CN110373593B - Microwave sintering process of titanium carbonitride-based composite metal ceramic material - Google Patents
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Abstract
The invention belongs to the field of material preparation, and particularly relates to a microwave sintering process of a titanium carbonitride-based composite metal ceramic material. The method comprises the following steps: step 1: weighing the powder according to a proportion, performing ball milling and mixing, adding 1-5% polyvinyl alcohol solution 1.5-2.5 hours before the ball milling is finished, drying, grinding and sieving after the ball milling; step 2: pressing and molding the screened powder; and step 3: and (3) putting the sample into a silicon carbide wafer auxiliary heating device by adopting a microwave sintering process, placing the silicon carbide wafer auxiliary heating device in a heat preservation box, continuously heating to 1550-1650 ℃ at the heating rate of 20-40 ℃/min, preserving the heat for 5-20 min, and then cooling along with a furnace to obtain the titanium carbonitride based composite metal ceramic material. In the microwave sintering, the silicon carbide wafer is adopted for auxiliary heating to replace the traditional powder-embedding auxiliary sintering, so that the polyvinyl alcohol can be fully volatilized in the sintering process, the internal pores of the material in the sintering process are reduced, and the density is improved; and the silicon carbide wafer is adopted for auxiliary heating, so that subsequent treatment is not needed, and the preparation flow is simplified.
Description
Technical Field
The invention belongs to the field of material preparation, and particularly relates to a microwave sintering process of a titanium carbonitride-based composite metal ceramic material.
Background
The titanium carbonitride-based cermet has high hardness, good wear resistance, excellent high-temperature chemical stability, extremely low friction coefficient to metal, strong heat deformation resistance and excellent mechanical property, especially has excellent high-temperature characteristic, has high strength even at 1300 ℃, and can be applied to the fields of aerospace parts, bearings, high-speed cutting tools and the like. At present, titanium carbonitride cermets are mostly prepared by using traditional sintering methods, such as reaction sintering, pressureless sintering, air pressure sintering, hot pressing sintering, hot isostatic pressing sintering and the like. However, conventional sintering suffers from a number of disadvantages, such as high equipment and maintenance costs; the heating mode of thermal radiation and thermal conduction causes the temperature gradient in the material to be larger, and the residual stress is easily generated in the material; the preparation period is long, the efficiency is low, and the batch production of materials is not facilitated. With the development of scientific technology, some new technologies are generated, and microwave sintering is taken as a novel sintering mode with high efficiency, energy conservation and environmental protection, thereby drawing attention and research of a plurality of scholars.
At present, the microwave sintering process of titanium carbonitride cermet materials is still not perfect, and reports thereof are relatively few. From the prior art (H.Hu, Y.Cheng, Z.yin, Y.Zhang, T.Lu, Mechanical properties and structural Ti (C, N) basedcergesting material fibrous ceramic material, ceramic International.41(2015)15017 and 15023), it is known that by adding Ni of 7.5% and Co of 7.5% in mass fraction as binders, a titanium carbonitride based cermet material with a hardness of up to 15.49 + -0.21 GPa and a fracture toughness of 10 + -0.55 MPa.m1/2 can be prepared by using a microwave sintering method. Compared with other ceramic materials, the toughness is relatively high, but the hardness is lower.
In the invention patent with patent application No. 201510779093.7, an alumina/titanium carbonitride composite ceramic is prepared, which is made of Al2O3Mainly Ti (C, N) is used as a reinforcing and toughening phase, when the content of aluminum oxide is 61 percent, the content of titanium carbonitride is 30 percent and the sintering temperature is 1550 ℃, the highest hardness reaches 18.4GPa, and the toughness is 6.72 MPa.m1/2The hardness is improved, but the toughness is still lower, and the lower toughness can cause the material to be easily subjected to brittle fracture, so that the application range of the material is greatly limited.
In conclusion, the existing microwave sintering process of titanium carbonitride cermet materials still has defects, and the prepared titanium carbonitride cermet materials have still unsatisfactory comprehensive mechanical properties.
