CN113061764A - Tungsten carbide-based hard alloy and preparation method thereof - Google Patents
Tungsten carbide-based hard alloy and preparation method thereof Download PDFInfo
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- CN113061764A CN113061764A CN202110279195.8A CN202110279195A CN113061764A CN 113061764 A CN113061764 A CN 113061764A CN 202110279195 A CN202110279195 A CN 202110279195A CN 113061764 A CN113061764 A CN 113061764A
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- 239000000956 alloy Substances 0.000 title claims abstract description 97
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 97
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 136
- 238000000498 ball milling Methods 0.000 claims abstract description 82
- 239000011812 mixed powder Substances 0.000 claims abstract description 40
- 239000000843 powder Substances 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 33
- 239000011268 mixed slurry Substances 0.000 claims abstract description 28
- 238000002156 mixing Methods 0.000 claims abstract description 28
- 238000000748 compression moulding Methods 0.000 claims abstract description 25
- 239000006229 carbon black Substances 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 38
- 238000009694 cold isostatic pressing Methods 0.000 claims description 23
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 229910003470 tongbaite Inorganic materials 0.000 claims description 4
- 239000011230 binding agent Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims description 2
- 239000010959 steel Substances 0.000 claims description 2
- 238000007873 sieving Methods 0.000 abstract description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 20
- 229910052786 argon Inorganic materials 0.000 description 10
- 238000000713 high-energy ball milling Methods 0.000 description 10
- 238000007796 conventional method Methods 0.000 description 5
- 238000007723 die pressing method Methods 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 229910017052 cobalt Inorganic materials 0.000 description 3
- 239000010941 cobalt Substances 0.000 description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 239000007888 film coating Substances 0.000 description 3
- 238000009501 film coating Methods 0.000 description 3
- 230000008676 import Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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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
-
- 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
- C22C29/06—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
-
- 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
- C22C29/06—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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a tungsten carbide-based hard alloy and a preparation method thereof, wherein the method comprises the following steps: according to the mass parts, 500 parts of WC mixed powder, 0-2 parts of carbon black, 1500-3000 parts of alloy balls and 80-250 parts of ball-milling medium are subjected to ball-milling mixing treatment to prepare mixed slurry, wherein the WC mixed powder comprises 0-1.5% of Cr by mass3C2VC or TiC with the mass percent of 0-2% and Co or Ni with the mass percent of 0-1.5%; mixing the mixed slurry with wax, drying and sieving to obtain non-low-viscosity phase powder; putting the powder with no/low-viscosity phase into a mould for compression molding to prepare a pre-processed blank; and sintering the pre-treated blank to obtain the tungsten carbide-based hard alloy. The tungsten carbide-based hard alloy prepared by the method has the advantages of high hardness, high temperature resistance, stable performance and the like.
Description
Technical Field
The invention relates to a tungsten carbide-based hard alloy and a preparation method thereof, belonging to the technical field of alloys.
Background
At present, tungsten carbide-based hard alloys produced in the market are mainly prepared by conventional methods such as hydrogen sintering, negative pressure sintering, hot isostatic pressing sintering (low pressure) and the like, but the hard alloys prepared by the conventional methods have relatively high cobalt content (more than or equal to 1.5 percent), and the hardness and wear resistance of alloy parts can be influenced due to the increase of the cobalt contentHRA is less than or equal to 94.2) and density (density is less than or equal to 15.10 g/cm3) Thus, leading to a reduction in the service life of the resulting cemented carbide. Meanwhile, the hard alloy prepared by the method has the defects of long production period, high energy consumption and the like.
In the prior art, some people adopt a conventional method to prepare the hard alloy without the low binder phase, holes can appear in the prepared hard alloy, the holes cannot be eliminated and are difficult to compact, so that the wear resistance of the hard alloy is poor, the use requirement of a high-precision die cannot be met, and therefore, the hard alloy is more dependent on import in the use of tungsten carbide-based hard alloy products without the low binder phase in China, and the production cost is increased.
