CN111893339A - Method for preparing high-performance WC-8Co-Y2O3 hard alloy by wet chemical method - Google Patents
Method for preparing high-performance WC-8Co-Y2O3 hard alloy by wet chemical method Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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
- C22C1/053—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds
- C22C1/055—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds using carbon
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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
- C22C1/053—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds
- C22C1/056—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds using gas
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- C—CHEMISTRY; METALLURGY
- 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
- C22C29/067—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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—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
Abstract
The invention discloses a wet chemical method for preparing high-performance WC-8Co-Y2O3The hard alloy is prepared by adding trace yttrium oxide Y to WC-8Co2O3The method can refine crystal grains and improve the comprehensive mechanical property of WC-8 Co. The method has the advantage that the trace substance Y is completed before the tungsten carbide is generated2O3Prepared according to the principle of a wet chemical method2O3The powder is carbonized and sintered with cobalt to prepare WC-8Co-Y2O3And (3) alloying. Y added in this way2O3The growth and aggregation of WC particles can be inhibited in the carbonization stage, WC crystal grains can be further refined in the sintering process, and the WC crystal grains can be further refined through Y2O3The dispersion strengthening and the like are generated by uniform distribution, and the hardness and the bending strength of the hard alloy are improved.
Description
Technical Field
The invention relates to a method for preparing a WC-based hard alloy material, in particular to a method for preparing high-performance WC-8Co-Y by a wet chemical method2O3A method of cemented carbide.
Background
The hard alloy is a powder metallurgy product which is mainly formed by sintering WC serving as a matrix and Co or Ni serving as a binder at the high temperature of 1300-1600 ℃. The hard alloy material has high hardness, good hot hardness and high wear resistance and corrosion resistance, so the hard alloy material is commonly used for manufacturing wear-resistant parts such as cutting tools, drilling tools, guide wheels and the like. The hard alloy tool has higher cutting speed and longer service life than a tool steel tool, can be used for cutting cast iron and common steel, and can also be used for processing high-strength steel such as stainless steel, heat-resistant steel, medium manganese steel and the like, and the hard alloy tool is widely commercialized and suitable for large-scale application in cost and process.
In order to improve the comprehensive mechanical properties of the hard alloy material, a trace amount of grain growth inhibitor is often added in the preparation process of the hard alloy material. Common inhibitors include vanadium carbide VC and chromium carbide Cr3C2And the addition of the inhibitor can refine tungsten carbide grains, so that the comprehensive mechanical property of the sintered hard alloy is improved. At present, an inhibitor is added to prepare a novel WC-8Co hard alloy, WC-Co composite powder is obtained by mainly mixing WC powder, Co powder and the inhibitor through ball milling, and the composite powder is sintered to obtain the alloy. Although the size of the crystal grains is controlled to a certain extent by the inhibitor added in the method, the size of the WC crystal grains is mainly determined by the size of WC powder particles, so that the improvement of the comprehensive mechanical property of the WC-8Co alloy is limited, and a novel WC-8Co hard alloy still needs to be further developed.
Disclosure of Invention
The invention aims to provide a wet chemical method for preparing high-performance WC-8Co-Y2O3The novel hard alloy is prepared by adding trace yttrium oxide Y on the basis of WC-8Co2O3The method can refine crystal grains and improve the comprehensive mechanical property of WC-8 Co.
