CN113210602A - Preparation method of copper-aluminum alloy coated diamond complex - Google Patents
Preparation method of copper-aluminum alloy coated diamond complex Download PDFInfo
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- CN113210602A CN113210602A CN202110541761.8A CN202110541761A CN113210602A CN 113210602 A CN113210602 A CN 113210602A CN 202110541761 A CN202110541761 A CN 202110541761A CN 113210602 A CN113210602 A CN 113210602A
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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
- B22F1/17—Metallic particles coated with metal
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/25—Diamond
- C01B32/28—After-treatment, e.g. purification, irradiation, separation or recovery
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Abstract
The invention discloses a preparation method of a copper-aluminum alloy coated diamond composite, which comprises the steps of firstly mixing aluminum powder and copper salt according to a certain proportion, and carrying out hydrothermal reaction at 80-120 ℃ for 30-90 min to obtain a copper-coated aluminum powder composite CA 1; and then uniformly mixing CA1 and the diamond according to a certain proportion, preserving heat for 1-3 h under the condition of non-oxidizing atmosphere at 660-800 ℃, cooling to room temperature along with the furnace, taking out, sieving, and cleaning to obtain the copper-aluminum alloy coated diamond complex.
Description
Technical Field
The invention relates to the technical field of superhard material application, in particular to a preparation method of a copper-aluminum alloy coated diamond composite.
Background
Diamond, as the hardest material for commercial applications, has the advantages of ultra-high hardness, insulation, ultra-high thermal conductivity and the like, so that the composite material and the product thereof are widely used in the fields of material processing, electronic packaging and heat dissipation substrates and the like. It is known that there is a large difference in properties between diamond and metal, which causes a serious problem of interface contact between diamond and metal interfaces such as copper and cemented carbide, and limits the further application space of diamond and shortens the service life of diamond products. At present, the surface of diamond is treated by methods such as salt bath plating, electroplating, chemical plating, vapor deposition and the like in industry, the interface bonding between the diamond and metal is improved to a certain extent, but the problems of poor bonding force, mainly physical bonding, high manufacturing cost and the like still exist. Therefore, the research and development of a new metal-coated diamond complex can greatly promote the development of the superhard material and electronic packaging industry.
Disclosure of Invention
The invention aims to provide a preparation method of a copper-aluminum alloy coated diamond composite, which is used for solving the problem of poor interface bonding between diamond and metal in the prior art.
The invention provides a preparation method of a copper-aluminum alloy coated diamond complex, which comprises the steps of mixing aluminum powder and copper salt according to a certain molar ratio, and carrying out hydrothermal reaction to obtain a copper-coated aluminum powder composite material CA 1; and then uniformly mixing CA1 and diamond according to a certain mass ratio to obtain an FCA1 mixed material, co-firing the FCA1 under a non-oxidizing atmosphere, cooling to room temperature along with a furnace, taking out, sieving, and cleaning to obtain the copper-aluminum alloy coated diamond complex.
Preferably, the copper salt used is a water-soluble copper salt including copper nitrate, copper sulfate and copper chloride.
Preferably, the soluble copper salt is added with deionized water to prepare 0.3 mol.L-1Then, the aluminum powder and the copper salt are mixed according to mol (Al: Cu) = (8-10: 3).
Preferably, the hydrothermal reaction temperature is 80-120 ℃, and the hydrothermal reaction heat preservation time is 30-90 min.
Preferably, uniformly mixing CA1 and diamond according to a mass ratio of m (CA1: diamond) = (2-9: 1) to obtain an FCA1 mixed material.
Preferably, the FCA1 mixed material is placed into a corundum crucible, co-fired at 660-800 ℃ under the non-oxidizing atmosphere condition, kept warm for 1-3 hours, cooled to room temperature along with a furnace, taken out, sieved and cleaned to obtain the copper-aluminum alloy coated diamond composite.
Preferably, the non-oxidizing atmosphere is vacuum or inert gas.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a preparation method of a copper-aluminum alloy coated diamond complex, which is characterized in that a copper-coated aluminum alloy material prepared by a hydrothermal method is used as a diamond surface modifier, aluminum in the modifier and diamond react in situ in a co-firing process with the diamond to generate carbide and form an aluminum coating layer, and further copper in the modifier and the aluminum coating layer form an alloy phase, so that a copper-aluminum alloy layer grows in situ on the surface of the diamond, and the interface contact between the diamond and metal can be effectively improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is an SEM image of a sample of example 1 of the present invention.
Figure 2 is an XRD pattern of a sample of example 1 of the invention.
FIG. 3 is an SEM image of a sample of example 2 of the present invention.
