CN116121579A - Preparation method of MoCoB-WCoB based composite material - Google Patents
Preparation method of MoCoB-WCoB based composite material Download PDFInfo
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- CN116121579A CN116121579A CN202211489844.8A CN202211489844A CN116121579A CN 116121579 A CN116121579 A CN 116121579A CN 202211489844 A CN202211489844 A CN 202211489844A CN 116121579 A CN116121579 A CN 116121579A
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- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000005245 sintering Methods 0.000 claims abstract description 17
- 239000011159 matrix material Substances 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 10
- 238000000498 ball milling Methods 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 6
- 239000011812 mixed powder Substances 0.000 claims abstract description 6
- 238000003825 pressing Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000009740 moulding (composite fabrication) Methods 0.000 claims description 3
- 230000002787 reinforcement Effects 0.000 claims description 3
- 239000012071 phase Substances 0.000 abstract description 34
- 230000003014 reinforcing effect Effects 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 238000011065 in-situ storage Methods 0.000 abstract description 3
- 239000007790 solid phase Substances 0.000 abstract description 3
- 238000000465 moulding Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 12
- 239000000919 ceramic Substances 0.000 description 11
- 239000002184 metal Substances 0.000 description 10
- 229910052751 metal Inorganic materials 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 6
- 239000011195 cermet Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000011153 ceramic matrix composite Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- -1 methods Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000126 substance Substances 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
- 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
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/12—Metallic powder containing non-metallic particles
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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
- B22F3/02—Compacting only
-
- 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
- B22F3/1039—Sintering only by reaction
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- 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
-
- 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
- C22C29/14—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on borides
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E40/00—Technologies for an efficient electrical power generation, transmission or distribution
- Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment
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Abstract
The invention discloses a preparation method of a MoCoB-WCoB matrix composite material. The disclosed method comprises the following steps: pressing and molding the mixed powder of Mo, co, B and W powder after ball milling to obtain a blank, and then sintering the blank in a vacuum carbon tube furnace to prepare a MoCoB-WCoB matrix composite; the weight percentages are as follows: 34.0 to 46.0 percent of Mo, 38.0 to 52.0 percent of Co, 3.0 to 7.0 percent of B and 5.0 to 15.0 percent of W. In the invention, two hard phases of MoCoB and WCoB are generated through solid-phase in-situ reaction in the sintering process, and the WCoB is used as an 'endogenous' reinforcing phase, so that the method has the advantages of no surface pollution and high interface bonding strength; the prepared MoCoB-WCoB-based composite material has the advantages of compact microstructure, fine grains, good compactness, high hardness and the like.
Description
Technical Field
The invention relates to a preparation method of a MoCoB-WCoB matrix composite material, belonging to the field of structural functional materials. Provides a novel method with short preparation period, stable process and easy industrialization for preparing MoCoB-based metal ceramic.
Background
The ternary boride-based metal ceramic is a boride-based composite material prepared according to the reaction boride sintering principle, has the advantages of high hardness, good wear resistance, corrosion resistance, high strength of metal, good plastic toughness and the like of the ceramic, and is widely applied to the fields of cutters, turning molds and the like. The hard phase in ternary boride-based metal ceramic is not added as a raw material, but is generated by in-situ reaction of intermediate product binary boride and metal by a solid phase, and belongs to an 'endogenous' hard phase, the surface of the ternary boride-based metal ceramic is free from pollution, the problem of poor compatibility with a matrix is avoided, and the interface bonding strength is high. The MoCoB-based metal ceramic is novel ternary boride-based metal ceramic developed in recent years, consists of a MoCoB hard phase and a Co binding phase, has the advantages of high hardness, good wear resistance, strong high-temperature oxidation resistance and the like, and has great potential in the field of wear-resistant materials.