The method adopts a special production process and aims to solve the existing defects.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a tungsten carbide-based hard alloy and a preparation method thereof, which can improve the hardness, high temperature resistance and wear resistance of the tungsten carbide-based hard alloy.
In order to solve the technical problems, the invention is realized by adopting the following technical scheme:
in a first aspect, a method for preparing a tungsten carbide-based cemented carbide is characterized by comprising the steps of:
according to the mass parts, 500 parts of WC mixed powder, 0-2 parts of carbon black, 1500-3000 parts of alloy balls and 80-250 parts of ball-milling medium are subjected to ball-milling mixing treatment to prepare mixed slurry, wherein the WC mixed powder comprises 0-1.5% of Cr by mass3C2VC or TiC with the mass percent of 0-2% and Co or Ni with the mass percent of 0-1.5%;
carrying out wax-doping, drying and screening treatment on the mixed slurry to obtain non-low-viscosity phase powder;
putting the powder with no/low-viscosity phase into a mould for compression molding, and carrying out cold isostatic pressing treatment to obtain a pretreated blank;
and sintering the pre-treated blank to obtain the tungsten carbide-based hard alloy.
As an alternative embodiment, the ball milling media comprises alcohol or n-hexane or acetone.
As an optional implementation mode, the ball milling rotation speed of the ball milling mixing treatment is 100-.
As an alternative embodiment, the mould is a rubber mould or an alloy mould or a steel mould.
As an alternative embodiment, the non/low-binding phase powder has a compression molding pressure of 50 to 300 MPa.
As an alternative embodiment, the cold isostatic pressure is 60-120MPa, and the cold isostatic time is 1-4 h.
As an alternative embodiment, the sintering process comprises a first sintering phase and a second sintering phase.
As an optional implementation manner, the sintering temperature of the first sintering stage is 1200-1600 ℃, and the sintering time is 1-3 h; the sintering temperature of the second sintering stage is 1400-1900 ℃, the sintering time is 1-4h, and the sintering pressure is 6-250 MPa.
In a second aspect, the present invention provides a tungsten carbide-based hard alloy, which comprises the following raw material components, by mass: 500 parts of WC mixed powder and 0-2 parts of carbon black, wherein the WC mixed powder comprises 0-1.5 mass percent of Cr3C2VC or TiC with the mass percent of 0-2% and Co or Ni with the mass percent of 0-1.5%.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention provides a preparation method of tungsten carbide-based hard alloy, which comprises the following steps: according to the mass parts, 500 parts of WC mixed powder, 0-2 parts of carbon black, 1500-3000 parts of alloy balls and 80-250 parts of ball-milling medium are subjected to ball-milling mixing treatment to prepare mixed slurry, wherein the WC mixed powder comprises 0-1.5% of Cr by mass3C2Mixing 0-2% of VC or TiC and 0-1.5% of Co or Ni by mass percent, drying and sieving the mixed slurry to obtain non-low-caking phase powder, putting the non-caking phase powder into a mould for compression molding, and performing cold isostatic pressing to obtain a pretreated blank; the pre-treated blank is subjected toSintering to obtain the tungsten carbide-based hard alloy. The tungsten carbide-based hard alloy prepared by the method has excellent performance, short production period and low energy consumption, is beneficial to changing the situation that China depends on import of the products, and greatly reduces the manufacturing cost of the tungsten carbide-based hard alloy.
2. The invention provides a tungsten carbide-based hard alloy which comprises the following raw material components in parts by mass: 500 parts of WC mixed powder and 0-2 parts of carbon black, wherein the WC mixed powder comprises 0-1.5 mass percent of Cr3C2VC or TiC with the mass percent of 0-2% and Co or Ni with the mass percent of 0-1.5%. The tungsten carbide-based hard alloy has excellent performance, and has the advantages of high hardness, high temperature resistance, stable performance and the like.