The wet chemical method of the invention prepares high-performance WC-8Co-Y2O3A method of cemented carbide comprising the steps of:
step 1: powder making
To biasAmmonium tungstate AMT as tungsten source, yttrium nitrate Y (NO) hexahydrate3)3·6H2O is yttrium source, and W-Y is prepared by wet chemical method2O3Powder; the method specifically comprises the following steps:
1a, adopting deionized water to mix AMT and Y (NO)3)3·6H2Dissolving O in a glass reaction kettle, adding oxalic acid (C)2H2O4·2H2O) precipitating the precursor from the solution. And heating the reaction kettle and stirring the mixed solution, wherein the heating temperature is controlled at 160 ℃, and the rotating speed of a stirring rod is controlled at 120 r/min. After evaporation and deposition, a yellowish W-Y is obtained2O3Drying the precursor in a blast drying oven, grinding the precursor powder by using a pulverizer, and sieving and collecting the precursor powder with the particle size of less than 200 meshes;
and 1b, uniformly and flatly paving the precursor powder obtained in the step 1a in a burning boat, and reducing in a continuous hydrogen reduction furnace at a boat pushing speed of 15 min/boat. The load of the burning boat is 1 Kg/boat, and the reducing atmosphere is H2At a flow velocity of 24m3H is used as the reference value. The continuous hydrogen reduction is carried out in a three-temperature zone reduction furnace, and the set temperature range is 880-930 ℃. After the burning boat passes through the three temperature zones in sequence, the powder in the burning boat is made to pass through W-Y2O3The precursor powder is reduced to W-Y2O3And (3) composite powder.
Step 2: cobalt complex carbide
The W-Y prepared in the step 12O3The composite powder is mixed with carbon according to the tungsten-carbon atomic ratio of 1:1, ball-milled and mixed for 2 hours, put into a high-temperature furnace, and carbonized at the temperature of 1850-2O3Mixing the powder with cobalt powder accounting for 8 percent of the total mass, and performing ball milling and powder mixing for 36 hours;
in the step 2, the granularity of WC powder obtained by carbonization is 2-3 microns;
in the step 2, the purity of the carbon powder is 99.9 percent, and the granularity is 100 nanometers;
in step 2, the purity of the cobalt powder is 99.9%, and the particle size is 1.23 microns.
And step 3: sintering
Step 2Obtained WC-8Co-Y2O3Pressing the composite powder into a green body, and then performing vacuum sintering under the conditions of the vacuum degree of 10-20Pa and the temperature of 1400 ℃ and 1500 ℃ to prepare the hard alloy with excellent comprehensive performance.
In step 3, the temperature preservation time at the temperature of 1400 ℃ and 1500 ℃ is 90 minutes.
The method has the advantage that the trace substance Y is completed before the tungsten carbide is generated2O3Prepared according to the principle of a wet chemical method2O3The powder is carbonized and sintered with cobalt to prepare WC-8Co-Y2O3And (3) alloying. Y added in this way2O3The growth and aggregation of WC grains can be inhibited in the carbonization stage, and WC grains can be further refined in the sintering process. By Y2O3The hardness and the bending strength of the hard alloy are respectively 89.2-90.3 HRA and 2320-2660 MPa, and compared with the hardness 87.5HRA and the bending strength 1815MPa of pure WC-8Co, the hardness and the bending strength of the hard alloy are greatly improved, so that the WC-8Co-Y is subjected to dispersion strengthening and the like generated by uniform distribution2O3Has more excellent comprehensive mechanical property.
Drawings
FIG. 1 shows wet-chemically prepared W-Y2O3In the scanning electron microscope image of the powder, W powder particles are hexagonal and about 1-2 microns in size.
Shown in FIG. 2 is W-Y2O3WC-Y produced by high-temperature carbonization2O3According to a scanning electron microscope image of the powder, WC particles are irregular and square, and the size of the WC particles is about 2-3 micrometers.
FIG. 3 shows cemented carbide W-8Co-Y2O3The micro-gold phase diagram of the alloy has compact combination of WC crystal grains and Co, and has no obvious holes and gaps.