The MoCoB-based cermet prepared at present has good hardness and can be used as a wear-resistant part of a car door die, a turning tool, a milling cutter and the like. However, with the rapid development of technology, high-performance materials are layered endlessly, the performance of materials to be processed is gradually improved, and the MoCoB-based metal ceramic is required to be further improved in hardness so as to keep market competitiveness. The hardness of the biphase ceramic matrix composite material can be improved by adding the second phase ceramic to the cermet. For example:
TiB in journal of hard alloy 2 Addition of second phase TiB in the paper study of influence of MoCoB-based cermet Structure and Performance 2 The influence of the particles on the microstructure and mechanical property of MoCoB-Co metal ceramic shows that TiB is added 2 The hardness of the composite material is improved, and the maximum hardness reaches 88.9HRA. TiB addition in the prior art study 2 Although the hardness of the composite material can be increased, tiB 2 The reinforcing phase belongs to an 'externally added' reinforcing phase, is not an 'internally generated' reinforcing phase, can reduce the wettability between the original MoCoB hard phase and the Co binding phase, and causes the reduction of interface strength, thereby influencing the service safety and the service life of the composite material. In addition, tiB is added 2 The hardness improvement effect on the composite material is limited.
Disclosure of Invention
Aiming at the defects or shortcomings of the prior art, the invention provides a preparation method of a MoCoB-WCoB matrix composite material.
For this purpose, the preparation method provided by the invention comprises the following steps: sequentially ball-milling, pressing and forming mixed powder of Mo, co, B and W powder to obtain a blank, and then sintering the blank in a vacuum carbon tube furnace to prepare the MoCoB-WCoB matrix composite;
the weight percentages are as follows: 34.0 to 46.0 percent of Mo, 38.0 to 52.0 percent of Co, 3.0 to 7.0 percent of B and 5.0 to 15.0 percent of W.
Optionally, the sintering process parameters are as follows: raising the temperature from room temperature to 1350-1450 ℃ at a heating rate of 5-15 ℃/min, preserving the temperature for 0-60 min, and cooling to room temperature.
Further, the MoCoB-WCoB matrix composite material comprises three phases: a MoCoB hard phase, a Co-based binder phase, and a WCoB reinforcement phase. The hardness of the MoCoB-WCoB matrix composite material is 88.8-90.6 HRA, and the density is 97.73-98.91%.
Compared with the prior art, (1) the composite material generated by the invention comprises three phases: a MoCoB hard phase, a Co-based binder phase, and a WCoB reinforcement phase; (2) the WCoB reinforcing phase is not directly added into the raw material, but generated by the raw material powder through solid phase in-situ reaction, is an 'endogenous' reinforcing phase, and has the advantages of no surface pollution and high interface bonding strength; (3) the prepared MoCoB-WCoB-based composite material has the advantages of compact microstructure, fine grains, good compactness, high hardness and the like.
Drawings
FIG. 1 is an XRD pattern for a MoCoB-WCoB based composite according to example 2 of the present invention;
FIG. 2 is a photograph of a microstructure of the MoCoB-WCoB matrix composite of example 2 of the present invention.
Detailed Description
Unless specifically stated otherwise, scientific and technical terms and methods herein have been understood or implemented by those of ordinary skill in the relevant art based on the knowledge of one of ordinary skill in the relevant art. It should also be understood that the temperature, hold time, and the like referred to herein are approximations for purposes of illustration. Although methods and materials similar or equivalent to those described herein can be used in the practice of the present disclosure, some suitable methods and materials are described below. Publications, patent applications, patents, and other references mentioned herein are incorporated by reference in their entirety to the extent that any conflict arises. In addition, the materials, methods, material ratios, and examples are illustrative only and not intended to be limiting. In a specific scheme, a person skilled in the art can optimize the material proportion and the operation parameter value involved in the method according to the disclosure of the invention by adopting a conventional experimental period to achieve the aim of the invention.
The purpose of the press forming according to the invention is to initially densify the powdery raw material, the shape and size of the green body produced depending on the shape of the mould. The molds used in the prior art of ceramics, such as molds with volume dimensions greater than 3mm by 3mm, are suitable for use in the present invention.