Drawings
Fig. 1 is a flowchart of a method for preparing a tungsten carbide-based cemented carbide according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the invention provides a preparation method of tungsten carbide-based hard alloy, which comprises the following steps:
the method comprises the following steps: according to the mass parts, 500 parts of WC mixed powder, 1500 parts of alloy balls and 80 parts of ball milling medium are placed into a ball milling tank for carrying out enhanced high-energy ball milling mixing treatment, the ball milling rotating speed of the ball milling mixing treatment is 300 r/min, the ball milling time is 60 hours, mixed slurry is prepared, the WC mixed powder comprises 1.5% of Co by mass percent, and the ball milling medium comprises alcohol or n-hexane or acetone, but the method is not limited to the above.
Step two: and (4) carrying out wax-doping, drying and sieving treatment on the mixed slurry to obtain low-viscosity phase powder.
Step three: and placing the low-bonding-phase powder into a mold for compression molding, wherein the compression molding pressure of the low-bonding-phase powder is 300MPa, so as to prepare a pretreatment blank, and after the pretreatment blank is molded, carrying out green compact cold isostatic pressing treatment on the pretreatment blank, wherein the cold isostatic pressing treatment pressure is 100MPa, and the treatment time is 4 h.
Step four: and sintering the pre-treated blank, wherein the sintering treatment comprises a first sintering stage and a second sintering stage. Specifically, under high-pressure argon, the sintering temperature of the first sintering stage is 1200 ℃, and the sintering time is 3 hours; and the sintering temperature of the second sintering stage is 1400 ℃, the sintering time is 3h, and the sintering pressure is 250MPa, so that the tungsten carbide-based low-bonding-phase hard alloy is prepared, and finally, the tungsten carbide-based hard alloy product is prepared.
Example 2:
the invention provides a preparation method of tungsten carbide-based hard alloy, which comprises the following steps:
the method comprises the following steps: according to the mass parts, 500 parts of WC mixed powder, 0.15 part of carbon black, 2000 parts of alloy balls and 120 parts of ball milling medium are placed into a ball milling tank for carrying out intensified high-energy ball milling mixing treatment, the ball milling rotating speed of the ball milling mixing treatment is 100 revolutions per minute, the ball milling time is 24 hours, and mixed slurry is prepared, wherein the WC mixed powder comprises 0.3% of Cr in mass percentage3C2VC accounting for 1.7 percent of the mass percent and Co accounting for 0.5 percent of the mass percent, wherein the ball milling medium comprises alcohol or normal hexane or acetone, but the ball milling medium is not limited to the alcohol or the normal hexane or the acetone.
Step two: and (4) carrying out wax-doping, drying and sieving treatment on the mixed slurry to obtain low-viscosity phase powder.
Step three: and placing the low-bonding-phase powder into a mold for compression molding, wherein the compression molding pressure of the low-bonding-phase powder is 50MPa, so as to prepare a pretreatment blank, and after the pretreatment blank is molded, performing green compact cold isostatic pressing treatment on the pretreatment blank, wherein the cold isostatic pressing treatment pressure is 100MPa, and the treatment time is 1 h.
Step four: and sintering the pre-treated blank, wherein the sintering treatment comprises a first sintering stage and a second sintering stage. Specifically, under high-pressure argon, the sintering temperature of the first sintering stage is 1200 ℃, and the sintering time is 3 hours; and the sintering temperature of the second sintering stage is 1900 ℃, the sintering time is 1h, and the sintering pressure is 6MPa, so that the tungsten carbide-based low-bonding-phase hard alloy is prepared, and finally, the tungsten carbide-based hard alloy product is prepared.
Example 3:
the invention provides a preparation method of tungsten carbide-based hard alloy, which comprises the following steps:
the method comprises the following steps: according to the mass parts, 500 parts of WC mixed powder, 0.4 part of carbon black, 2200 parts of alloy balls and 150 parts of ball milling medium are placed into a ball milling tank for carrying out intensified high-energy ball milling mixing treatment, the ball milling rotating speed of the ball milling mixing treatment is 130 revolutions per minute, the ball milling time is 30 hours, and mixed slurry is prepared, wherein the WC mixed powder comprises 0.6% of Cr in mass percentage3C2And VC with the mass percent of 1.4%, wherein the ball milling medium comprises alcohol or normal hexane or acetone, but is not limited to the alcohol or the normal hexane or the acetone.
