CN111057928B - WC-Co-Y with excellent comprehensive mechanical properties2O3Hard alloy and preparation method thereof - Google Patents
WC-Co-Y with excellent comprehensive mechanical properties2O3Hard alloy and preparation method thereof Download PDFInfo
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- 239000000956 alloy Substances 0.000 title claims abstract description 47
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 44
- 229910020514 Co—Y Inorganic materials 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims description 12
- 239000002131 composite material Substances 0.000 claims abstract description 36
- 239000000843 powder Substances 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 29
- 238000005245 sintering Methods 0.000 claims description 28
- 229910009043 WC-Co Inorganic materials 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- 239000011812 mixed powder Substances 0.000 claims description 10
- 229910052593 corundum Inorganic materials 0.000 claims description 7
- 239000010431 corundum Substances 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 229910052727 yttrium Inorganic materials 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims 1
- 239000006185 dispersion Substances 0.000 abstract description 3
- 238000005728 strengthening Methods 0.000 abstract description 3
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 abstract description 3
- 230000001151 other effect Effects 0.000 abstract description 2
- 238000009827 uniform distribution Methods 0.000 abstract description 2
- 238000002490 spark plasma sintering Methods 0.000 abstract 1
- 238000007605 air drying Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 3
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- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 239000003870 refractory metal Substances 0.000 description 2
- 238000009412 basement excavation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
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- 229910052742 iron Inorganic materials 0.000 description 1
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- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
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- 239000011573 trace mineral Substances 0.000 description 1
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- 229910052723 transition metal Inorganic materials 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
- 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
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- B22F1/0003—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
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- 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
- C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
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Abstract
The invention discloses WC-Co-Y with excellent comprehensive mechanical property2O3The hard alloy is prepared by solid-liquid doping process and spark plasma sintering process, wherein Y is2O3The mass fraction of (A) is 0.4-1.6%. The Y is obtained by solid-liquid doping and calcining processes2O3Uniformly distributed WC-Co-Y2O3The composite powder is sintered by discharge plasma to obtain Y2O3Uniformly distributed WC-Co-Y2O3A cemented carbide composite material. By Y2O3The dispersion strengthening and other effects generated by uniform distribution refine tungsten carbide grains, and improve the hardness and the fracture toughness of the hard alloy, which respectively reach 1425.1HV-1498.7HV and 11.5 MPa.m1/2‑12.4MPa·m1/2So that the composite material has more excellent comprehensive mechanical properties.
Description
Technical Field
The invention relates to a WC-based hard alloy material and a preparation method thereof, in particular to WC-Co-Y with excellent comprehensive mechanical property2O3Hard alloy and a preparation method thereof.
Background
The hard alloy is a multiphase composite material prepared by taking one or more refractory metal compounds (WC, TaC, TiC, NbC and the like) with high hardness and high elastic modulus as a matrix and transition metals (Co, Ni, Fe and the like) or alloys as a binder and usually by a powder metallurgy method, and is one of the most typical and important material products in the field of powder metallurgy. The refractory carbide has the characteristics of high melting point, high hardness, good chemical stability, good thermal stability, small mutual dissolution with bonding metal at normal temperature and the like. The bonding metal needs to have good wettability with refractory metal hard compounds, does not react with carbides at a sintering temperature, has good mechanical properties, and does not generate liquid phase at the working temperature of the hard alloy. The hard alloy is widely applied to the aspects of metal cutting processing, metal forming tools, mine excavation, petroleum drilling, national defense and military industry, stone cutting, wood cutting and the like, and is known as 'industrial teeth'. The most widely used at present is WC-Co cemented carbide.
However, with the improvement of processing requirements and the changeful use environment of people, the traditional WC-Co hard alloy can not meet the requirements of people gradually. The hard alloy is easy to wear and break in the using process, which is dangerous for the whole engineering, so a new method for improving the comprehensive mechanical property of the hard alloy is required to be researched. Research shows that the performance of the alloy can be improved by adding trace elements into the alloy and changing the components, the structure and the preparation process of the alloy, and the elements which can be added usually comprise Ni, Cr, Mo, rare earth elements and the like. Y as a rare earth element, usually Y2O3In various alloys, Y2O3The comprehensive mechanical property of the alloy and the service life of the alloy in various environments are improved through the functions of dispersion strengthening and the like.
Disclosure of Invention
The invention aims to provide WC-Co-Y with excellent comprehensive mechanical property2O3Hard alloy and preparation method thereof, WC-Co-Y prepared by sintering2O3Compared with WC-Co hard alloy material, the hardness and the fracture toughness of the hard alloy material are obviously improved.