Based on the disclosure of the present invention, a person skilled in the art may optimize specific sintering by using a conventional experimental means for different formulation materials and effects of the present invention, and the specific sintering process adopted in the following examples is only one specific example to explain the scheme of the present invention, and the sintering process of the present invention is not limited thereto. The sintering process conditions are exemplified by raising the temperature from room temperature to 1350-1450 ℃ at a heating rate of 5-15 ℃/min, and maintaining the temperature for 0-60 min, and then furnace cooling to room temperature.
The invention is illustrated in further detail by the following examples. The raw materials Mo, W, co and B powder used in the embodiment of the invention are all commercial chemical pure powder reagents, and a planetary ball mill (QM-3 SP 4) is adopted for ball milling. The present invention is not limited to these specific devices.
In the invention, the density of the MoCoB-WCoB based composite material is tested by adopting an Archimedes drainage method; the hardness of the MoCoB-WCoB based composite was measured using HRS-150 rockwell hardness tester.
Example 1:
in the embodiment, mo, co, B and W powder with purity not lower than 99.0% are selected as raw materials, and the raw materials are as follows by mass percent: 46.0% Mo, 46% Co, 3.0% B, 5.0% W;
ball milling and compacting the mixed powder to prepare a cylindrical (diameter 44mm, height 8-9 mm) blank;
then placing the blank into a vacuum carbon tube furnace for sintering, wherein the sintering process parameters are as follows: the temperature was raised from room temperature to 1350 ℃ at a heating rate of 5 ℃/min and incubated for 0min, after which the furnace cooled to room temperature.
The MoCoB-WCoB-based composite material prepared in the embodiment comprises a MoCoB hard phase, a Co-based binding phase and a WCoB reinforcing phase, wherein the hardness is 89.2HRA, and the compactness is 97.73%.
Example 2:
in the embodiment, mo, co, B and W powder with purity not lower than 99.0% are selected as raw materials, and the raw materials are as follows by mass percent: 40.0% of Mo, 45% of Co, 5% of B and 10.0% of W;
ball milling and compacting the mixed powder to prepare a cylindrical (diameter 44mm, height 8-9 mm) blank;
then placing the blank into a vacuum carbon tube furnace for sintering, wherein the sintering process parameters are as follows: the temperature was raised from room temperature to 1400℃at a heating rate of 10℃per minute and kept at that temperature for 30 minutes, after which the furnace was cooled to room temperature.
The MoCoB-WCoB-based composite material prepared in the embodiment comprises a MoCoB hard phase, a Co-based binding phase and a WCoB reinforcing phase (XRD pattern is shown in figure 1), and the microstructure is shown in figure 2; the hardness of the composite material is 90.6HRA, and the compactness is 98.54%.
Example 3:
in the embodiment, mo, co, B and W powder with purity not lower than 99.0% are selected as raw materials, and the raw materials are as follows by mass percent: 34.0% of Mo, 44.0% of Co, 7.0% of B and 15.0% of W;
ball milling and compacting the mixed powder to prepare a cylindrical (diameter 44mm, height 8-9 mm) blank;
then placing the blank into a vacuum carbon tube furnace for sintering, wherein the sintering process parameters are as follows: the temperature was raised from room temperature to 1450℃at a heating rate of 15℃per minute and kept at that temperature for 60 minutes, after which the furnace was cooled to room temperature.
The MoCoB-WCoB-based composite material prepared in the embodiment comprises a MoCoB hard phase, a Co-based binding phase and a WCoB reinforcing phase, wherein the hardness is 88.8HRA, and the compactness is 98.91%.
Comparative example:
the comparative example differs from example 2 in mass: the raw materials do not contain W powder.
The MoCoB-based cermet obtained in this comparative example contained a MoCoB hard phase and a Co-based binder phase, and had a hardness of 87.6HRA and a density of 97.39%.