Step two: and (4) carrying out wax-doping, drying and sieving treatment on the mixed slurry to obtain the non-binding phase powder.
Step three: putting the powder without the binding phase into a mould for compression molding, wherein the compression molding pressure of the powder without the binding phase is 100MPa, preparing a pretreatment blank, and after the pretreatment blank is molded, carrying out green compact cold isostatic pressing treatment on the pretreatment blank, wherein the cold isostatic pressing treatment pressure is 65MPa, and the treatment time is 3.5 h.
Step four: and sintering the pre-treated blank, wherein the sintering treatment comprises a first sintering stage and a second sintering stage. Specifically, under high-pressure argon, the sintering temperature of the first sintering stage is 1260 ℃, and the sintering time is 1.5 h; the sintering temperature of the second sintering stage is 1500 ℃, the sintering time is 1.5h, and the sintering pressure is 60MPa, so that the tungsten carbide-based non-binding phase hard alloy is prepared, and finally, the tungsten carbide-based hard alloy product is prepared.
Example 4:
the invention provides a preparation method of tungsten carbide-based hard alloy, which comprises the following steps:
the method comprises the following steps: according to the mass parts, 500 parts of WC mixed powder, 0.8 part of carbon black, 2500 parts of alloy balls and 160 parts of ball milling medium are placed into a ball milling tank for carrying out intensified high-energy ball milling mixing treatment, the ball milling rotating speed of the ball milling mixing treatment is 200 revolutions per minute, the ball milling time is 38 hours, and mixed slurry is prepared, wherein the WC mixed powder comprises 1.0% of Cr by mass3C2VC accounting for 2 percent of the mass percent and Co accounting for 1.0 percent of the mass percent, wherein the ball milling medium comprises alcohol or normal hexane or acetone, but the ball milling medium is not limited to the alcohol or the normal hexane or the acetone.
Step two: and (4) carrying out wax-doping, drying and sieving treatment on the mixed slurry to obtain low-viscosity phase powder.
Step three: and placing the low-bonding-phase powder into a mold for compression molding, wherein the compression molding pressure of the low-bonding-phase powder is 150MPa, so as to prepare a pretreatment blank, and after the pretreatment blank is molded, carrying out green compact cold isostatic pressing treatment on the pretreatment blank, wherein the cold isostatic pressing treatment pressure is 75MPa, and the treatment time is 3 h.
Step four: and sintering the pre-treated blank, wherein the sintering treatment comprises a first sintering stage and a second sintering stage. Specifically, under high-pressure argon, the sintering temperature of the first sintering stage is 1380 ℃, and the sintering time is 2 hours; and the sintering temperature of the second sintering stage is 1600 ℃, the sintering time is 2h, and the sintering pressure is 120MPa, so that the tungsten carbide-based low-bonding-phase hard alloy is prepared, and finally, the tungsten carbide-based hard alloy product is prepared.
Example 5:
the invention provides a preparation method of tungsten carbide-based hard alloy, which comprises the following steps:
the method comprises the following steps: according to the mass parts, 500 parts of WC mixed powder, 1.2 parts of carbon black, 2800 parts of alloy balls and 180 parts of ball milling medium are placed into a ball milling tank for carrying out intensified high-energy ball milling mixing treatment, the ball milling rotating speed of the ball milling mixing treatment is 250 revolutions per minute, the ball milling time is 46 hours, and mixed slurry is prepared, wherein the WC mixed powder comprises 1.2% of Cr in mass percentage3C2VC accounting for 1 percent by mass and Co accounting for 1.2 percent by mass, wherein the ball milling medium comprises alcohol or normal hexane or acetone, but the ball milling medium is not limited to the alcohol or the normal hexane or the acetone.
Step two: and (4) carrying out wax-doping, drying and sieving treatment on the mixed slurry to obtain low-viscosity phase powder.
