CN109252081B - High-entropy alloy binding phase superfine tungsten carbide hard alloy and preparation method thereof - Google Patents
High-entropy alloy binding phase superfine tungsten carbide hard alloy and preparation method thereof Download PDFInfo
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- CN109252081B CN109252081B CN201811288722.6A CN201811288722A CN109252081B CN 109252081 B CN109252081 B CN 109252081B CN 201811288722 A CN201811288722 A CN 201811288722A CN 109252081 B CN109252081 B CN 109252081B
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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
- C22C29/06—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 carbides, but not containing other metal compounds
- C22C29/08—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 carbides, but not containing other metal compounds based on tungsten carbide
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- 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
- C22C29/06—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 carbides, but not containing other metal compounds
- C22C29/067—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 carbides, but not containing other metal compounds comprising a particular metallic binder
Abstract
The invention belongs to the technical field of hard alloy, and discloses high-entropy alloy binding phase superfine tungsten carbide hard alloy and a preparation method thereof. The high-entropy alloy bonding phase superfine tungsten carbide hard alloy takes high-entropy alloy as a bonding phase and tungsten carbide as a hard phase; the high-entropy alloy comprises at least five elements of Al, Co, Cr, Cu, Fe and Ni, and the atomic percentage of each element is 5-35%. The method comprises the following steps: and mixing the high-entropy alloy powder with WC powder, and then performing discharge plasma sintering molding to obtain the high-entropy alloy binding phase superfine tungsten carbide hard alloy. The tungsten carbide hard alloy has fine crystal grains and good comprehensive mechanical property; no crystal grain growth inhibitor is needed to be added; obviously reduces the consumption of cobalt and the cost of raw materials.
Description
Technical Field
The invention relates to a high-entropy alloy binding phase superfine tungsten carbide hard alloy and a preparation method thereof, belonging to the technical field of hard alloys.
Background
The hard alloy has high hardness, good high-temperature strength and fracture toughness, and is widely applied to industries such as metal cutting tools, drill bits, drawing dies and the like, thus being praised as 'industrial teeth'. Cemented carbides are produced by powder metallurgy processes from a hard phase that provides the cemented carbide with high hardness and a binder phase that provides it with toughness, and fracture toughness generally decreases with increasing hardness. In order to improve the comprehensive performance of cemented carbide and reduce the cost to meet the demand of industrial development, a great deal of research is carried out on the preparation of ultrafine/nanocrystalline cemented carbide and the development of novel binder phase. Although the preparation of the ultra-fine/nano-crystalline cemented carbide can improve the comprehensive performance of the cemented carbide, the process is complex, and the ultra-fine/nano-crystalline cemented carbide powder rapidly grows during the sintering process so that the ultra-fine/nano-crystalline characteristics are lost, thus a grain growth inhibitor needs to be added. On the other hand, although some new binder phases have been developed, cobalt, which is magnetic and toxic and a strategic resource, remains the most widely used binder phase at present, which is also a significant challenge in preparing new binder phases.
Therefore, in order to further improve the comprehensive mechanical property of the hard alloy and develop a binder phase with excellent performance capable of replacing Co, the invention provides a method for preparing the superfine tungsten carbide hard alloy with good comprehensive mechanical property by using the high-entropy alloy as the binder phase and adopting spark plasma sintering.
Disclosure of Invention
In order to overcome the defects of the existing tungsten carbide hard alloy, the invention aims to provide the superfine tungsten carbide hard alloy with good comprehensive mechanical property and the preparation method thereof.
The binding phase in the high-entropy alloy binding phase superfine tungsten carbide hard alloy is solid-solution high-entropy alloy, and WC is a hard phase. Co element can be partially or completely replaced by adjusting the components and the content thereof in the high-entropy alloy binding phase, so that the cost of raw materials is effectively reduced. The invention utilizes the inhibition effect of the high-entropy alloy on the growth of WC crystal grains, can realize the preparation of the superfine tungsten carbide hard alloy without adding a crystal grain growth inhibitor, and the hard alloy has good comprehensive mechanical properties.
