CN108624772B - Ultra-fine grain tungsten carbide-based hard alloy material and preparation method thereof - Google Patents
Ultra-fine grain tungsten carbide-based hard alloy material and preparation method thereof Download PDFInfo
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- CN108624772B CN108624772B CN201810671837.7A CN201810671837A CN108624772B CN 108624772 B CN108624772 B CN 108624772B CN 201810671837 A CN201810671837 A CN 201810671837A CN 108624772 B CN108624772 B CN 108624772B
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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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- 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
- C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
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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
Abstract
The invention discloses an ultra-fine grain tungsten carbide-based hard alloy material and a preparation method thereof. The ultra-fine grain tungsten carbide-based hard alloy comprises the following components in percentage by weight8 percent of cobalt, 90.2 to 90.8 percent of tungsten carbide, 0.2 to 0.8 percent of vanadium carbide and 1 percent of cubic boron nitride. The method adopts a discharge plasma sintering technology, continuously heats up to 1250-1300 ℃ at a heating rate of 100 +/-20 ℃/min under the protection of vacuum atmosphere, and controls the pressure to be 30 +/-2 Mpa, so as to prepare the ultra-fine grain tungsten carbide-based hard alloy. The hard alloy of the invention not only has higher hardness, but also has good toughness, the sample with the highest comprehensive performance has the hardness of 20.17 +/-0.20 GPa, and the fracture toughness of 12.18 +/-0.2 MPa.m1/2Compared with the current commercial YG8 hard alloy, the hardness is improved by 10-20%, and the fracture toughness is improved by 10-18%.
Description
Technical Field
The invention belongs to the technical field of Spark Plasma Sintering (SPS) materials, and relates to an ultrafine grain tungsten carbide-based hard alloy material and a preparation method thereof.
Background
The tungsten carbide (WC) based hard alloy material is a material with high hardness, high wear resistance and corrosion resistance, is suitable for the working conditions with severe environments such as high temperature, friction, heavy load and the like, and is also used in the fields of aerospace parts, bearings, high-speed cutting tools and the like. When the grain size is reduced to submicron size, the strength, hardness, toughness and wear resistance of the hard alloy material are all improved in a larger range. The ultrafine grain hard alloy with the size of 0.1-0.6 mu m has higher hardness and wear resistance, simultaneously has good toughness and has wider application prospect. At present, the traditional sintering process of WC-based hard alloy mainly comprises the following steps: reaction sintering, pressureless sintering, air pressure sintering, hot pressing sintering and hot isostatic pressing sintering. However, conventional sintering has many disadvantages: 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.
The SPS sintering technology is an economic, energy-saving, efficient and environment-friendly sintering mode, and has the advantages of high temperature rise and fall rate, sintering temperature reduction, particle surface purification, density improvement, short heat preservation time and the like. The application of SPS sintering technology to the field of ceramic material preparation has become a hot topic in recent years, and in the case of WC-based hard alloyAt present, a lot of public reports are available. Document 1(S.G.Huang, K.Vanmensel, Tailored sintered of VC-doped WC-Co segmented carbide by pulsed electric current sintered ceramic, Int J Refract Mater Hard Mater.26(2008) 256- & lt262.) prepares WC +12 wt.% Co +0.9 wt.% VC Hard alloy, adopts SPS technology to keep the temperature at 1240 ℃ for 2min, and the hardness of the Hard alloy is 17.3GPa, and the fracture toughness is 9.1MPa.m1/2The grain size was 0.17 μm, but the hardness and fracture toughness of the cemented carbide were low. Reference 2(Lan Sun, Chengchangjia, Effects of Cr3C2addition on the condensation, gradingrowth and properties of ultra fine WC-11 Co composition by spark plasma sintering, Int J Refract MaterHard Mater.26(2008)357 and 361.) preparation of WC +11 wt.% Co +0.6 wt.% Cr3C2The hard alloy is insulated for 5min at 1200 ℃ by adopting SPS technology, the density of the prepared material is 98.4 percent, the hardness is about 18GPa, and the fracture toughness is 13.MPa.m1/2Left and right. The prepared material has better toughness but reduced hardness due to the addition of more Co. In document 3(XIAO Dai-hong, HE Yue-hui, Effect of VC and NbC additives on microstructure and properties of ultra WC-10Co segmented carbides, trans. Nonforrus Met. Soc. China.19(2009)1520 152), the addition of the inhibitor is found to be capable of effectively refining grains, wherein the inhibition Effect of VC is the best. However, the simultaneous addition of the two components results in performance degradation.