Step three: and placing the low-bonding-phase powder into a mold for compression molding, wherein the compression molding pressure of the low-bonding-phase powder is 200MPa, so as to prepare a pretreatment blank, and after the pretreatment blank is molded, carrying out green compact cold isostatic pressing treatment on the pretreatment blank, wherein the cold isostatic pressing treatment pressure is 80MPa, and the treatment time is 2 h.
Step four: and sintering the pre-treated blank, wherein the sintering treatment comprises a first sintering stage and a second sintering stage. Specifically, under high-pressure argon, the sintering temperature of the first sintering stage is 1480 ℃, and the sintering time is 1.2 h; and the sintering temperature of the second sintering stage is 1700 ℃, the sintering time is 2.5h, and the sintering pressure is 180MPa, so that the tungsten carbide-based low-bonding-phase hard alloy is prepared, and finally, a tungsten carbide-based hard alloy product is prepared.
Example 6:
the invention provides a preparation method of tungsten carbide-based hard alloy, which comprises the following steps:
the method comprises the following steps: according to the mass parts, 500 parts of WC mixed powder, 1.5 parts of carbon black, 3000 parts of alloy balls and 210 parts of ball-milling medium are placed into a ball-milling tank for carrying out enhanced high-energy ball-milling mixing treatment, the ball-milling rotation speed of the ball-milling mixing treatment is 280 revolutions per minute, the ball-milling time is 54 hours, and mixed slurry is prepared, wherein the WC mixed powder comprises 0.8% of Cr in mass percentage3C2VC accounting for 0.5 percent by mass and Co accounting for 0.2 percent by mass, wherein the ball milling medium comprises alcohol or normal hexane or acetone, but the ball milling medium is not limited to the alcohol or the normal hexane or the acetone.
Step two: and (4) carrying out wax-doping, drying and sieving treatment on the mixed slurry to obtain low-viscosity phase powder.
Step three: and placing the low-bonding-phase powder into a mold for compression molding, wherein the compression molding pressure of the low-bonding-phase powder is 230MPa, so as to prepare a pretreatment blank, and after the pretreatment blank is molded, performing green compact cold isostatic pressing treatment on the pretreatment blank, wherein the cold isostatic pressing treatment pressure is 90MPa, and the treatment time is 1.5 h.
Step four: and sintering the pre-treated blank, wherein the sintering treatment comprises a first sintering stage and a second sintering stage. Specifically, under high-pressure argon, the sintering temperature of the first sintering stage is 1540 ℃, and the sintering time is 1.8 h; and the sintering temperature of the second sintering stage is 1800 ℃, the sintering time is 1.6h, and the sintering pressure is 240MPa, so that the tungsten carbide-based low-bonding-phase hard alloy is prepared, and finally, a tungsten carbide-based hard alloy product is prepared.
Example 7:
the invention provides a preparation method of tungsten carbide-based hard alloy, which comprises the following steps:
the method comprises the following steps: according to the mass parts, 500 parts of WC mixed powder, 2.0 parts of carbon black, 2500 parts of alloy balls and 250 parts of ball-milling medium are placed into a ball-milling tank for carrying out enhanced high-energy ball-milling mixing treatment, the ball-milling rotating speed of the ball-milling mixing treatment is 220 r/min, the ball-milling time is 51h, and mixed slurry is prepared, wherein the WC mixed powder comprises 0.9% of Cr by mass3C2TiC with the mass percent of 2.0 percent and Co with the mass percent of 0.8 percent, and the ball milling medium comprises alcohol or normal hexane or acetone, but is not limited to the alcohol or the normal hexane or the acetone.
Step two: and (4) carrying out wax-doping, drying and sieving treatment on the mixed slurry to obtain low-viscosity phase powder.
Step three: and placing the low-bonding-phase powder into a mold for compression molding, wherein the compression molding pressure of the low-bonding-phase powder is 170MPa, so as to prepare a pretreatment blank, and after the pretreatment blank is molded, carrying out green compact cold isostatic pressing treatment on the pretreatment blank, wherein the cold isostatic pressing treatment pressure is 70MPa, and the treatment time is 2.2 h.