The purpose of the invention is realized by the following technical scheme:
a high-entropy alloy binding phase superfine tungsten carbide hard alloy takes a high-entropy alloy as a binding phase and takes tungsten carbide (WC) as a hard phase;
the high-entropy alloy comprises at least five elements of Al, Co, Cr, Cu, Fe and Ni, and the atomic percentage of each element is 5-35%.
The mass percentage of the high-entropy alloy in the high-entropy alloy binding phase superfine tungsten carbide hard alloy is 5-20%.
The preparation method of the high-entropy alloy binding phase superfine tungsten carbide hard alloy comprises the following steps:
and mixing the high-entropy alloy powder with WC powder, and then performing discharge plasma sintering molding to obtain the high-entropy alloy binding phase superfine tungsten carbide hard alloy. The sintering conditions are as follows: the sintering pressure is more than or equal to 30 MPa; the sintering temperature is 1200-1350 ℃.
The preparation method of the high-entropy alloy binding phase superfine tungsten carbide hard alloy specifically comprises the following steps of (1) preparing high-entropy alloy powder by ball milling
Uniformly mixing Al, Co, Cr, Cu, Fe and Ni powder according to a ratio, and performing ball milling to obtain high-entropy alloy powder; the ball milling is carried out in an inert atmosphere, wherein the inert atmosphere is argon; the ball milling refers to dry milling and then wet milling, and drying is needed after wet milling;
(2) ball milling mixing material
Mixing the high-entropy alloy powder and the WC powder uniformly, ball-milling and sieving to obtain a mixture;
the ball milling is carried out in an inert atmosphere, wherein the inert atmosphere is argon; the ball milling refers to dry milling and then wet milling, and drying is needed after wet milling;
(3) spark plasma sintering forming
Prepressing the mixture obtained in the step (2), then placing the mixture in a discharge plasma sintering furnace for discharge plasma sintering, and cooling to obtain the high-entropy alloy binding phase superfine tungsten carbide hard alloy; the sintering conditions are as follows: the sintering pressure is more than or equal to 30 MPa; the sintering temperature is 1200-1350 ℃.
And the sintering specifically comprises vacuumizing, adjusting sintering pressure, heating to 795-805 ℃, preserving heat, and continuously heating to 1200-1350 ℃ for heat preservation and sintering. And raising the temperature to 795-805 ℃ for heat preservation, preferably raising the temperature to 800 ℃ for heat preservation. The heat preservation time is 1-2 min. The heat preservation sintering time at 1200-1350 ℃ is 3-6 min.
Compared with the prior art, the invention has the following advantages and effects:
(1) according to the high-entropy alloy bonding phase superfine tungsten carbide hard alloy, the high-entropy alloy is used as a bonding phase, Co can be partially or completely replaced by adjusting the components and the content thereof in the high-entropy alloy bonding phase, the Co consumption is reduced while the performance of the hard alloy is ensured, and the raw material cost is effectively reduced.
(2) The high-entropy alloy binding phase superfine tungsten carbide hard alloy provided by the invention adopts the high-entropy alloy as the binding phase, and utilizes the inhibition effect of the high-entropy alloy on the growth of WC grains in the sintering process, so that the superfine WC hard alloy can be obtained without adding a grain growth inhibitor.
(3) The high-entropy alloy binding phase superfine tungsten carbide hard alloy is solidified and formed by adopting a spark plasma sintering process. Because the spark plasma sintering has the advantages of high heating rate, short sintering time, low sintering temperature, high cooling rate and the like, the hard alloy with good density can be obtained by short-time sintering at lower sintering temperature, the growth of WC crystal grains in the sintering process can be obviously inhibited, and the comprehensive mechanical property of the hard alloy is effectively improved.