From the above, the sintering process of the existing hard alloy is still not perfect, the performance difference of the prepared material is large, and in the existing report, a large amount of binder phase is usually added when the SPS is a hard alloy with high toughness which is wanted to be sintered, which inevitably causes the reduction of the hardness, and the preparation of the material with high hardness and high toughness under the low cobalt state is less. Therefore, the research and the improvement of the SPS sintering process of the hard alloy are carried out, and the optimization of the content of the inhibitor and the reinforced phase has great significance for improving the mechanical property of the hard alloy and promoting the industrialization of the hard alloy.
Disclosure of Invention
The invention aims to provide an ultra-fine grain tungsten carbide-based hard alloy material and a preparation method thereof. The material is prepared by adding a proper amount of inhibitor (vanadium carbide) and reinforcing phase (cubic boron nitride) into a tungsten carbide matrix, and controlling the proportion of the inhibitor and the reinforcing phase to ensure that the material has high hardness and excellent mechanical properties of high toughness.
The technical scheme for realizing the purpose of the invention is as follows:
the ultra-fine grain tungsten carbide-based hard alloy material comprises the following components in percentage by weight: 8 percent of cobalt (Co), 90.2 to 90.8 percent of tungsten carbide (WC), 0.2 to 0.8 percent of Vanadium Carbide (VC) and 1 percent of cubic boron nitride (cBN).
Furthermore, the invention also provides a preparation method of the ultrafine-grained tungsten carbide-based hard alloy material, which adopts an efficient and energy-saving sintering technology, realizes the preparation of the hard alloy material with higher comprehensive mechanical properties in a short time by optimizing the technological parameters such as sintering temperature, heat preservation time and the like, and comprises the following steps:
step 1, weighing Co, WC, VC and cBN powder according to a proportion, mixing, and performing ultrasonic oscillation, stirring and powder mixing at room temperature by taking absolute ethyl alcohol as an oscillation medium;
step 2, drying, grinding and sieving the mixed powder;
step 3, directly pouring the sieved powder into a mold for prepressing;
and 4, adopting a discharge plasma sintering process in a vacuum environment, continuously heating to 1250-1300 ℃ at the heating rate of 100 +/-20 ℃/min, controlling the pressure to be 30 +/-2 Mpa, preserving heat, and then cooling along with a furnace to prepare the ultrafine-grained tungsten carbide-based hard alloy.
In the step 1, the oscillation mixing time is 2-3 hours.
In the step 2, the drying temperature is 100-120 ℃, and the mesh number of the screen is 100 meshes.
In the step 3, the pre-pressing pressure is 10-30 Mpa, and the pressure maintaining time is 2-4 min.
And 4, vacuumizing to 5-8 pa to form a vacuum environment, and keeping the temperature for 4-6 min, preferably 5 min.
Compared with the prior art, the invention has the following remarkable advantages:
(1) compared with the hard alloy on the market, the grain is finer, the grain size is kept at 238-248 nm, and the grain is ultrafine grain hard alloy;
(2) the ultra-fine grain hard alloy prepared by adopting the SPS sintering technology has excellent mechanical property and microstructure through the synergistic effect of the inhibitor and the reinforcing phase, wherein the sample with the highest comprehensive performance has the hardness of 20.17 +/-0.20 GPa and the fracture toughness of 12.18 +/-0.02 MPa.m1/2Compared with the current commercial YG8 hard alloy, the hardness is improved by 10-20%, and the fracture toughness is improved by 10-18%.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
Mixing the components according to the mass percentages of Co 8%, WC 90.8%, VC 0.2% and cBN 1%, placing the mixture into a boronized conical flask by taking absolute ethyl alcohol as a medium, vibrating and stirring for 2 hours, and adding clean water in due time in the vibrating process to ensure that the water temperature is always at room temperature; vibrating, mixing, drying, grinding, sieving with a 100-mesh sieve, directly adding the prepared mixed powder into a graphite mold, and maintaining the pressure at 10MPa for 3 minutes; putting the pre-pressed green compact into a heat preservation device, placing the heat preservation device in a discharge plasma sintering furnace, vacuumizing the furnace chamber to 6pa, and applying pressure of 30 Mpa; heating the sample to 1300 ℃ at the heating rate of 100 ℃/min, preserving the heat for 5min, and then cooling along with the furnace. The test shows that the density is 98.3 percent of the material, the Vickers hardness is 20.17 +/-0.2 GPa, and the fracture toughness is 12.18 +/-0.2 MPa.m1/2Average grain size 246 nm.