Step four: and sintering the pre-treated blank, wherein the sintering treatment comprises a first sintering stage and a second sintering stage. Specifically, under high-pressure argon, the sintering temperature of the first sintering stage is 1500 ℃, and the sintering time is 2.2 h; and the sintering temperature of the second sintering stage is 1750 ℃, the sintering time is 2.5h, and the sintering pressure is 180MPa, so that the tungsten carbide-based low-bonding-phase hard alloy is prepared, and finally, the tungsten carbide-based hard alloy product is prepared.
Example 8:
the invention provides a preparation method of tungsten carbide-based hard alloy, which comprises the following steps:
the method comprises the following steps: according to the mass parts, 500 parts of WC mixed powder, 0.28 part of carbon black, 2350 part of alloy balls and 85 parts of ball milling medium are placed into a ball milling tank for carrying out enhanced high-energy ball milling mixing treatment, the ball milling rotation speed of the ball milling mixing treatment is 240 r/min, the ball milling time is 45 hours, and mixed slurry is prepared, wherein the WC mixed powder comprises 0.9% of Cr by mass3C2VC accounting for 1.2 percent of the mass percent and Ni accounting for 1.5 percent of the mass percent, wherein the ball milling medium comprises alcohol or normal hexane or acetone, but is not limited to the above.
Step two: and (4) carrying out wax-doping, drying and sieving treatment on the mixed slurry to obtain low-viscosity phase powder.
Step three: and placing the low-bonding-phase powder into a mold for compression molding, wherein the compression molding pressure of the low-bonding-phase powder is 120MPa, so as to prepare a pretreatment blank, and after the pretreatment blank is molded, carrying out green compact cold isostatic pressing treatment on the pretreatment blank, wherein the cold isostatic pressing treatment pressure is 76MPa, and the treatment time is 2.3 h.
Step four: and sintering the pre-treated blank, wherein the sintering treatment comprises a first sintering stage and a second sintering stage. Specifically, under high-pressure argon, the sintering temperature of the first sintering stage is 1560 ℃, and the sintering time is 2.7 h; and the sintering temperature of the second sintering stage is 1800 ℃, the sintering time is 2h, and the sintering pressure is 230MPa, so that the tungsten carbide-based low-bonding-phase hard alloy is prepared, and finally, the tungsten carbide-based hard alloy product is prepared.
Example 9:
the invention provides a preparation method of tungsten carbide-based hard alloy, which comprises the following steps:
the method comprises the following steps: according to the mass parts, 500 parts of WC mixed powder, 0.25 part of carbon black, 2450 parts of alloy balls and 87 parts of ball-milling medium are placed into a ball-milling tank for carrying out intensified high-energy ball-milling mixing treatment, the ball-milling rotation speed of the ball-milling mixing treatment is 220 r/min, the ball-milling time is 46h, and mixed slurry is prepared, wherein the WC mixed powder comprises 0.6% of Cr by mass3C2Quality ofVC accounting for 1.1 percent and Ni accounting for 1.0 percent by mass, and the ball milling medium comprises alcohol or normal hexane or acetone, but is not limited to the alcohol or the normal hexane or the acetone.
Step two: and (4) carrying out wax-doping, drying and sieving treatment on the mixed slurry to obtain low-viscosity phase powder.
Step three: and placing the low-bonding-phase powder into a mold for compression molding, wherein the compression molding pressure of the low-bonding-phase powder is 110MPa, so as to prepare a pretreatment blank, and after the pretreatment blank is molded, carrying out green compact cold isostatic pressing treatment on the pretreatment blank, wherein the cold isostatic pressing treatment pressure is 74MPa, and the treatment time is 2.5 h.
