sintering the pressed compact by adopting vacuum sintering or nitrogen sintering, and cooling along with a furnace to obtain the densified superfine crystal Ti (C, N) -based cermet.
The principle of the invention is as follows:
based on the 'pore filling theory', the densification process is in a negative correlation with the particle size of the densification process, so that the growth of crystal grains plays a certain role in promoting the densification of the material in the liquid phase sintering process, and for multi-component Ti (C, N) -based cermet, the driving force of the growth of the crystal grains is not only related to the particle size distribution of the initial raw material powder, but also influenced by the component gradient among different components and the difference of the dissolution degrees in the liquid phase; under the condition that the particle size distribution of the initial raw material powder is the same, thermodynamically unstable (higher lattice energy) carbon (nitride) particles tend to dissolve and precipitate on the surfaces of the particles with higher thermodynamic stability; therefore, by regulating and controlling the type and the addition amount of the high-melting-point carbide, the sintering temperature and the heat preservation time, the growth of specific grains can be realized, the liquid phase is induced to fill pores, and the densification of the pressureless sintered ultrafine-grained Ti (C, N) -based cermet is promoted.
The invention has the following beneficial effects:
1. the invention can realize the pressureless sintering preparation of high-density ultrafine-grained Ti (C, N) -based cermet by regulating and controlling the type and the addition amount of high-melting-point carbide, the sintering temperature and the heat preservation time, thereby improving the service performance and the reliability of the material, simplifying the preparation process and reducing the production cost;
2. in the densified ultrafine-grained Ti (C, N) -based cermet prepared by the method, the high-melting-point carbide additive phase is beneficial to improving the high-temperature mechanical property and the oxidation resistance of the cermet;
3. the densified ultrafine-grained Ti (C, N) -based cermet prepared by the method continues to use the traditional preparation process of coarse-grained and medium-grained Ti (C, N) -based cermet, does not need new process steps, is simple to operate and is suitable for large-scale industrial production;
4. the density of the prepared densified superfine crystal Ti (C, N) -based cermet is 96.67-99%.
The invention can obtain ultra-fine grain Ti (C, N) -based cermet.
Drawings
FIG. 1 is a SEM/BSE photograph of densified ultra-fine grain Ti (C, N) -based cermets prepared in example 1, example 5, example 6 and example 7;
FIG. 2 is an SEM/BSE photograph of densified ultra-fine grain Ti (C, N) -based cermets prepared in comparative example 1, comparative example 2, comparative example 3 and comparative example 4.
Detailed Description
The following examples further illustrate the present invention but are not to be construed as limiting the invention. Modifications and substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit of the invention.
The first embodiment is as follows: the embodiment of the invention relates to a method for densifying grain growth induced pressureless sintering ultrafine-grained Ti (C, N) -based cermet, which is specifically completed according to the following steps:
1. weighing:
(1) weighing 50-60 parts of Ti (C, N), 10-30 parts of WC, 5-10 parts of TaC, 1-5 parts of VC, 10-20 parts of metal bonding phase, 0.5-3 parts of carbon black and 1-4 parts of polyvinyl alcohol according to parts by weight to obtain a raw material;
the metal bonding phase in the step one (1) is one or two of Ni and Co;
(2) adding water and absolute ethyl alcohol into the raw materials to obtain slurry;
2. ball milling and mixing:
ball-milling the slurry to obtain ball-milled slurry;
3. drying and granulating:
drying the ball-milled slurry under a vacuum condition to obtain metal ceramic mixed powder;
4. compression molding:
filling the metal ceramic mixed powder into a powder pressing mold, applying pressure to perform press forming, and maintaining the pressure to obtain a pressed blank;
5. and (3) sintering:
sintering the pressed compact by adopting vacuum sintering or nitrogen sintering, and cooling along with a furnace to obtain the densified superfine crystal Ti (C, N) -based cermet.
The second embodiment is as follows: the present embodiment differs from the present embodiment in that: the grain diameters of the Ti (C, N), the additive phase for improving the wettability, the key additive phase for inducing the densification through the grain growth, the additive phase for inhibiting the grain growth and the metal binder phase in the step one (1) are 100-300 nm, and the oxygen content is lower than 0.5wt.%. Other steps are the same as in the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the solid content of the slurry in the step one (2) is 40-70%. The other steps are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is as follows: the volume ratio of the water to the absolute ethyl alcohol in the step one (2) is (10-90) to (90-10). The other steps are the same as those in the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: and in the ball milling in the step two, the slurry is subjected to ball milling in a roller ball milling or stirring ball milling mode under the protection of nitrogen atmosphere, the grinding balls used in the ball milling are hard alloy balls, the ball-to-material ratio is (4-20): 1, and the ball milling time is 12-48 h. The other steps are the same as those in the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: the pressure applied in the fourth step is 50 MPa-200 MPa. The other steps are the same as those in the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the pressure maintaining time in the fourth step is 1-5 min. The other steps are the same as those in the first to sixth embodiments.