Detailed Description
Example 1:
WC-8Co-Y in the present example2O3The hard alloy is made of W-Y2O3The powder is obtained by carbonization and cobalt-matching sintering, and the sintering temperature is 1400 ℃. Wherein the components by mass percent are WC 91.5%, Co 8%, Y2O30.5％。
WC-8Co-Y in the present example2O3The preparation method of the hard alloy comprises the following steps:
1. milling: 1.3kg of Ammonium Metatungstate (AMT), 500g of oxalic acid (C)2H2O4·2H2O) and 16.5g of yttrium nitrate hexahydrate (Y (NO)3)3·6H2O)(Y(NO3)3·6H2The amount of O is 0.5% by mass of Y in the cemented carbide2O3Calculated addition) was placed in a reaction kettle and dissolved with deionized water. Heating and stirring the mixed solution to evaporate water to obtain light yellow W-Y2O3And (3) precursor. Mixing W-Y2O3Drying the precursor in an oven, grinding and sieving the dried agglomerates to obtain W-Y with the particle size of less than 200 meshes2O3And (3) precursor powder. Last pair of W-Y2O3Reducing the precursor powder by using a hydrogen reducing furnace, wherein the reduction temperature is 880-930 ℃, and the gas flow speed is 24m3H is used as the reference value. Reduction of the resulting W-Y2O3Is black and has a particle size of about 1 micron.
2. And (3) cobalt preparation by carbonization: mixing W-Y2O3Mixing the powder with carbon powder (the amount of the carbon powder is determined according to the tungsten-carbon atomic ratio of 1: 1), ball-milling for 2 hours, putting the mixture into a high-temperature furnace, heating to 1900 ℃, preserving the heat for 2 hours at high temperature, then cooling along with the furnace, and detecting the granularity and the carbon content of the carbonized powder. The carbon content of the carbonized powder is between 6.07 percent and 6.13 percent, and then 8 percent of the total mass of the powder is mixed with cobalt powder. Then to WC-Y2O3Ball-milling and mixing the cobalt-mixed composite powder at a ball-to-material ratio of 4:1 for 36 hours to prepare WC-8Co-Y2O3And (3) compounding powder.
3. And (3) vacuum sintering: mixing WC-8Co-Y2O3Putting the composite powder into a square graphite die to press a green body, putting the green body into a high-temperature vacuum furnace, vacuumizing to 10-20Pa, heating to 1400 ℃, preserving heat for 90 minutes, and then cooling along with the furnace to obtain the sintered and densified WC-8Co-Y2O3Hard alloy.
The hardness and the bending strength of the sintered sample are tested, and the hardness value is 89.2HRA, the bending strength is 2320Mpa, and the hardness is 87.5HRA and the bending strength is 1815MPa which are higher than the national standard WC-8 Co.
Example 2:
WC-8Co-Y in the present example2O3The hard alloy is made of W-Y2O3The powder is obtained by carbonization and cobalt-matching sintering, and the sintering temperature is 1450 ℃. Wherein the components by mass percent are WC 91.5%, Co 8%, Y2O30.5％。
WC-8Co-Y in the present example2O3The preparation method of the hard alloy comprises the following steps:
1. milling: 1.3kg of Ammonium Metatungstate (AMT), 500g of oxalic acid (C)2H2O4·2H2O) and 16.5g of yttrium nitrate hexahydrate (Y (NO)3)3·6H2O)(Y(NO3)3·6H2The amount of O is 0.5% by mass of Y in the cemented carbide2O3Calculated addition) was placed in a reaction kettle and dissolved with deionized water. Heating and stirring the mixed solution to evaporate water to obtain light yellow W-Y2O3And (3) precursor. Mixing W-Y2O3Drying the precursor in an oven, grinding and sieving the dried agglomerates to obtain W-Y with the particle size of less than 200 meshes2O3And (3) precursor powder. Last pair of W-Y2O3Reducing the precursor powder by using a hydrogen reducing furnace, wherein the reduction temperature is 880-930 ℃, and the gas flow speed is 24m3H is used as the reference value. Reduction of the resulting W-Y2O3Is black and has a particle size of about 1 micron.