Step four: and sintering the pre-treated blank, wherein the sintering treatment comprises a first sintering stage and a second sintering stage. Specifically, under high-pressure argon, the sintering temperature of the first sintering stage is 1550 ℃, and the sintering time is 2.8 hours; the sintering temperature of the second sintering stage is 1810 ℃, the sintering time is 2.1h, and the sintering pressure is 220MPa, so that the tungsten carbide-based low-bonding-phase hard alloy is prepared, and finally the tungsten carbide-based hard alloy product is prepared.
Example 10:
the invention provides a preparation method of tungsten carbide-based hard alloy, which comprises the following steps:
the method comprises the following steps: according to the mass parts, 500 parts of WC mixed powder, 0.30 part of carbon black, 2500 parts of alloy balls and 90 parts of ball milling medium are placed into a ball milling tank for carrying out intensified high-energy ball milling mixing treatment, the ball milling rotating speed of the ball milling mixing treatment is 280 revolutions per minute, the ball milling time is 53 hours, and mixed slurry is prepared, wherein the WC mixed powder comprises 0.7% of Cr in mass percentage3C21.0% by mass of TiC and 1.1% by mass of Co, and the ball milling medium includes alcohol or n-hexane or acetone, but is not limited thereto.
Step two: and (4) carrying out wax-doping, drying and sieving treatment on the mixed slurry to obtain low-viscosity phase powder.
Step three: and placing the low-bonding-phase powder into a mold for compression molding, wherein the compression molding pressure of the low-bonding-phase powder is 175MPa, so as to prepare a pretreatment blank, and after the pretreatment blank is molded, carrying out green compact cold isostatic pressing treatment on the pretreatment blank, wherein the cold isostatic pressing treatment pressure is 80MPa, and the treatment time is 2.4 h.
Step four: and sintering the pre-treated blank, wherein the sintering treatment comprises a first sintering stage and a second sintering stage. Specifically, under high-pressure argon, the sintering temperature of the first sintering stage is 1520 ℃, and the sintering time is 2.3 h; the sintering temperature of the second sintering stage is 1730 ℃, the sintering time is 2.6h, and the sintering pressure is 170MPa, so that the tungsten carbide-based low-bonding-phase hard alloy is prepared, and finally, the tungsten carbide-based hard alloy product is prepared.
Using the WC mixed powder, carbon black, alloy balls and ball milling media in different weight parts in examples 1 to 10 to prepare a tungsten carbide-based cemented carbide product, performing a single film coating and die pressing frequency test experiment, and obtaining the single film coating and die pressing frequency results of the tungsten carbide-based cemented carbide product as shown in table one:
watch 1
The tungsten carbide-based hard alloy product is prepared from the WC mixed powder, the carbon black, the alloy balls and the ball-milling medium which are prepared in different mass parts in the embodiments 1-10, and a thermal expansion coefficient test experiment is carried out at a high temperature of 600 ℃, so that the thermal expansion coefficient results of the tungsten carbide-based hard alloy product are shown in the following table two:
watch two
In this embodiment, a single film-coating molding frequency study is performed on a tungsten carbide-based cemented carbide product, and as shown in table one, it is found that when the WC mixed powder, the carbon black, the alloy balls and the ball-milling medium are mixed in the proportions of 500 parts, 0-2 parts, 1500-3000 parts and 80-250 parts by mass, wherein the WC mixed powder includes 0-1.5% by mass of Cr3C2VC or TiC with the mass percent of 0-2 percent and Co or Ni with the mass percent of 0-1.5 percent, and the tungsten carbide-based hard material prepared by the method of the inventionDuring alloying, the single coating film die pressing frequency of the tungsten carbide-based hard alloy product is more than or equal to 480 times, while in the prior art, the single coating film die pressing frequency of the hard alloy prepared by the conventional method is about 200 times, so that the single coating film die pressing frequency of the tungsten carbide-based hard alloy prepared by the method is improved by more than 1.5 times compared with the prior art.