The specific implementation mode is eight: the difference between this embodiment and one of the first to seventh embodiments is: the vacuum sintering method in the fifth step specifically comprises the following steps: placing the pressed compact in a sintering furnace, vacuumizing to below 50Pa, starting heating, heating to 1400-1500 ℃ at the heating rate of 5-10 ℃/min, and preserving heat for 1-2 h at 1400-1500 ℃. The other steps are the same as those in the first to seventh embodiments.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is: the nitrogen sintering method in the fifth step specifically comprises the following steps: placing the pressed compact in a sintering furnace, vacuumizing to below 50Pa, starting heating, heating to 1400-1500 ℃ at the heating rate of 5-10 ℃/min, introducing high-purity nitrogen of 1-10 kPa, and preserving heat for 1-2 h at the temperature of 1400-1500 ℃ in nitrogen. The other steps are the same as those in the first to eighth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
example 1: a method for densifying grain growth induced pressureless sintering ultra-fine grain Ti (C, N) -based cermet is specifically completed according to the following steps:
1. weighing;
(1) weighing 56 parts of Ti (C) according to parts by weight 0.5 N 0.5 ) 17 parts of WC, 8.5 parts of TaC, 1.5 parts of VC, 4.25 parts of Ni, 12.75 parts of Co, 0.5 part of carbon black and 4 parts of polyvinyl alcohol to obtain a raw material;
ti (C) described in step one (1) 0.5 N 0.5 ) The grain sizes of WC, taC, VC, ni and Co are all 100 nm-300 nm, and the oxygen content is lower than 0.5 wt%;
(2) adding water and absolute ethyl alcohol into the raw materials to obtain slurry;
the solid content of the slurry in the step one (2) is 50 percent;
the volume ratio of the water to the absolute ethyl alcohol in the step one (2) is 3;
2. ball milling and mixing:
placing the slurry obtained in the step one (2) in a ball milling tank with a hard alloy lining, filling nitrogen, adding hard alloy grinding balls according to a ball-to-material ratio of 10;
3. drying and granulating:
drying the ball-milled slurry under a vacuum condition to obtain metal ceramic mixed powder;
4. compression molding:
filling the metal ceramic mixed powder into a powder pressing mold, applying 100MPa pressure for pressing and forming, and maintaining the pressure for 3min to obtain a pressed blank;
5. and (3) sintering:
and placing the pressed blank in a sintering furnace, vacuumizing to below 50Pa, starting to heat, heating to 1425 ℃ at the heating rate of 5 ℃/min, preserving heat for 1h at 1425 ℃, and cooling to room temperature along with the furnace to obtain the densified ultrafine-grained Ti (C, N) -based cermet.
Comparative example 1: the present embodiment is different from embodiment 1 in that: step one (1), weighing 56 parts of Ti (C) according to parts by weight 0.5 N 0.5 ) 25.5 parts of WC, 1.5 parts of VC, 4.25 parts of Ni, 12.75 parts of Co, 0.5 part of carbon black and 4 parts of polyvinyl alcohol to obtain a raw material; ti (C) described in step one (1) 0.5 N 0.5 ) The grain diameters of WC, VC, ni and Co are all 100 nm-300 nm, and the oxygen content is lower than 0.5wt.%. The other steps and parameters were exactly the same as in example 1.
Comparative example 1 compared to example 1, without TaC; the densification of the densified ultra-fine grained Ti (C, N) -based cermets prepared in example 1 and comparative example 1 was tested and the results showed that: example 1 the densified ultra-fine grained Ti (C, N) -based cermet prepared using TaC had a density of 96.67%, and comparative example 1, without TaC, prepared a densified ultra-fine grained Ti (C, N) -based cermet having a density of 91.38%, which differed by about 4%.