The invention has excellent comprehensive mechanical property of WC-Co-Y2O3The hard alloy is prepared by a solid-liquid doping process and discharge plasma sintering, wherein the mass fraction of WC is 86.6-87.6%, the mass fraction of Co is 11.8-12.0%, and Y is2O3The mass fraction of (A) is 0.4-1.6%.
The invention has excellent comprehensive mechanical property of WC-Co-Y2O3The preparation method of the hard alloy comprises the following steps:
step 1: powder making
Mixing WC-Co powder (available from Wutokotalong alloy Co., Ltd.) with fully dissolved Y (NO)3)3(purchased from Beijing YinuoKai science and technology Co., Ltd.) solution and magnetic rotor were placed in a beaker, the beaker was placed in a magnetic stirrer for heating, after the solution was dried, the beaker was placed in a forced air drying oven for drying to obtain WC-Co-Y (NO)3)3Mixing powder; the obtained WC-Co-Y (NO)3)3Placing the mixed powder into a corundum crucible, placing the corundum crucible into a tubular high-temperature sintering furnace, and calcining to obtain WC-Co-Y2O3Mixing the powder.
In step 1, the WC-Co powder and Y (NO)3)3The purity was 99.9%.
In the step 1, the model of the magnetic stirrer is DF-1 type heat collection type magnetic stirrer, the heating medium is methyl silicone oil, and the heating temperature is set to be 120-140 ℃.
In the step 1, the model of the air drying oven is DHG-9070 type electric heating constant temperature air drying oven, and the heating temperature is set to be 130-150 ℃.
In the step 1, the model of the tube furnace is GSL-1700X high-temperature tube furnace, the heating temperature is 580-700 ℃, the heating rate is 10 ℃/min, and the cooling rate is 10 ℃/min.
In step 1, said Y2O3Is through Y (NO)3)3Is obtained by thermal decomposition.
Step 2: sintering
The WC-Co-Y obtained in the step 12O3Putting the mixed powder into a graphite mold, putting the mold into a discharge plasma sintering furnace, vacuumizing the furnace chamber at room temperature, heating to 600 ℃ and preserving heat for 5min, heating to 1150-1250 ℃ and preserving heat for 5min, and cooling to room temperature after finishing preserving heat to obtain WC-Co-Y2O3A cemented carbide composite material.
In step 2, the diameter of the graphite mold is 20 mm.
In step 2, the temperature rise rate is 100 ℃/min, and the temperature drop rate is 100 ℃/min.
In the step 2, the pre-pressure is 10MPa, and the highest pressure is 50 MPa.
The invention has the beneficial effects that:
the rare earth element Y is generally represented by Y2O3Since the form of (B) is present in various alloys, Y is usually added to the alloy2O3So as to improve the comprehensive mechanical property of the alloy. The Y is obtained by a solid-liquid doping and calcining process2O3Uniformly distributed WC-Co-Y2O3The composite powder is sintered by discharge plasma to obtain Y2O3Uniformly distributed WC-Co-Y2O3A cemented carbide composite material. By Y2O3The dispersion strengthening and other effects generated by uniform distribution refine tungsten carbide grains, and improve the hardness and the fracture toughness of the hard alloy, which respectively reach 1425.1HV-1498.7HV and 11.5 MPa.m1/2-12.4MPa·m1/2So that the composite material has more excellent comprehensive mechanical properties. Under various use conditions, the service life of the hard alloy composite material can be prolonged, and the risk caused by the damage of the hard alloy parts is reduced.
Drawings
FIG. 1 is WC-Co-Y (NO)3)3The morphology of the composite powder particles can be seen from FIG. 1, which shows WC-Co-Y (NO)3)3The surface of the composite powder particle is coated with a layer of Y (NO)3)3。
FIG. 2 is WC-Co-Y2O3The morphology of the composite powder particles can be seen from FIG. 2Out of WC-Co-Y2O3The surface of the composite powder particle is coated with a layer of Y2O3。
FIG. 3 is WC-Co-Y2O3The morphology of the hard alloy composite material port can be seen from figure 3, the tungsten carbide crystal grains are well bonded with cobalt, and no obvious holes or gaps exist.
Detailed Description
Example 1:
WC-Co-Y in the present example2O3The hard alloy composite material is prepared by a solid-liquid doping process and discharge plasma sintering, wherein the mass fraction of WC is 87.6%, the mass fraction of Co is 12.0%, and Y is2O3Is 0.4% by mass. WC-Co powder and Y (NO)3)3The purity was 99.9%.