Disclosure of Invention
The invention aims to provide a microwave sintering process of a titanium carbonitride-based composite metal ceramic material.
The technical solution for realizing the purpose of the invention is as follows:
a microwave sintering process for a titanium carbonitride-based composite cermet material comprises the following components in percentage by weight: 62 to 68 percent of Ti (C, N) and Mo215% of C, 5% of WC, 3% -6% of Ni, 6% -9% of Co and 3% -6% of Mo; the method comprises the following steps:
step 1: weighing Ti (C, N) and Mo in proportion2C. Ball milling and mixing WC, Ni, Co and Mo powder, adding 1-5% concentration polyvinyl alcohol solution 1.5-2.5 hr before ball milling, drying, grinding and sieving;
step 2: pressing and molding the screened powder under the pressure of 100-300MPa to obtain a metal ceramic biscuit (4);
and step 3: in an inert gas atmosphere, a microwave sintering process is adopted, a sample is placed in a silicon carbide wafer auxiliary heating device and placed in a heat preservation box, the temperature is continuously raised to 1550-1650 ℃ at the temperature rise rate of 20-40 ℃/min, the heat preservation is carried out for 5-20 min, and then furnace cooling is carried out, so that the titanium carbonitride based composite metal ceramic material is prepared.
Further, in the step (1), the ball milling and mixing step is to put the weighed powder into a corundum ball milling tank, and absolute ethyl alcohol is used as a ball milling medium, and the grinding ball is a tungsten carbide ball.
Further, the inert gas in the step (3) is nitrogen, and the nitrogen pressure is in the range of 0.1-0.12MPa and is in a flowing state.
Further, the auxiliary heating device in the step (3) comprises a silicon carbide ring and two silicon carbide pieces, wherein the silicon carbide ring is sleeved on the periphery of the metal ceramic biscuit, and the two silicon carbide pieces are respectively arranged on the upper side and the lower side of the metal ceramic biscuit.
Furthermore, the auxiliary heating device with the metal ceramic biscuit is arranged in a crucible which is arranged in a heat preservation box.
Compared with the prior art, the invention has the following remarkable advantages:
(1) in the microwave sintering, the silicon carbide wafer is adopted for auxiliary heating to replace the traditional powder-embedding auxiliary sintering, so that the polyvinyl alcohol can be fully volatilized in the sintering process, internal pores of the material in the sintering process are reduced, the density of the product is improved, and the performance is improved; and the silicon carbide wafer is adopted for auxiliary heating without subsequent treatment, so that the preparation process is simplified, the production efficiency is improved, and the production cost is reduced.
(2) The density and the comprehensive mechanical property of the metal ceramic are improved by taking Ni, Co and Mo as metal additives; ni and Co are liquefied at high temperature and generate transverse flow under the action of high-temperature driving energy, so that Ti (C, N) solid particles are subjected to particle rearrangement, and the microstructure of the metal ceramic is more uniform; the addition of Mo can improve the wettability between the liquid phase Ni and the solid particles Ti (C, N), so that the liquid phase Ni can better fill gaps among the solid particles, and the compactness of the metal ceramic is improved; during sintering, Ti (C, N) particles are partially dissolved in liquid phase Ni and Co, and a (Ti, W, Mo) (C, N) -Ni-Co solid solution is formed through precipitation and precipitation; the structure can effectively inhibit the growth of crystal grains, thereby improving the hardness of the material; the metal has good toughness, so the addition of the metal phase can greatly improve the fracture toughness of the material.
The present invention is described in further detail below with reference to the attached drawing figures.
Drawings
FIG. 1 shows an auxiliary heating device used in the present application.
FIG. 2 is an SEM image of a cross-section of a titanium carbonitride based composite cermet material prepared in example 9.
Description of reference numerals:
1-high temperature mullite, 2-high temperature mullite fiber, 3-silicon carbide chip and 4-metal ceramic biscuit.