Example 2: the present embodiment is different from embodiment 1 in that: and fifthly, placing the pressed compact in a sintering furnace, vacuumizing to below 50Pa, starting heating, heating to 1450 ℃ at the heating rate of 5 ℃/min, preserving heat for 1h at 1450 ℃, and cooling to room temperature along with the furnace to obtain the densified ultrafine-grained Ti (C, N) -based cermet. The other steps and parameters were exactly the same as in example 1.
Example 3: the present embodiment is different from embodiment 1 in that: and step five, placing the pressed blank in a sintering furnace, vacuumizing to below 50Pa, starting heating, heating to 1475 ℃ at the heating rate of 5 ℃/min, preserving the heat at 1475 ℃ for 1h, and cooling to room temperature along with the furnace to obtain the densified superfine crystal Ti (C, N) -based cermet. The other steps and parameters were exactly the same as in example 1.
Example 4: the present example is different from example 1 in that: and fifthly, placing the pressed blank in a sintering furnace, vacuumizing to below 50Pa, starting heating, heating to 1500 ℃ at the heating rate of 5 ℃/min, preserving heat for 1h at 1500 ℃, and cooling to room temperature along with the furnace to obtain the densified superfine crystal Ti (C, N) -based cermet. The other steps and parameters were exactly the same as in example 1.
The highest sintering temperatures of example 1, example 2, example 3 and example 4 were 1425 ℃, 1450 ℃, 1475 ℃ and 1500 ℃; the densification of the densified ultra-fine grained Ti (C, N) -based cermets prepared in examples 1 to 4 are shown in table 1;
TABLE 1
Example 5: the present example is different from example 1 in that: and fifthly, placing the pressed compact in a sintering furnace, vacuumizing to below 50Pa, starting heating, heating to 1425 ℃ at the heating rate of 5 ℃/min, preserving heat for 0h at 1425 ℃, and cooling to room temperature along with the furnace to obtain the densified superfine crystal Ti (C, N) -based cermet. The other steps and parameters were exactly the same as in example 1.
Example 6: the present example is different from example 1 in that: and fifthly, placing the pressed compact in a sintering furnace, vacuumizing to below 50Pa, starting heating, heating to 1425 ℃ at the heating rate of 5 ℃/min, preserving heat for 2h at 1425 ℃, and cooling to room temperature along with the furnace to obtain the densified superfine crystal Ti (C, N) -based cermet. The other steps and parameters were exactly the same as in example 1.
Example 7: the present example is different from example 1 in that: and fifthly, placing the pressed compact in a sintering furnace, vacuumizing to below 50Pa, starting heating, heating to 1425 ℃ at the heating rate of 5 ℃/min, preserving heat for 4h at 1425 ℃, and cooling to room temperature along with the furnace to obtain the densified superfine crystal Ti (C, N) -based cermet. The other steps and parameters were exactly the same as in example 1.
Examples 1, 5, 6 and 7 were held at a maximum sintering temperature of 1425 ℃ for different holding times, and the densification densities and grain sizes of the densified ultra-fine grained Ti (C, N) -based cermets prepared in examples 1, 5, 6 and 7 are shown in table 2;
TABLE 2
Comparative example 2: the present example is different from comparative example 1 in that: and step five, placing the pressed blank in a sintering furnace, vacuumizing to below 50Pa, starting to heat, heating to 1425 ℃ at the heating rate of 5 ℃/min, preserving heat for 0h at 1425 ℃, and cooling to room temperature along with the furnace to obtain the densified ultrafine-grained Ti (C, N) -based cermet. The other steps and parameters were exactly the same as in comparative example 1.
Comparative example 3: the present example is different from comparative example 1 in that: and step five, placing the pressed blank in a sintering furnace, vacuumizing to below 50Pa, starting to heat, heating to 1425 ℃ at the heating rate of 5 ℃/min, preserving heat for 2 hours at 1425 ℃, and cooling to room temperature along with the furnace to obtain the densified ultrafine-grained Ti (C, N) -based cermet. The other steps and parameters were exactly the same as in comparative example 1.
Comparative example 4: the present example is different from comparative example 1 in that: and fifthly, placing the pressed compact in a sintering furnace, vacuumizing to below 50Pa, starting heating, heating to 1425 ℃ at the heating rate of 5 ℃/min, preserving heat for 4h at 1425 ℃, and cooling to room temperature along with the furnace to obtain the densified superfine crystal Ti (C, N) -based cermet. The other steps and parameters were exactly the same as in comparative example 1.