(4) According to the high-entropy alloy binding phase superfine tungsten carbide hard alloy, when 10 mass percent of AlCoCrCuFeNi high-entropy alloy is used as a binding phase, under the process conditions that the sintering pressure is 30MPa, the sintering temperature is 1250 ℃ and the sintering time is 5 minutes, the WC average grain size of the hard alloy is 238nm, and the Vickers hardness is 1922HV30The fracture toughness is 10.41MPa m1/2. Replacing the binding phase with 10% Al under the same process conditions0.5The WC average grain size of the CoCrCuFeNi high-entropy alloy and the hard alloy is 223nm, the Vickers hardness is 2070HV30Fracture toughness of 10.27MPam1/2。
Drawings
FIG. 1 is an X-ray diffraction pattern of a high-entropy alloy binder phase-based ultrafine tungsten carbide cemented carbide obtained in example 1;
FIG. 2 is a scanning electron microscope image of the high-entropy alloy binder phase-based ultrafine tungsten carbide cemented carbide obtained in example 1.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
A preparation method of high-entropy alloy binding phase superfine tungsten carbide hard alloy comprises the following steps:
1) weighing Al, Co, Cr, Cu, Fe and Ni powder with the purity of more than 99.9 percent and the average grain diameter of less than 45 mu m according to the molar ratio of 1:1:1:1:1, uniformly mixing, putting into a hard alloy ball milling tank, filling into hard alloy grinding balls according to the ball-to-material ratio of 10:1, vacuumizing the ball milling tank, and filling high-purity argon; then carrying out dry milling for 40 hours at the rotating speed of 300 revolutions per minute, and then carrying out wet milling for 2 hours (the wet milling medium is ethanol) to obtain high-entropy alloy powder; after the ball milling process is finished, putting the high-entropy alloy powder into a vacuum drying oven, drying for 48 hours at the temperature of 70 ℃, sieving by a No. 300 sample sieve, and granulating;
2) placing 15g of the high-entropy alloy powder obtained in the step 1) and 135g of WC powder with purity of more than 99.5% and average particle size of 0.8 μm into a tank, mixing the materials on a powder mixer for 5 hours, then carrying out dry grinding for 30 hours under the protection of argon gas, and then carrying out wet grinding for 2 hours; wherein the ball-material ratio during ball milling is 5:1, the wet milling medium is ethanol, and the rotation speed of the ball milling is 300 r/min; after the ball milling process is finished, putting the mixed powder into a vacuum drying oven for drying, sieving by a 100# sample sieve, and granulating to obtain mixed powder;
3) loading 25g of the mixed powder obtained in the step 2) into a die cavity with a graphite die diameter of 20mm, primarily pressing the mixed powder into a sample, loading the sample into a discharge plasma sintering furnace, pumping the sample until the vacuum is less than 10Pa, adjusting the sintering pressure to 30MPa, then heating to 800 ℃ at a heating rate of 100 ℃/min, keeping the temperature for 2 minutes, facilitating the release of gas adsorbed in the powder, heating to 1250 ℃ (heating rate of 100 ℃/min), keeping the temperature for 5 minutes, and finally cooling to 100 ℃ along with the furnace to obtain the WC with the average grain size of 238nm and the Vickers hardness of 1922HV30The fracture toughness is 10.41MPa m1/2The superfine tungsten carbide hard alloy based on the high-entropy alloy binding phase. FIG. 1 is an X-ray diffraction pattern of a high-entropy alloy binder phase-based ultrafine tungsten carbide cemented carbide obtained in example 1; FIG. 2 is a scanning electron microscope image of the high-entropy alloy binder phase-based ultrafine tungsten carbide cemented carbide obtained in example 1.