In this example, a thermal expansion coefficient study was also performed on the tungsten carbide-based cemented carbide product, and the experimental test results of the thermal expansion coefficient of the cemented carbide product at 600 ℃ are shown in table two. Researches show that when the WC mixed powder, the carbon black, the alloy balls and the ball-milling medium are mixed according to the mixture ratio of 500 parts, 0-2 parts, 3000 parts and 80-250 parts by mass, the WC mixed powder comprises 0-1.5% of Cr by mass3C2VC or TiC accounting for 0-2% by mass and Co or Ni accounting for 0-1.5% by mass, and when the tungsten carbide-based hard alloy product prepared by the method is adopted, the thermal expansion coefficient of the tungsten carbide-based hard alloy product is less than or equal to 4.7E-6/K, and the thermal expansion coefficient of the hard alloy product prepared by the conventional method is more than or equal to 5.3E-6/K at 600 ℃, so that the hard alloy prepared by the method has more stable performance and is not easy to deform at high temperature.
Further analysis on the material performance of the tungsten carbide-based hard alloy product shows that the tungsten carbide-based hard alloy prepared by the method has the grain size of less than or equal to 0.4 mu m, the HV10 of more than or equal to 2430 and the density of more than or equal to 15.35g/cm3Bending strength is not less than 1500MPA, and fracture toughness is 7-8MPAM1/2. The tungsten carbide-based hard alloy prepared by the method only contains trace or no cobalt. However, the tungsten carbide-based hard alloy prepared by the method has higher hardness and stronger high-temperature resistance, and can prolong the service life of the tungsten carbide-based hard alloy product. Meanwhile, the tungsten carbide-based hard alloy prepared by the method has the advantages of short production period, low energy consumption and the like, is favorable for changing the situation that China depends on import of the products, and greatly reduces the manufacturing cost of the tungsten carbide-based hard alloy.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A preparation method of tungsten carbide-based hard alloy is characterized by comprising the following steps:
according to the mass parts, 500 parts of WC mixed powder, 0-2 parts of carbon black, 1500-3000 parts of alloy balls and 80-250 parts of ball-milling medium are subjected to ball-milling mixing treatment to prepare mixed slurry, wherein the WC mixed powder comprises 0-1.5% of Cr by mass3C2VC or TiC with the mass percent of 0-2% and Co or Ni with the mass percent of 0-1.5%;
carrying out wax-doping, drying and screening treatment on the mixed slurry to obtain non-low-viscosity phase powder;
putting the powder with no/low-viscosity phase into a mould for compression molding, and carrying out cold isostatic pressing treatment to obtain a pretreated blank;
and sintering the pre-treated blank to obtain the tungsten carbide-based hard alloy.
2. The method of claim 1, wherein the ball milling media comprises alcohol or n-hexane or acetone.
3. The method for preparing the tungsten carbide-based hard alloy as claimed in claim 1, wherein the ball milling rotation speed of the ball milling mixing treatment is 100-.
4. The method for preparing a tungsten carbide-based cemented carbide according to claim 1, wherein the mold is a rubber mold or an alloy mold or a steel mold.
5. The method for producing a tungsten carbide-based cemented carbide according to claim 1, wherein the press-forming pressure of the non/low-binder phase powder is 50 to 300 MPa.
6. The method for preparing a tungsten carbide-based cemented carbide according to claim 1, wherein the cold isostatic pressure is 60 to 120MPa and the cold isostatic time is 1 to 4 hours.
7. The method of producing a tungsten carbide-based cemented carbide according to claim 1, wherein the sintering treatment includes a first sintering stage and a second sintering stage.
8. The method for preparing the tungsten carbide-based hard alloy as claimed in claim 7, wherein the sintering temperature in the first sintering stage is 1200-1600 ℃, and the sintering time is 1-3 h; the sintering temperature of the second sintering stage is 1400-1900 ℃, the sintering time is 1-4h, and the sintering pressure is 6-250 MPa.
9. The tungsten carbide-based hard alloy is characterized by comprising the following raw material components in parts by mass: 500 parts of WC mixed powder and 0-2 parts of carbon black, wherein the WC mixed powder comprises 0-1.5 mass percent of Cr3C2VC or TiC with the mass percent of 0-2% and Co or Ni with the mass percent of 0-1.5%.
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