Example 2
Mixing the materials according to the mass percentages of Co 8%, WC 90.5%, VC 0.5% and cBN 1%, placing the mixture into a boronized conical flask by taking absolute ethyl alcohol as a medium, vibrating and stirring for 2 hours, and adding clean water in due time in the vibrating process to ensure that the water temperature is always at room temperature; vibrating, mixing, drying, grinding, sieving with 100 mesh sieve, adding the prepared mixed powder into graphite mold, and maintaining pressure at 10MPa3 minutes; putting the pre-pressed green compact into a heat preservation device, placing the heat preservation device in a discharge plasma sintering furnace, vacuumizing the furnace chamber to 6pa, and applying pressure of 30 Mpa; heating the sample to 1300 ℃ at the heating rate of 100 ℃/min, preserving the heat for 5min, and then cooling along with the furnace. The test shows that the density is 97.4 percent of the material, the Vickers hardness is 19.86 +/-0.2 GPa, and the fracture toughness is 10.62 +/-0.2 MPa1/2Average grain size 241 nm.
Example 3
Mixing the components according to the mass percentages of Co 8%, WC 90.2%, VC 0.8% and cBN 1%, placing the mixture into a boronized conical flask by taking absolute ethyl alcohol as a medium, vibrating and stirring for 2 hours, and adding clean water in due time in the vibrating process to ensure that the water temperature is always at room temperature; vibrating, mixing, drying, grinding, sieving with a 100-mesh sieve, directly adding the prepared mixed powder into a graphite mold, and maintaining the pressure at 10MPa for 3 minutes; putting the pre-pressed green compact into a heat preservation device, placing the heat preservation device in a discharge plasma sintering furnace, vacuumizing the furnace chamber to 6pa, and applying pressure of 30 Mpa; heating the sample to 1300 ℃ at the heating rate of 100 ℃/min, preserving the heat for 5min, and then cooling along with the furnace. The test shows that the density is 96.8 percent of the material, the Vickers hardness is 20.48 +/-0.15 GPa, and the fracture toughness is 10.78 +/-0.1 MPa.m1/2Average grain size 238 nm.
Example 4
Mixing the components according to the mass percentages of Co 8%, WC 90.8%, VC 0.2% and cBN 1%, placing the mixture into a boronized conical flask by taking absolute ethyl alcohol as a medium, vibrating and stirring for 2 hours, and adding clean water in due time in the vibrating process to ensure that the water temperature is always at room temperature; vibrating, mixing, drying, grinding, sieving with a 100-mesh sieve, directly adding the prepared mixed powder into a graphite mold, and maintaining the pressure at 10MPa for 3 minutes; putting the pre-pressed green compact into a heat preservation device, placing the heat preservation device in a discharge plasma sintering furnace, vacuumizing the furnace chamber to 6pa, and applying pressure of 28 Mpa; heating the sample to 1250 ℃ at the heating rate of 80 ℃/min, preserving heat for 5min, and then cooling along with the furnace. The test shows that the density is 98.2 percent of the material, the Vickers hardness is 19.99 +/-0.2 GPa, and the fracture toughness is 11.99 +/-0.1 MPa.m1/2Average grain size 244 nm.
Example 5
Mixing the components according to the mass percentages of Co 8%, WC 90.2%, VC 0.8% and cBN 1%, placing the mixture into a boronized conical flask by taking absolute ethyl alcohol as a medium, vibrating and stirring for 2 hours, and adding clean water in due time in the vibrating process to ensure that the water temperature is always at room temperature; vibrating, mixing, drying, grinding, sieving with a 100-mesh sieve, directly adding the prepared mixed powder into a graphite mold, and maintaining the pressure at 30MPa for 3 minutes; putting the pre-pressed green compact into a heat preservation device, placing the heat preservation device in a discharge plasma sintering furnace, vacuumizing the furnace chamber to 6pa, and applying pressure to 32 Mpa; heating the sample to 1300 ℃ at the heating rate of 120 ℃/min, preserving the heat for 5min, and then cooling along with the furnace. The test shows that the density is 97.3 percent of the material, the Vickers hardness is 19.93 +/-0.2 GPa, and the fracture toughness is 10.95 +/-0.1 MPa.m1/2Average grain size 235 nm.