Detailed Description
The titanium carbonitride based composite cermet material comprises the following components in percentage by weight: 62 to 68 percent of Ti (C, N) and Mo2C 15％、WC 5％、Ni 3％-6％、Co 6％-9％、Mo 3％-6％。
Preferred material components are Ti (C, N) 62%, Mo215% of C, 5% of WC, 6% of Ni, 6% of Co and 6% of Mo, the sample hardness reaches 16.25 +/-0.09 GPa, and the toughness reaches 12.41 +/-0.33 MPa1/2。
The invention also provides a microwave sintering method of the titanium carbonitride composite cermet material, which adopts an efficient and energy-saving microwave sintering technology to realize the preparation of the titanium carbonitride composite cermet material with higher comprehensive mechanical properties in a short period by improving an auxiliary heating device, optimizing parameters such as phase content, sintering temperature, heat preservation time and the like, and comprises the following steps:
In step 3, the auxiliary heating device is composed of two silicon carbide pieces and a silicon carbide ring as shown in fig. 1, the metal ceramic biscuit 4 is arranged between the two silicon carbide pieces, and the silicon carbide ring is sleeved around the sample piece and is arranged in the crucible. The heat preservation box is made of high-temperature mullite materials and is filled with high-temperature mullite fibers, and the crucible is arranged in the middle of the heat preservation box.
The density and the comprehensive mechanical property of the metal ceramic are improved by adopting Ni, Co and Mo as metal additives. Ni and Co are liquefied at high temperature and generate transverse flow under the action of high-temperature driving energy, so that Ti (C, N) solid particles are subjected to particle rearrangement, and the microstructure of the metal ceramic is more uniform. The addition of Mo can improve the wettability between the liquid phase Ni and the solid particles Ti (C, N), so that the liquid phase Ni can better fill the gaps between the solid particles, and the compactness of the metal ceramic is improved. During sintering, Ti (C, N) particles are partially dissolved in liquid phases of Ni and Co, and a (Ti, W, Mo) (C, N) -Ni-Co solid solution is formed by precipitation (shown in figure 2). The structure can wrap Ti (C, N) particles, thereby effectively inhibiting the growth of crystal grains and improving the hardness of the material. The metal has good toughness, so the addition of the metal phase can greatly improve the fracture toughness of the material. In summary, cermets having both good hardness and fracture toughness can be prepared by optimizing the component ratios of the metal additives. (Innovation points are described in a technical means way), the xxx structure is generated (in a microscopic or far-away way), and the xxx structure has the effect (combining hardness and toughness)
The following examples are further described in detail.
Example 1:
a titanium carbonitride based composite cermet material and a microwave sintering method thereof are disclosed, which comprises the following steps: 68% of Ti (C, N) and Mo in percentage by mass2C15%, WC 5%, Ni 3% and Co 9% are mixed, the prepared mixed powder is put into a corundum ball milling tank for ball milling for 24 hours by taking absolute ethyl alcohol as a medium and taking tungsten carbide balls as milling balls, the ball-material ratio is 8:1, and polyvinyl alcohol aqueous solution with the concentration of 3 wt% is added 2 hours before the ball milling is finished; carrying out drying and grinding after ball milling, sieving by a 100-mesh sieve, carrying out dry pressing molding on the sieved powder under the pressure of 300MPa, and keeping the pressure for 2 minutes; putting the pressed compact into a silicon carbide wafer auxiliary heating device, placing the silicon carbide wafer auxiliary heating device into a microwave sintering furnace, vacuumizing the furnace chamber, and then filling nitrogen with the pressure of 0.11 MPa; and (3) starting a microwave power supply to heat, heating the sample to 1600 ℃ at the heating rate of 20 ℃/min, preserving the temperature for 10min, and then cooling along with the furnace. The Vickers hardness of the material is 14.92 +/-0.90 GPa, and the fracture toughness is 11.58 +/-2.22 MPa.m1/2。
Example 2:
a titanium carbonitride based composite cermet material and a microwave sintering method thereof are disclosed, which comprises the following steps: 68% of Ti (C, N) and Mo in percentage by mass2C15%, WC 5%, Ni 3%, Co 6% and Mo 3% are proportioned, the prepared mixed powder is put into a corundum ball-milling tank for ball milling for 24 hours by taking absolute ethyl alcohol as a medium and taking tungsten carbide balls as milling balls, the ball-material ratio is 8:1, and polyvinyl alcohol aqueous solution with the concentration of 3 wt% is added 2 hours before the ball milling is finished; carrying out drying and grinding after ball milling, sieving by a 100-mesh sieve, carrying out dry pressing molding on the sieved powder under the pressure of 300MPa, and keeping the pressure for 2 minutes; putting the pressed compact into a silicon carbide wafer auxiliary heating device, placing the silicon carbide wafer auxiliary heating device into a microwave sintering furnace, vacuumizing the furnace chamber, and then filling nitrogen with the pressure of 0.11 MPa; and (3) starting a microwave power supply to heat, heating the sample to 1600 ℃ at the heating rate of 20 ℃/min, preserving the temperature for 10min, and then cooling along with the furnace. The Vickers hardness of the material is 13.14 +/-0.88 GPa, and the fracture toughness is obtained through testingThe property is 13.92 +/-3.31 MPa.m1/2。
As compared with example 1, when Mo is partially substituted for Co, the properties are different, the fracture toughness is improved, and the Vickers hardness is reduced in the same sintering process.
Example 3:
a titanium carbonitride based composite cermet material and a microwave sintering method thereof are disclosed, which comprises the following steps: 68% of Ti (C, N) and Mo in percentage by mass2C15%, WC 5%, Ni 3%, Co 3% and Mo 6% are proportioned, the prepared mixed powder is put into a corundum ball-milling tank for ball milling for 24 hours by taking absolute ethyl alcohol as a medium and taking tungsten carbide balls as milling balls, the ball-material ratio is 8:1, and polyvinyl alcohol aqueous solution with the concentration of 3 wt% is added 2 hours before the ball milling is finished; carrying out drying and grinding after ball milling, sieving by a 100-mesh sieve, carrying out dry pressing molding on the sieved powder under the pressure of 300MPa, and keeping the pressure for 2 minutes; putting the pressed compact into a silicon carbide wafer auxiliary heating device, placing the silicon carbide wafer auxiliary heating device into a microwave sintering furnace, vacuumizing the furnace chamber, and then filling nitrogen with the pressure of 0.11 MPa; and (3) starting a microwave power supply to heat, heating the sample to 1600 ℃ at the heating rate of 20 ℃/min, preserving the temperature for 10min, and then cooling along with the furnace. The Vickers hardness of the material is 6.08 +/-0.15 GPa, and the fracture toughness is 6.02 +/-1.26 MPa.m1/2。
Example 4:
a titanium carbonitride based composite cermet material and a microwave sintering method thereof are disclosed, which comprises the following steps: 62 percent of Ti (C, N) and Mo in percentage by mass2C15%, WC 5%, Ni 6%, Co 6% and Mo 6% are proportioned, the prepared mixed powder is put into a corundum ball-milling tank for ball milling for 24 hours by taking absolute ethyl alcohol as a medium and taking tungsten carbide balls as milling balls, the ball-material ratio is 8:1, and polyvinyl alcohol aqueous solution with the concentration of 3 wt% is added 2 hours before the ball milling is finished; carrying out drying and grinding after ball milling, sieving by a 100-mesh sieve, carrying out dry pressing molding on the sieved powder under the pressure of 300MPa, and keeping the pressure for 2 minutes; putting the pressed compact into a silicon carbide wafer auxiliary heating device, placing the silicon carbide wafer auxiliary heating device into a microwave sintering furnace, vacuumizing the furnace chamber, and then filling nitrogen with the pressure of 0.11 MPa; starting a microwave power supply to heat, heating the sample to 1600 ℃ at the heating rate of 20 ℃/min, preserving heat for 10min, and then cooling along with the furnace. The Vickers hardness of the material is 16.43 +/-0.65 GPa, and the fracture toughness is 7.61 +/-0.94 MPa.m1/2。
Compared with example 3, increasing the content of the binder phase Ni and Co can significantly improve the Vickers hardness and the fracture toughness under the same sintering process.