Example 2
A preparation method of high-entropy alloy binding phase superfine tungsten carbide hard alloy comprises the following steps:
1) weighing Al, Co, Cr, Cu, Fe and Ni powder with the purity of more than 99.9 percent and the average grain diameter of less than 45 mu m according to the molar ratio of 1:1:1:1:1, uniformly mixing, putting into a hard alloy ball milling tank, filling into hard alloy grinding balls according to the ball-to-material ratio of 10:1, vacuumizing the ball milling tank, and filling high-purity argon; then carrying out dry milling for 40 hours at the rotating speed of 300 revolutions per minute, and then carrying out wet milling for 2 hours (the wet milling medium is ethanol) to obtain high-entropy alloy powder; after the ball milling process is finished, putting the high-entropy alloy powder into a vacuum drying oven, drying for 48 hours at the temperature of 70 ℃, sieving by a No. 300 sample sieve, and granulating;
2) placing 7.5g of the high-entropy alloy powder obtained in the step 1) and 142.5g of WC powder with purity of more than 99.5% and average particle size of 0.8 μm into a tank, mixing the mixture on a powder mixer for 5 hours, then carrying out dry grinding for 30 hours under the protection of argon gas, and then carrying out wet grinding for 2 hours; wherein the ball-material ratio during ball milling is 5:1, the wet milling medium is ethanol, and the rotation speed of the ball milling is 300 r/min; after the ball milling process is finished, putting the mixed powder into a vacuum drying oven for drying, sieving by a 100# sample sieve, and granulating to obtain mixed powder;
3) weighing 25g of the mixed powder in the step 2), and filling the mixed powder into a die cavity with the diameter of 20mm of a graphite die to preliminarily press the mixed powder into a sample; putting the sample into a discharge plasma sintering furnace, pumping to vacuum of less than 10Pa, adjusting sintering pressure to 30MPa, heating to 800 ℃ at a heating rate of 100 ℃/min, keeping the temperature for 2 minutes, facilitating the release of gas adsorbed in the powder, heating to 1250 ℃ (heating rate of 100 ℃/min), keeping the temperature for 5 minutes, and finally cooling to 100 ℃ along with the furnace to obtain WC with the average grain size of 256nm and Vickers hardness of 2033HV30The fracture toughness is 9.71MPa m1/2The superfine tungsten carbide hard alloy based on the high-entropy alloy binding phase.
Example 3
A preparation method of high-entropy alloy binding phase superfine tungsten carbide hard alloy comprises the following steps:
1) weighing Al, Co, Cr, Cu, Fe and Ni powder with the purity of more than 99.9 percent and the average grain diameter of less than 45 mu m according to the molar ratio of 0.5:1:1:1:1, uniformly mixing, putting into a hard alloy ball milling tank, putting into hard alloy grinding balls according to the ball-to-material ratio of 10:1, vacuumizing the ball milling tank, and filling high-purity argon; then carrying out dry milling for 40 hours at the rotating speed of 300 revolutions per minute, and then carrying out wet milling for 2 hours (the wet milling medium is ethanol) to obtain high-entropy alloy powder; after the ball milling process is finished, putting the high-entropy alloy powder into a vacuum drying oven, drying for 48 hours at the temperature of 70 ℃, sieving by a No. 300 sample sieve, and granulating;
2) placing 15g of the high-entropy alloy powder obtained in the step 1) and 135g of WC powder with purity of more than 99.5% and average particle size of 0.8 μm into a tank, mixing the materials on a powder mixer for 5 hours, then carrying out dry grinding for 30 hours under the protection of argon gas, and then carrying out wet grinding for 2 hours; wherein the ball-material ratio during ball milling is 5:1, the wet milling medium is ethanol, and the rotation speed of the ball milling is 300 r/min; after the ball milling process is finished, putting the mixed powder into a vacuum drying oven for drying, sieving by a 100# sample sieve, and granulating to obtain mixed powder;
3) weighing 25g of the mixed powder obtained in the step 2), placing the mixed powder into a die cavity with the diameter of 20mm of a graphite die, primarily pressing the mixed powder into a sample, placing the sample into a discharge plasma sintering furnace, pumping the sample until the vacuum is less than 10Pa, adjusting the sintering pressure to 30MPa, then heating the mixed powder to 800 ℃ at the heating rate of 100 ℃/min, preserving the heat for 2 minutes to facilitate the release of gas adsorbed in the powder, heating the mixed powder to 1250 ℃ (the heating rate is 100 ℃/min), preserving the heat for 5 minutes, and finally cooling the mixed powder to 100 ℃ along with the furnace to obtain the WC average grain size of 223nm, the Vickers hardness of 2070HV30The fracture toughness is 10.27MPa m1/2The superfine tungsten carbide hard alloy based on the high-entropy alloy binding phase.