2. And (3) cobalt preparation by carbonization: mixing W-Y2O3Mixing the powder with carbon powder (the amount of the carbon powder is determined according to the tungsten-carbon atomic ratio of 1: 1), ball-milling for 2 hours, putting the mixture into a high-temperature furnace, heating to 1900 ℃, preserving the heat for 2 hours at high temperature, then cooling along with the furnace, and detecting the granularity and the carbon content of the carbonized powder. The carbon content of the carbonized powder is between 6.07 percent and 6.13 percent, and then 8 percent of the total mass of the powder is mixed with cobalt powder. Then to WC-Y2O3Ball-milling and mixing the cobalt-mixed composite powder at a ball-to-material ratio of 4:1 for 36 hours to prepare WC-8Co-Y2O3And (3) compounding powder.
3. And (3) vacuum sintering: mixing WC-8Co-Y2O3Filling composite powderPressing a green body in a square graphite die, putting the green body into a high-temperature vacuum furnace, vacuumizing to 10-20Pa, heating to 1450 ℃, preserving heat for 90 minutes, and then cooling along with the furnace to obtain the sintered compact WC-8Co-Y2O3Hard alloy.
The hardness and the bending strength of the sintered sample are tested, and the hardness value is 89.9HRA, the bending strength is 2660Mpa, and the hardness is 87.5HRA and the bending strength is 1815MPa which are higher than the national standard WC-8 Co.
Example 3:
WC-8Co-Y in the present example2O3The hard alloy is made of W-Y2O3The powder is obtained by carbonizing, matching with cobalt and sintering, and the sintering temperature is 1500 ℃. Wherein the components by mass percent are WC 91.5%, Co 8%, Y2O30.5％。
WC-8Co-Y in the present example2O3The preparation method of the hard alloy comprises the following steps:
1. milling: 1.3kg of Ammonium Metatungstate (AMT), 500g of oxalic acid (C)2H2O4·2H2O) and 16.5g of yttrium nitrate hexahydrate (Y (NO)3)3·6H2O)(Y(NO3)3·6H2The amount of O is 0.5% by mass of Y in the cemented carbide2O3Calculated addition) was placed in a reaction kettle and dissolved with deionized water. Heating and stirring the mixed solution to evaporate water to obtain light yellow W-Y2O3And (3) precursor. Mixing W-Y2O3Drying the precursor in an oven, grinding and sieving the dried agglomerates to obtain W-Y with the particle size of less than 200 meshes2O3And (3) precursor powder. Last pair of W-Y2O3Reducing the precursor powder by using a hydrogen reducing furnace, wherein the reduction temperature is 880-930 ℃, and the gas flow speed is 24m3H is used as the reference value. Reduction of the resulting W-Y2O3Is black and has a particle size of about 1 micron.
2. And (3) cobalt preparation by carbonization: mixing W-Y2O3Mixing the powder with carbon powder (the amount of the carbon powder is determined according to the tungsten-carbon atomic ratio of 1: 1), ball-milling for 2 hours, placing into a high-temperature furnace, heating to 1900 ℃, keeping the temperature for 2 hours at high temperature, then cooling along with the furnace, and detecting the granularity and the carbon content of the carbonized powder. The carbon content of the carbonized powder is between 6.07 percent and 6.13 percent, and then 8 percent of the total mass of the powder is mixed with cobalt powder. Then to WC-Y2O3Ball-milling and mixing the cobalt-mixed composite powder at a ball-to-material ratio of 4:1 for 36 hours to prepare WC-8Co-Y2O3And (3) compounding powder.
3. And (3) vacuum sintering: mixing WC-8Co-Y2O3Putting the composite powder into a square graphite die to press a green body, putting the green body into a high-temperature vacuum furnace, vacuumizing to 10-20Pa, heating to 1500 ℃, keeping the temperature for 90 minutes, and then cooling along with the furnace to obtain the sintered and densified WC-8Co-Y2O3Hard alloy.
The hardness and the bending strength of the sintered sample are tested, and the hardness value is 90.3HRA, the bending strength is 2650Mpa, and the hardness is 87.5HRA and the bending strength is 1815MPa which are higher than the national standard WC-8 Co.