Comparative example 1
Mixing the components according to the mass percentages of Co 8%, WC 82.8%, VC 0.2% and cBN 9%, placing the mixture into a boronized conical flask by taking absolute ethyl alcohol as a medium, oscillating and stirring for 2 hours, and adding clean water in due time in the oscillating process to ensure that the water temperature is always at room temperature; vibrating, mixing, drying, grinding, sieving with a 100-mesh sieve, directly adding the prepared mixed powder into a graphite mold, and maintaining the pressure at 10MPa for 3 minutes; putting the pre-pressed green compact into a heat preservation device, placing the heat preservation device in a discharge plasma sintering furnace, vacuumizing the furnace chamber to 6pa, and applying pressure of 28 Mpa; heating the sample to 1250 ℃ at the heating rate of 80 ℃/min, preserving heat for 5min, and then cooling along with the furnace. The test shows that the density is 90.0 percent of the material, the Vickers hardness is 10.74 +/-0.15 GPa, and the fracture toughness is 9.8 +/-0.1 MPa.m1/2Average grain size 240 nm.
This comparative example illustrates that excessive cBN causes the degree of densification of the cemented carbide to decrease rapidly, and that both hardness and toughness become so poor due to the presence of a large number of pores in the material.
Comparative example 2
Mixing the materials according to the mass percentages of Co 8%, WC 82%, VC 1% and cBN 1%, placing the mixture into a boronized conical flask by taking absolute ethyl alcohol as a medium, oscillating and stirring for 2 hours, and adding clean water in a proper time during the oscillating process to ensure that the water temperature is always at room temperature; vibrating, mixing, drying, grinding, sieving with a 100-mesh sieve, directly adding the prepared mixed powder into a graphite mold, and maintaining the pressure at 10MPa for 3 minutes; putting the pre-pressed green compact into a heat preservation device, placing the heat preservation device in a discharge plasma sintering furnace, vacuumizing the furnace chamber to 6pa, and applying pressure to 32 Mpa; heating the sample to 1300 ℃ at the heating rate of 120 ℃/min, preserving the heat for 5min, and then cooling along with the furnace. The test shows that the density is 92.8 percent of the material, the Vickers hardness is 18.3 +/-0.25 GPa, the fracture toughness is 8.0 +/-0.2 MPa.m1/2, and the average grain size is 243 nm.
This comparative example illustrates that excess VC results in a reduction in the densification of the cemented carbide due to the presence of a large number of pores in the material, resulting in a reduction in hardness and toughness.
Claims (2)
1. The preparation method of the ultrafine-grained tungsten carbide-based hard alloy material is characterized by comprising the following steps of:
step 1, weighing cobalt, tungsten carbide, vanadium carbide and cubic boron nitride powder according to the proportion of 8% of cobalt, 90.2% -90.8% of tungsten carbide, 0.2% -0.8% of vanadium carbide and 1% of cubic boron nitride in percentage by weight, mixing, and performing ultrasonic oscillation, stirring and powder mixing at room temperature by taking absolute ethyl alcohol as an oscillation medium, wherein the oscillation mixing time is 2-3 hours;
step 2, drying, grinding and sieving the mixed powder, wherein the drying temperature is 100-120 ℃, and the mesh number of a screen is 100 meshes;
step 3, directly pouring the sieved powder into a mold, and pre-pressing, wherein the pre-pressing pressure is 10-30 MPa, and the pressure maintaining time is 2-4 min;
and 4, adopting a discharge plasma sintering process in a vacuum environment, continuously heating to 1250-1300 ℃ at the heating rate of 100 +/-20 ℃/min, controlling the pressure to be 30 +/-2 MPa, preserving the heat, and then cooling along with the furnace to prepare the ultrafine-grained tungsten carbide-based hard alloy.
2. The method for preparing an ultra-fine grained tungsten carbide-based hard alloy material according to claim 1, wherein in step 4, a vacuum environment is formed by vacuumizing to 5-8 Pa, and the heat preservation time is 4-6 min.
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| CN110157969B (en) * | 2019-07-10 | 2021-07-27 | 合肥工业大学 | Preparation method of ultra-coarse tungsten carbide hard alloy containing trace cobalt |
| CN110253028A (en) * | 2019-07-16 | 2019-09-20 | 湖南伊澍智能制造有限公司 | A kind of self-lubricating 3D printing alloy powder and preparation method thereof |
| CN111088450B (en) * | 2020-01-07 | 2021-06-11 | 北京科技大学 | Rare earth-added ultrafine-grained high-toughness WC-10Co hard alloy material and preparation method thereof |
| CN113059157B (en) * | 2021-03-09 | 2022-11-25 | 南京理工大学 | Method for sintering superfine crystal WC-based hard alloy special-shaped cutter under SPS pressure |
| FR3120636A1 (en) | 2021-03-15 | 2022-09-16 | Sintermat | Method for manufacturing tungsten carbide parts and material obtained based on SPS sintering of tungsten carbide |
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