Example 5:
a titanium carbonitride based composite cermet material and a microwave sintering method thereof are disclosed, which comprises the following steps: mixing 62% of Ti (C, N), 15% of Mo2C 15, 5% of WC, 6% of Ni, 6% of Co and 6% of Mo in percentage by mass, putting the prepared mixed powder into a corundum ball-milling tank for ball milling for 24 hours by taking absolute ethyl alcohol as a medium and taking tungsten carbide balls as milling balls, wherein the ball-material ratio is 8:1, and adding 3 wt% of polyvinyl alcohol aqueous solution 2 hours before the ball milling is finished; carrying out drying and grinding after ball milling, sieving by a 100-mesh sieve, carrying out dry pressing molding on the sieved powder under the pressure of 300MPa, and keeping the pressure for 2 minutes; putting the pressed compact into a silicon carbide wafer auxiliary heating device, placing the silicon carbide wafer auxiliary heating device into a microwave sintering furnace, vacuumizing the furnace chamber, and then filling nitrogen with the pressure of 0.11 MPa; and (3) starting a microwave power supply to heat, heating the sample to 1550 ℃ at the heating rate of 20 ℃/min, preserving heat for 10min, and then cooling along with the furnace. The Vickers hardness of the material is 15.93 +/-0.15 GPa, and the fracture toughness is 6.01 +/-0.92 MPa.m1/2。
Example 6:
a titanium carbonitride based composite cermet material and a microwave sintering method thereof are disclosed, which comprises the following steps: mixing 62% of Ti (C, N), 15% of Mo2C 15, 5% of WC, 6% of Ni, 6% of Co and 6% of Mo in percentage by mass, putting the prepared mixed powder into a corundum ball-milling tank for ball milling for 24 hours by taking absolute ethyl alcohol as a medium and taking tungsten carbide balls as milling balls, wherein the ball-material ratio is 8:1, and adding 3 wt% of polyvinyl alcohol aqueous solution 2 hours before the ball milling is finished; carrying out drying and grinding after ball milling, sieving by a 100-mesh sieve, carrying out dry pressing molding on the sieved powder under the pressure of 300MPa, and keeping the pressure for 2 minutes; putting the pressed compact into a silicon carbide wafer auxiliary heating device, placing the silicon carbide wafer auxiliary heating device into a microwave sintering furnace, vacuumizing the furnace chamber, and then filling nitrogen with the pressure of 0.11 MPa; starting a microwave power supply to heat, heating the sample to 1650 ℃ at a heating rate of 20 ℃/min, and keeping the temperature for 10minAnd then cooled with the furnace. The Vickers hardness of the material is 16.67 plus or minus 0.42GPa, and the fracture toughness is 7.20 plus or minus 1.44MPa.m1/2。
Examples 4-6 illustrate that sintering temperature has an effect on material properties with the same material composition, and that the higher the temperature, the better the overall mechanical properties.