Table 1 below shows the cemented carbide WC-8Co-Y at different sintering temperatures2O3The hardness and strength of the alloy obtained by sintering at 1500 ℃ are 90.3HRA (Rockwell hardness) maximum, and the bending strength of the alloy obtained by sintering at 1450 ℃ is 2660MPa maximum.
TABLE 1
| Hard alloy | Sintering temperature (. degree. C.) | Hardness (HRA) | Bending strength (Mpa) |
| WC-8Co | 1300～1600 | 87.5 | 1815 |
| WC-8Co-0.5Y2O3 | 1400 | 89.2 | 2320 |
| WC-8Co-0.5Y2O3 | 1450 | 89.9 | 2660 |
| WC-8Co-0.5Y2O3 | 1500 | 90.3 | 2650 |
Claims (7)
1. Wet chemical method for preparing high-performance WC-8Co-Y2O3A method of cemented carbide characterized by:
adding a trace amount of yttrium oxide Y on the basis of WC-8Co2O3And completing the trace of substance Y before the formation of tungsten carbide2O3Prepared according to the principle of a wet chemical method2O3The powder is carbonized and sintered with cobalt to prepare WC-8Co-Y2O3Alloy to improve the comprehensive mechanical property of the material.
2. The method according to claim 1, characterized by comprising the steps of:
step 1: powder making
1a, adopting deionized water to mix AMT and Y (NO)3)3·6H2Dissolving O in a glass reaction kettle, adding oxalic acid to separate out the precursor from the solution, heating the reaction kettle and stirring the mixed solution, controlling the heating temperature at 160 ℃, and obtaining light yellow W-Y after evaporation and deposition2O3A precursor ofDrying in a blast drying oven, grinding the precursor powder by a pulverizer, sieving and collecting the precursor powder below 200 meshes;
and 1b, uniformly and flatly paving the precursor powder obtained in the step 1a in a burning boat, and reducing in a continuous hydrogen reduction furnace at a boat pushing speed of 15 min/boat. The continuous hydrogen reduction is carried out in a three-temperature-zone reduction furnace, and after the burning boat passes through three temperature zones in sequence, the powder in the burning boat is formed by W-Y2O3The precursor powder is reduced to W-Y2O3Composite powder;
step 2: cobalt complex carbide
The W-Y prepared in the step 12O3The composite powder is mixed with carbon according to the tungsten-carbon atomic ratio of 1:1, ball-milled and mixed for 2 hours, put into a high-temperature furnace, and carbonized at the temperature of 1850-2O3Mixing the powder with cobalt powder accounting for 8 percent of the total mass, and performing ball milling and powder mixing for 36 hours;
and step 3: sintering
The WC-8Co-Y obtained in the step 22O3Pressing the composite powder into a green body, and then performing vacuum sintering under the conditions of the vacuum degree of 10-20Pa and the temperature of 1400 ℃ and 1500 ℃ to prepare the hard alloy with excellent comprehensive performance.
3. The method of claim 2, wherein:
in step 1b, the load of the burning boat is 1 Kg/boat, and the reducing atmosphere is H2At a flow velocity of 24m3/h。
4. The method of claim 2, wherein:
in the step 1b, the temperature range of the three-temperature zone reduction furnace is set to 880-930 ℃.
5. The method of claim 2, wherein:
in the step 2, the granularity of WC powder obtained by carbonization is 2-3 microns.
6. The method of claim 2, wherein:
in the step 2, the purity of the carbon powder is 99.9 percent, and the granularity is 100 nanometers; the purity of the cobalt powder was 99.9% and the particle size was 1.23 microns.
7. The method of claim 2, wherein:
in step 3, the temperature preservation time at the temperature of 1400 ℃ and 1500 ℃ is 90 minutes.
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| CN115070042A (en) * | 2022-06-07 | 2022-09-20 | 合肥工业大学 | Rare earth oxide modified hard alloy turning tool blade and preparation method thereof |
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