The test properties of the above-described composite materials of examples and comparative examples are shown in Table 1.
Table 1 microstructure and mechanical Properties of the composite Material
| Sample of | hardness/HRA | Density of the product |
| Comparative example | 87.6 | 97.39％ |
| Example 1 | 89.2 | 97.73％ |
| Example 2 | 90.6 | 98.54％ |
| Example 3 | 88.8 | 98.91％ |
As can be seen from the test results in Table 1, compared with the comparative example, the hardness and the compactness of the MoCoB-WCoB-based composite material prepared by the method are both increased, the compactness is increased by about 1.5%, the hardness is up to 90.6HRA, the hardness is increased by 3.0HRA, and a large breakthrough is achieved.
Claims (4)
1. A method for preparing a MoCoB-WCoB-based composite material, the method comprising: sequentially ball-milling, pressing and forming mixed powder of Mo, co, B and W powder to obtain a blank, and then sintering the blank in a vacuum carbon tube furnace to prepare the MoCoB-WCoB matrix composite;
the weight percentages are as follows: 34.0 to 46.0 percent of Mo, 38.0 to 52.0 percent of Co, 3.0 to 7.0 percent of B and 5.0 to 15.0 percent of W.
2. The method for preparing a MoCoB-WCoB-based composite material of claim 1 wherein said sintering process parameters are: raising the temperature from room temperature to 1350-1450 ℃ at a heating rate of 5-15 ℃/min, preserving the temperature for 0-60 min, and cooling to room temperature.
3. The method of preparing a MoCoB-WCoB-based composite material of claim 1 wherein said MoCoB-WCoB-based composite material comprises three phases: a MoCoB hard phase, a Co-based binder phase, and a WCoB reinforcement phase.
4. The method for preparing a MoCoB-WCoB-based composite material according to claim 1, wherein the MoCoB-WCoB-based composite material has a hardness of 88.8-90.6 HRA and a compactness of 97.73% -98.91%.
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| CN107904474A (en) * | 2017-11-02 | 2018-04-13 | 北京科技大学 | A kind of molybdenum cobalt boron Ternary Boride Base Cermets material and preparation method thereof |
| CN109299561A (en) * | 2018-10-09 | 2019-02-01 | 北京科技大学 | The method that screening can improve the transient metal doped element of Cemented Carbide Hardness |
| CN112080678A (en) * | 2020-09-15 | 2020-12-15 | 广东博杰特新材料科技有限公司 | Ternary boride alloy screw material and production process thereof |
| JP2021080542A (en) * | 2019-11-22 | 2021-05-27 | 株式会社日本製鋼所 | Sintered material and method for producing the same |
| CN113355611A (en) * | 2021-06-15 | 2021-09-07 | 上海海事大学 | Carbon fiber reinforced MoCoB metal ceramic and preparation method thereof |
| CN115011830A (en) * | 2022-05-30 | 2022-09-06 | 河源富马硬质合金股份有限公司 | Molybdenum-cobalt-boron ternary boride-based metal ceramic material and preparation method thereof |
-
2022
- 2022-11-25 CN CN202211489844.8A patent/CN116121579A/en active Pending
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|---|---|---|---|---|
| JPH05132734A (en) * | 1991-11-08 | 1993-05-28 | Japan Steel Works Ltd:The | Composite material having wear resistance and corrosion resistance |
| JPH09268361A (en) * | 1996-04-03 | 1997-10-14 | Sumitomo Metal Mining Co Ltd | Powder for boride cermet thermal spraying |
| JP2002080281A (en) * | 2000-09-07 | 2002-03-19 | Akita Prefecture | Wc-wb or wc-wb-w2b-based composite with high hardness and young' modulus and its manufacturing method |
| WO2002081764A1 (en) * | 2001-04-09 | 2002-10-17 | Widia Gmbh | Complex boride-cermet body, method for production and use of said body |
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