Example 7:
a titanium carbonitride based composite cermet material and a microwave sintering method thereof are disclosed, which comprises the following steps: 62 percent of Ti (C, N) and Mo in percentage by mass2C15%, WC 5%, Ni 6%, Co 6% and Mo 6% are proportioned, the prepared mixed powder is put into a corundum ball-milling tank for ball milling for 24 hours by taking absolute ethyl alcohol as a medium and taking tungsten carbide balls as milling balls, the ball-material ratio is 8:1, and polyvinyl alcohol aqueous solution with the concentration of 3 wt% is added 2 hours before the ball milling is finished; carrying out drying and grinding after ball milling, sieving by a 100-mesh sieve, carrying out dry pressing molding on the sieved powder under the pressure of 300MPa, and keeping the pressure for 2 minutes; putting the pressed compact into a silicon carbide wafer auxiliary heating device, placing the silicon carbide wafer auxiliary heating device into a microwave sintering furnace, vacuumizing the furnace chamber, and then filling nitrogen with the pressure of 0.11 MPa; and (3) starting a microwave power supply to heat, heating the sample to 1600 ℃ at the heating rate of 20 ℃/min, preserving the temperature for 0min, and then cooling along with the furnace. The Vickers hardness of the material is 16.58 +/-0.12 GPa, and the fracture toughness is 6.79 +/-0.24 MPa.m1/2。
Example 8:
a titanium carbonitride based composite cermet material and a microwave sintering method thereof are disclosed, which comprises the following steps: 62 percent of Ti (C, N) and Mo in percentage by mass2C15%, WC 5%, Ni 6%, Co 6% and Mo 6% are proportioned, the prepared mixed powder is put into a corundum ball-milling tank for ball milling for 24 hours by taking absolute ethyl alcohol as a medium and taking tungsten carbide balls as milling balls, the ball-material ratio is 8:1, and polyvinyl alcohol aqueous solution with the concentration of 3 wt% is added 2 hours before the ball milling is finished; carrying out drying and grinding after ball milling, sieving by a 100-mesh sieve, carrying out dry pressing molding on the sieved powder under the pressure of 300MPa, and keeping the pressure for 2 minutes; putting the pressed compact into a silicon carbide wafer auxiliary heating device, placing the silicon carbide wafer auxiliary heating device into a microwave sintering furnace, vacuumizing the furnace chamber, and then filling nitrogen with the pressure of 0.11 MPa; starting a microwave power supply to heat at a temperature of 20 ℃/minHeating the sample to 1600 ℃ at a temperature rate, preserving the heat for 5min, and then cooling along with the furnace. The Vickers hardness of the material is 15.85 +/-0.31 GPa, and the fracture toughness is 9.27 +/-0.82 MPa.m1/2。
Example 9:
a titanium carbonitride based composite cermet material and a microwave sintering method thereof are disclosed, which comprises the following steps: 62 percent of Ti (C, N) and Mo in percentage by mass2C15%, WC 5%, Ni 6%, Co 6% and Mo 6% are proportioned, the prepared mixed powder is put into a corundum ball-milling tank for ball milling for 24 hours by taking absolute ethyl alcohol as a medium and taking tungsten carbide balls as milling balls, the ball-material ratio is 8:1, and polyvinyl alcohol aqueous solution with the concentration of 3 wt% is added 2 hours before the ball milling is finished; carrying out drying and grinding after ball milling, sieving by a 100-mesh sieve, carrying out dry pressing molding on the sieved powder under the pressure of 300MPa, and keeping the pressure for 2 minutes; putting the pressed compact into a silicon carbide wafer auxiliary heating device, placing the silicon carbide wafer auxiliary heating device into a microwave sintering furnace, vacuumizing the furnace chamber, and then filling nitrogen with the pressure of 0.11 MPa; and (3) starting a microwave power supply to heat, heating the sample to 1600 ℃ at the heating rate of 20 ℃/min, preserving the temperature for 20min, and then cooling along with the furnace. The Vickers hardness of the material is 16.25 +/-0.09 GPa, and the fracture toughness is 12.41 +/-0.33 MPa.m1/2。
Examples 7-9 compare to illustrate that incubation at 1600 c for different times has an effect on material properties under the same material composition.
In conclusion, a proper amount of carbide and metal additives are added, and the compactness, hardness and fracture toughness of the metal ceramic can be effectively improved by upgrading the auxiliary heating device and optimizing the sintering temperature and the heat preservation time. The preparation process greatly improves the comprehensive performance of the metal ceramic and enlarges the application range of the material.