WC-Co-Y in the present example2O3The preparation method of the hard alloy composite material comprises the following steps:
1. milling: mixing WC-Co powder with fully dissolved Y (NO)3)3Placing the solution and magnetic rotor in a beaker, placing the beaker in a magnetic stirrer for heating at 120 deg.C, drying the solution, placing the beaker in a forced air drying oven for drying at 130 deg.C to obtain WC-Co-Y (NO)3)3Mixing powder; the obtained WC-Co-Y (NO)3)3Placing the mixed powder in a corundum crucible, placing in a tubular high-temperature sintering furnace, heating to 580 deg.C at a rate of 10 deg.C/min, keeping the temperature for 90min, cooling to room temperature at a rate of 10 deg.C/min, and passing through Y (NO)3)3To obtain WC-Co-Y2O3Mixing the powder.
2. And (3) sintering: putting the mixed powder obtained in the step 1 into a graphite mold, putting the mold into a discharge plasma sintering furnace, vacuumizing the furnace chamber at room temperature, heating to 600 ℃ at the heating rate of 100 ℃/min, keeping the temperature for 5min, heating to 1150 ℃ for 5min, cooling to room temperature at the cooling rate of 100 ℃/min, setting the pre-pressure to 10MPa and the highest pressure to 50MPa during sintering, and obtaining the WC-Co-Y2O3A cemented carbide composite material.
WC-Co-Y after sintering2O3The Vickers hardness of the hard alloy composite material reaches 1425.1HV, which is higher than 1417.8HV of the WC-Co hard alloy composite material; the fracture toughness of the material reaches 11.5 MPa.m1/210.9 MPa.m higher than that of WC-Co hard alloy composite material1/2。
Example 2:
WC-Co-Y in the present example2O3The hard alloy composite material is prepared by a solid-liquid doping process and discharge plasma sintering, wherein the mass fraction of WC is 87.1%, the mass fraction of Co is 11.9%, and Y is2O3The mass fraction of (b) is 1.0%. WC-Co powder and Y (NO)3)3The purity was 99.9%.
WC-Co-Y in the present example2O3The preparation method of the hard alloy composite material comprises the following steps:
1. milling: mixing WC-Co powder with fully dissolved Y (NO)3)3Placing the solution and magnetic rotor in a beaker, placing the beaker in a magnetic stirrer for heating at a set heating temperature of 130 ℃, after the solution is dried, placing the beaker in a blast drying oven for drying at a set temperature of 140 ℃ to obtain WC-Co-Y (NO)3)3Mixing powder; the obtained WC-Co-Y (NO)3)3Placing the mixed powder in a corundum crucible, placing in a tubular high-temperature sintering furnace, heating to 650 ℃ at a speed of 10 ℃/min, keeping the temperature for 90min, cooling to room temperature at a speed of 10 ℃/min, and passing through Y (NO)3)3To obtain WC-Co-Y2O3Mixing the powder.
2. And (3) sintering: putting the mixed powder obtained in the step 1 into a graphite mold, putting the mold into a discharge plasma sintering furnace, vacuumizing the furnace chamber at room temperature, heating to 600 ℃ at the heating rate of 100 ℃/min, keeping the temperature for 5min, heating to 1200 ℃ and keeping the temperature for 5min, cooling to room temperature at the cooling rate of 100 ℃/min, setting the pre-pressure to be 10MPa and the highest pressure to be 50MPa during sintering, and obtaining the WC-Co-Y2O3A cemented carbide composite material.
WC-Co-Y after sintering2O3The Vickers hardness of the hard alloy composite material reaches1446.9HV, 1417.8HV higher than WC-Co cemented carbide composite; the fracture toughness of the material reaches 11.9 MPa.m1/210.9 MPa.m higher than that of WC-Co hard alloy composite material1/2。
Example 3:
WC-Co-Y with excellent comprehensive mechanical properties in the example2O3The hard alloy composite material is prepared by a solid-liquid doping process and discharge plasma sintering, wherein the mass fraction of WC is 86.6%, the mass fraction of Co is 11.8%, and Y is2O3The mass fraction of (a) is 1.6%. WC-Co powder and Y (NO)3)3The purity was 99.9%.
WC-Co-Y with excellent comprehensive mechanical properties in the examples2O3The preparation method of the hard alloy composite material comprises the following steps:
1. milling: mixing WC-Co powder with fully dissolved Y (NO)3)3Placing the solution and magnetic rotor in a beaker, placing the beaker in a magnetic stirrer for heating at 140 deg.C, drying the solution, placing the beaker in a forced air drying oven for drying at 150 deg.C to obtain WC-Co-Y (NO)3)3Mixing powder; the obtained WC-Co-Y (NO)3)3Placing the mixed powder in a corundum crucible, placing in a tubular high-temperature sintering furnace, heating to 700 deg.C at a rate of 10 deg.C/min, keeping the temperature for 90min, cooling to room temperature at a rate of 10 deg.C/min, and passing through Y (NO)3)3To obtain WC-Co-Y2O3Mixing the powder.