Example 4
A preparation method of high-entropy alloy binding phase superfine tungsten carbide hard alloy comprises the following steps:
1) al, Co, Cr, Cu, Fe and Ni powder with the purity of more than 99.9 percent and the average grain diameter of less than 45 mu m are mixed according to the mol ratio of 1.5: weighing according to the ratio of 1:1:1:1:1, uniformly mixing, putting into a hard alloy ball milling tank, filling into hard alloy grinding balls according to the ball-to-material ratio of 10:1, vacuumizing the ball milling tank, and filling high-purity argon. Then carrying out dry milling for 40 hours at the rotating speed of 300 revolutions per minute, and then carrying out wet milling for 2 hours (the wet milling medium is ethanol) to obtain high-entropy alloy powder; after the ball milling process is finished, putting the high-entropy alloy powder into a vacuum drying oven, drying for 48 hours at the temperature of 70 ℃, sieving by a No. 300 sample sieve, and granulating;
2) placing 15g of the high-entropy alloy powder obtained in the step 1) and 135g of WC powder with purity of more than 99.5% and average particle size of 0.8 μm into a tank, mixing the materials on a powder mixer for 5 hours, then carrying out dry grinding for 30 hours under the protection of argon gas, and then carrying out wet grinding for 2 hours; wherein the ball-material ratio during ball milling is 5:1, the wet milling medium is ethanol, and the rotation speed of the ball milling is 300 r/min; after the ball milling process is finished, putting the mixed powder into a vacuum drying oven for drying, sieving by a 100# sample sieve, and granulating to obtain mixed powder;
3) weighing 25g of the mixed powder in the step 2), and filling the mixed powder into a die cavity with the diameter of 20mm of a graphite die to preliminarily press the mixed powder into a sample; putting the sample into a discharge plasma sintering furnace, pumping to vacuum of less than 10Pa, adjusting sintering pressure to 30MPa, heating to 800 ℃ at a heating rate of 100 ℃/min, keeping the temperature for 2 minutes, facilitating the release of gas adsorbed in the powder, heating to 1250 ℃ (heating rate of 100 ℃/min), keeping the temperature for 5 minutes, and finally cooling to 100 ℃ along with the furnace to obtain WC with average grain size of 238nm and Vickers hardness of 2127HV30The fracture toughness is 9.89MPa m1/2The superfine tungsten carbide hard alloy based on the high-entropy alloy binding phase.
Comparative example
A preparation method of tungsten carbide hard alloy comprises the following steps:
1) weighing 15g of Co powder with the purity of more than 99.9 percent and the average grain diameter of less than 45 mu m and 135g of WC powder with the purity of more than 99.5 percent and the average grain diameter of 0.8 mu m, putting the Co powder and the WC powder into a tank, mixing the mixture on a powder mixer for 5 hours, then carrying out dry grinding for 30 hours under the protection of argon gas, and then carrying out wet grinding for 2 hours; wherein the ball-material ratio is 5:1, the wet grinding medium is ethanol, and the rotation speed of ball milling is 300 r/min; after the ball milling process is finished, putting the mixed powder into a vacuum drying oven for drying, sieving by a 100# sample sieve, and granulating to obtain mixed powder;
2) weighing 25g of the mixed powder obtained in the step 1), and filling the mixed powder into a mold cavity with the diameter of 20mm of a graphite mold for preliminary pressing to obtain a sample. Putting the sample into a discharge plasma sintering furnace, pumping to vacuum of less than 10Pa, adjusting sintering pressure to 30MPa, heating to 800 ℃ at a heating rate of 100 ℃/min, keeping the temperature for 2 minutes, facilitating the release of gas adsorbed in the powder, heating to 1250 ℃ (heating rate of 100 ℃/min), keeping the temperature for 5 minutes, cooling to 100 ℃ along with the furnace to obtain WC average crystal grain size of 536nm and Vickers hardness of 1736HV30The fracture toughness is 12.99MPa m1/2WC-Co cemented carbide of (1).