The densities of the densified ultra-fine grained Ti (C, N) -based cermets prepared in comparative example 1, comparative example 2, comparative example 3 and comparative example 4 are shown in table 3;
TABLE 3
SEM/BSE photographs of the densified ultra-fine grained Ti (C, N) -based cermets prepared in comparative example 1, comparative example 2, comparative example 3 and comparative example 4 are shown in FIG. 2;
as can be seen from fig. 2: the dissolution degree of black Ti (C, N) phase in the metal ceramic system without adding TaC is low, the boundary of gray phase crystal grains is difficult to distinguish through color contrast, and no obvious phenomenon of coarsening of the gray phase crystal grains is seen.
Claims (6)
1. A method for densifying ultra-fine grain Ti (C, N) -based cermet through grain growth-induced pressureless sintering is characterized by comprising the following steps:
1. weighing:
(1) weighing 50-60 parts of Ti (C, N), 10-30 parts of WC, 5-10 parts of TaC, 1-5 parts of VC, 10-20 parts of metal bonding phase, 0.5-3 parts of carbon black and 1-4 parts of polyvinyl alcohol according to parts by weight to obtain a raw material;
the metal bonding phase in the step one (1) is one or two of Ni and Co;
the particle sizes of Ti (C, N), WC, taC, VC and the metal binding phase in the step one (1) are all 100-300 nm, and the oxygen content is lower than 0.5 wt%;
(2) adding water and absolute ethyl alcohol into the raw materials to obtain slurry;
2. ball milling and mixing:
performing ball milling on the slurry to obtain ball-milled slurry;
3. drying and granulating:
drying the ball-milled slurry under a vacuum condition to obtain metal ceramic mixed powder;
4. compression molding:
filling the metal ceramic mixed powder into a powder pressing mold, applying pressure to perform press forming, and maintaining the pressure to obtain a pressed blank;
5. and (3) sintering:
sintering the pressed blank by adopting vacuum sintering or nitrogen sintering, and cooling along with a furnace to obtain densified ultrafine-grained Ti (C, N) -based cermet;
the vacuum sintering method in the fifth step specifically comprises the following steps: placing the pressed blank in a sintering furnace, vacuumizing to below 50Pa, starting heating, heating to 1475-1500 ℃ at the heating rate of 5-10 ℃/min, and keeping the temperature at 1475-1500 ℃ for 1-2 h;
the nitrogen sintering method in the fifth step specifically comprises the following steps: placing the pressed compact in a sintering furnace, vacuumizing to below 50Pa, starting heating, heating to 1475-1500 ℃ at the heating rate of 5-10 ℃/min, introducing high-purity nitrogen with the pressure of 1-10 kPa, and keeping the temperature for 1-2 h at the temperature of 1475-1500 ℃ in nitrogen.
2. The method of grain growth induced pressureless sintered ultra-fine grained Ti (C, N) -based cermet densification of claim 1 wherein the slurry in step one (2) has a solids content of 40% to 70%.
3. The method for grain growth-induced pressureless sintered ultra-fine grained Ti (C, N) -based cermet densification according to claim 1, wherein the volume ratio of water and absolute ethanol in step one (2) is (10-90) to (90-10).
4. The method for densifying a grain growth-induced pressureless sintered ultrafine grained Ti (C, N) -based cermet according to claim 1, wherein the ball milling in step two is performed on the slurry by roller ball milling or stirring ball milling under the protection of nitrogen atmosphere, the ball milling uses cemented carbide balls with a ball-to-material ratio of (4-20): 1, and the ball milling time is 12-48 h.
5. The method for densifying a grain growth-induced pressureless sintered ultrafine-grained Ti (C, N) -based cermet according to claim 1, wherein the pressure applied in step four is in the range of 50MPa to 200MPa.
6. The method for grain growth-induced pressureless sintering of ultra-fine grain Ti (C, N) -based cermet densification of claim 1 wherein the pressure is maintained in step four for a period of time ranging from 1min to 5min.
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| JP3669689B2 (en) * | 2001-02-13 | 2005-07-13 | 日立ツール株式会社 | TiCN-based cermet tool |
| JP5217417B2 (en) * | 2007-12-25 | 2013-06-19 | 三菱マテリアル株式会社 | Titanium carbonitride-based cermet cutting tool with excellent wear resistance |
| CN103981419B (en) * | 2014-04-09 | 2016-05-11 | 宁波东联密封件有限公司 | A kind of high strength carbon titanium-nitride cermet encapsulant and preparation method thereof |
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