2. And (3) sintering: putting the mixed powder obtained in the step 1 into a graphite mold, putting the mold into a discharge plasma sintering furnace, vacuumizing the furnace chamber at room temperature, heating to 600 ℃ at the heating rate of 100 ℃/min, keeping the temperature for 5min, heating to 1250 ℃ at the temperature for 5min, cooling to room temperature at the cooling rate of 100 ℃/min, setting the pre-pressure to be 10MPa and the highest pressure to be 50MPa during sintering, and obtaining the WC-Co-Y2O3A cemented carbide composite material.
WC-Co-Y after sintering2O3The Vickers hardness of the hard alloy composite material reaches 1498.7HV, which is higher than that of WC-Co hard alloy1417.8HV for composite; the fracture toughness of the material reaches 12.4 MPa.m1/210.9 MPa.m higher than that of WC-Co hard alloy composite material1/2。
Table 1 below is WC-Co-Y2O3Hardness and fracture toughness of the cemented carbide composites are compared to WC-Co cemented carbide composites, and from Table 1 it can be seen that Y2O3The hardness and the fracture toughness of the WC-Co hard alloy composite material are improved by doping, and the hardness and the fracture toughness respectively reach 1425.1HV-1498.7HV and 11.5 MPa.m1/2-12.4MPa·m1/2。
TABLE 1
Claims (8)
1. WC-Co-Y with excellent comprehensive mechanical properties2O3The preparation method of the hard alloy is characterized by comprising the following steps:
the WC-Co-Y2O3The hard alloy is prepared by a solid-liquid doping process and discharge plasma sintering, wherein the mass fraction of WC is 86.6-87.6%, the mass fraction of Co is 11.8-12.0%, and Y is2O3The mass fraction of (A) is 0.4-1.6%; the method comprises the following steps:
step 1: powder making
Mixing WC-Co powder with fully dissolved Y (NO)3)3Placing the solution and magnetic rotor in a beaker, placing the beaker in a magnetic stirrer for heating, drying the solution, and placing the beaker in a blast drying oven for drying to obtain WC-Co-Y (NO)3)3Mixing powder; the obtained WC-Co-Y (NO)3)3Placing the mixed powder into a corundum crucible, placing the corundum crucible into a tubular high-temperature sintering furnace, and calcining to obtain WC-Co-Y2O3Mixing powder;
step 2: sintering
The WC-Co-Y obtained in the step 12O3The mixed powder is loaded into a graphite mould, then the mould is placed into a discharge plasma sintering furnace, the furnace chamber is vacuumized at room temperature,then heating to 600 ℃ and preserving heat for 5min, then heating to 1150-1250 ℃ and preserving heat for 5min, cooling to room temperature after heat preservation is finished, and obtaining WC-Co-Y2O3A cemented carbide composite material.
2. The method of claim 1, wherein:
in step 1, the WC-Co powder and Y (NO)3)3The purity of (2) was 99.9%.
3. The method of claim 1, wherein:
in step 1, the heating temperature of the magnetic stirrer is 120-140 ℃.
4. The method of claim 1, wherein:
in the step 1, the drying temperature of the air-blast drying oven is set to be 130-150 ℃.
5. The method of claim 1, wherein:
in step 1, the calcination temperature is 580-700 ℃, the heating rate is 10 ℃/min, and the cooling rate is 10 ℃/min.
6. The method of claim 1, wherein:
in step 2, the temperature rise rate is 100 ℃/min, and the temperature drop rate is 100 ℃/min.
7. The method of claim 1, wherein:
in the step 2, the pre-pressure is 10MPa, and the highest pressure is 50 MPa.
8. WC-Co-Y with excellent comprehensive mechanical properties2O3Cemented carbide, characterized in that the WC-Co-Y2O3The cemented carbide is obtained by the preparation method of any one of claims 1-7.
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| CN113337747B (en) * | 2021-05-31 | 2023-04-18 | 合肥工业大学 | Preparation method of high-strength and high-conductivity copper alloy |
| CN113416862B (en) * | 2021-06-04 | 2022-04-15 | 合肥工业大学 | Preparation method of hard alloy and hard alloy prepared by adopting same |
| CN113355550B (en) * | 2021-06-15 | 2022-07-15 | 合肥工业大学 | Doped Y2O3Preparation method of reinforced CuCrZr alloy |
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| US6596397B2 (en) * | 2001-04-06 | 2003-07-22 | Shin-Etsu Chemical Co., Ltd. | Thermal spray particles and sprayed components |
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