Under the same technological parameters, the WC average grain size of the WC-Co hard alloy is obviously larger than that of the superfine tungsten carbide hard alloy of the high-entropy alloy binding phase, and the Vickers hardness HV of the WC-Co hard alloy is30Obviously lower than the Vickers hardness of the superfine tungsten carbide hard alloy of the high-entropy alloy binding phase, but the fracture toughness of the superfine tungsten carbide hard alloy is higher than that of the superfine tungsten carbide hard alloy of the high-entropy alloy binding phase. Meanwhile, the comprehensive mechanical property of the superfine tungsten carbide hard alloy of the high-entropy alloy binding phase is superior to that of commercial WC-CO hard alloy with the same granularity, such as WC-Co hard alloy with the Chen et al report mark of EF05 and the Vickers hardness and the fracture toughness of the WC-Co hard alloy are 1900HV30，9.1MPa m1/2。
Claims (5)
1. A preparation method of high-entropy alloy binding phase superfine tungsten carbide hard alloy is characterized by comprising the following steps: the method comprises the following steps:
mixing the high-entropy alloy powder and WC powder, and then performing discharge plasma sintering molding to obtain the high-entropy alloy binding phase superfine tungsten carbide hard alloy;
the sintering specifically comprises vacuumizing, adjusting sintering pressure, heating to 795-805 ℃, preserving heat, and continuously heating to 1200-1350 ℃ for heat preservation sintering; the sintering pressure is more than or equal to 30 MPa; the heat preservation time is 1-2 min; the sintering time at 1200-1350 ℃ is 3-6 min;
the high-entropy alloy binding phase superfine tungsten carbide hard alloy takes the high-entropy alloy as a binding phase and takes tungsten carbide as a hard phase; the high-entropy alloy comprises at least five elements of Al, Co, Cr, Cu, Fe and Ni, and the atomic percentage of each element is 5-35%.
2. The preparation method of the high-entropy alloy binding phase superfine tungsten carbide hard alloy according to claim 1, is characterized in that: and raising the temperature to 795-805 ℃ and preserving the heat, namely raising the temperature to 800 ℃.
3. The preparation method of the high-entropy alloy binding phase superfine tungsten carbide hard alloy according to claim 1, is characterized in that: the mass percentage of the high-entropy alloy in the high-entropy alloy binding phase superfine tungsten carbide hard alloy is 5-20%.
4. The preparation method of the high-entropy alloy binder phase superfine tungsten carbide hard alloy according to any one of claims 1 to 3, characterized by comprising the following steps: the method specifically comprises the following steps:
(1) ball milling preparation of high-entropy alloy powder
Uniformly mixing Al, Co, Cr, Cu, Fe and Ni powder according to a ratio, and performing ball milling to obtain high-entropy alloy powder; the ball milling is carried out in an inert atmosphere;
(2) ball milling mixing material
Mixing the high-entropy alloy powder and the WC powder uniformly, ball-milling and sieving to obtain a mixture; the ball milling is carried out in an inert atmosphere;
(3) spark plasma sintering forming
And (3) prepressing the mixture obtained in the step (2), then placing the mixture in a spark plasma sintering furnace for spark plasma sintering, and cooling to obtain the high-entropy alloy binding phase superfine tungsten carbide hard alloy.
5. The preparation method of the high-entropy alloy binding phase superfine tungsten carbide hard alloy according to claim 4, is characterized in that: the inert atmosphere in the step (1) is argon; the ball milling refers to dry milling and then wet milling, and drying is needed after wet milling;
the inert atmosphere in the step (2) is argon; the ball milling means dry milling and then wet milling, and drying is needed after wet milling.
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