Claims (5)
1. The microwave sintering process of the titanium carbonitride-based composite cermet material is characterized in that the titanium carbonitride-based composite cermet material comprises the following components in percentage by weight: 62 to 68 percent of Ti (C, N) and Mo2C15%, WC 5%, Ni 3% -6%, Co 6% -9%, Mo 3% -6%; the method comprises the following steps:
step 1: according to the ratioExample weighing Ti (C, N) and Mo2C. Ball milling and mixing WC, Ni, Co and Mo powder, adding 1-5% concentration polyvinyl alcohol solution 1.5-2.5 hr before ball milling, drying, grinding and sieving;
step 2: pressing and molding the screened powder under the pressure of 100-300MPa to obtain a metal ceramic biscuit (4);
and step 3: in an inert gas atmosphere, a microwave sintering process is adopted, a sample is placed in a silicon carbide wafer auxiliary heating device and placed in a heat preservation box, the temperature is continuously raised to 1550-1650 ℃ at the temperature rise rate of 20-40 ℃/min, the heat preservation is carried out for 5-20 min, and then furnace cooling is carried out, so that the titanium carbonitride based composite metal ceramic material is prepared.
2. The process according to claim 1, wherein in the step (1), the ball milling mixing is to put the weighed powder into a corundum ball milling tank, absolute ethyl alcohol is used as a ball milling medium, and a grinding ball is a tungsten carbide ball.
3. The process according to claim 1, wherein the inert gas in the step (3) is nitrogen, and the nitrogen gas has a pressure in the range of 0.1 to 0.12MPa and is in a flowing state.
4. The process according to claim 1, wherein the auxiliary heating device in the step (3) comprises a silicon carbide ring and two silicon carbide pieces, wherein the silicon carbide ring is sleeved on the periphery of the metal ceramic biscuit (4), and the two silicon carbide pieces are respectively arranged on the upper side and the lower side of the metal ceramic biscuit (4).
5. Process according to claim 4, characterized in that the auxiliary heating means, on which the cermet biscuit (4) is placed, are placed in a crucible, which is placed in a holding tank.
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| CN102115841A (en) * | 2009-12-30 | 2011-07-06 | 常熟市东涛金属复合材料有限公司 | Method for processing metal ceramic composite material |
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| CN102382997B (en) * | 2011-10-24 | 2013-02-27 | 中南大学 | Method for preparing WC-Co cemented carbide through microwave sintering |
| CN102816964A (en) * | 2012-03-30 | 2012-12-12 | 刘昭晖 | Manufacturing method for ultra-fine grain Ti (C, N) based metal ceramic tools |
| CN103695685B (en) * | 2013-12-26 | 2016-02-24 | 昆明理工大学 | A kind of microwave sintering reaction prepares the method for WC-Co hard alloy |
| CN104878267A (en) * | 2015-05-29 | 2015-09-02 | 南京理工大学 | TiCN-base metal ceramic tool material and its microwave sintering process |
| JP6743663B2 (en) * | 2016-11-18 | 2020-08-19 | 日本製鉄株式会社 | Cemented Carbide and Cemented Carbide |
| CN108637268B (en) * | 2018-04-24 | 2021-12-28 | 海南大学 | Method for preparing composite Ti (C, N) metal ceramic powder by microwave carbothermic reduction |
| CN108624772B (en) * | 2018-06-26 | 2020-12-18 | 南京理工大学 | Ultra-fine grain tungsten carbide-based hard alloy material and preparation method thereof |
| CN108950342B (en) * | 2018-07-24 | 2020-09-01 | 三峡大学 | Ti (C, N) -based cermet and preparation method thereof |
| CN109898004A (en) * | 2019-03-20 | 2019-06-18 | 莱芜职业技术学院 | A kind of high tough titanium carbide-high manganese steel bonded carbide and preparation method and application |
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