Figure 4 is an XRD pattern of a sample of example 2 of the invention.
FIG. 5 is an SEM image of a sample of example 3 according to the invention.
Figure 6 is an XRD pattern of a sample of example 3 of the 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.
The embodiment of the invention provides a preparation method of a copper-aluminum alloy coated diamond complex, which is realized by the following steps:
mixing aluminum powder and copper salt according to a certain molar ratio, and carrying out hydrothermal reaction to obtain a copper-coated aluminum powder composite material CA 1; and then uniformly mixing CA1 and diamond according to a certain mass ratio to obtain an FCA1 mixed material, co-firing the FCA1 under a non-oxidizing atmosphere, cooling to room temperature along with a furnace, taking out, sieving, and cleaning to obtain the copper-aluminum alloy coated diamond complex.
In the embodiment of the present invention, the copper salt used is a water-soluble copper salt including copper nitrate, copper sulfate and copper chloride.
In the embodiment of the invention, the soluble copper salt is added with deionized water to prepare 0.3 mol.L-1Then, the aluminum powder and the copper salt are mixed according to mol (Al: Cu) = (8-10: 3).
In the embodiment of the invention, the hydrothermal reaction temperature is 80-120 ℃, and the hydrothermal reaction heat preservation time is 30-90 min.
In the embodiment of the invention, CA1 and diamond are uniformly mixed according to a mass ratio of m (CA1: diamond) = (2-9: 1) to obtain an FCA1 mixed material.
In the embodiment of the invention, the FCA1 mixed material is placed into a corundum crucible, is co-fired at 660-800 ℃ under the non-oxidizing atmosphere condition, is kept warm for 1-3 hours, is cooled to room temperature along with a furnace, is taken out, and is sieved and cleaned to obtain the copper-aluminum alloy coated diamond composite.
In the embodiment of the invention, the non-oxidizing atmosphere condition is vacuum or inert gas is introduced.
The invention obtains the copper-aluminum alloy coated diamond complex under the condition of relatively low temperature by simple equipment.
Example 1
Firstly, copper nitrate is added with deionized water to prepare 0.3 mol.L-1Adding aluminum powder into the solution C1 according to the mol ratio of aluminum powder to copper salt (Al: Cu) = mol (8:3), then placing the solution C1 mixed with the aluminum powder into a reaction kettle for hydrothermal reaction at 80 ℃, and keeping the temperature for 90 min to obtain the copper-coated aluminum powder composite material CA 1; and then uniformly mixing CA1 and diamond according to the mass ratio of m (CA1: diamond) = (3:1) to obtain an FCA1 mixed material, co-firing the FCA1 at 800 ℃ under a vacuum condition, preserving heat for 1h, cooling the mixture to room temperature along with a furnace, taking out the cooled mixture, and screening and cleaning the cooled mixture to obtain the copper-aluminum alloy coated diamond composite. Fig. 1 shows SEM analysis of the cu-al alloy coated diamond composite prepared by the technique of example 1, which shows that a phase with metal particles is grown on the surface of the diamond. FIG. 2 shows an XRD pattern of the Cu-Al alloy coated diamond composite prepared by the technique of example 1, and XRD analysis shows that the surface of the diamond is growing Cu-Al alloy;
example 2
Firstly, copper sulfate is added with deionized water to prepare 0.3 mol.L-1Adding aluminum powder into the solution C1 according to the mol ratio of aluminum powder to copper salt (Al: Cu) = mol (10:3), then placing the solution C1 mixed with the aluminum powder into a reaction kettle for hydrothermal reaction at 120 ℃, and keeping the temperature for 30 min to obtain the copper-coated aluminum powder composite material CA 1; then uniformly mixing CA1 and diamond according to the mass ratio of m (CA1: diamond) = (2:1) to obtain an FCA1 mixed material, co-firing the FCA1 at 720 ℃ under a vacuum condition, preserving heat for 2 hours, cooling the FCA1 to room temperature along with a furnace, taking out the FCA1,and sieving and cleaning to obtain the copper-aluminum alloy coated diamond complex. Fig. 3 shows an SEM analysis of the cu-al alloy coated diamond composite prepared by the technique of example 2, which shows that a phase with metal particles is grown on the surface of the diamond. FIG. 4 shows an XRD pattern of the Cu-Al alloy coated diamond composite prepared by the technique of example 2, and XRD analysis shows that Cu-Al alloy grows on the surface of the diamond;
example 3
Firstly, copper chloride is added with deionized water to prepare 0.3 mol.L-1Adding aluminum powder into the solution C1 according to the mol ratio of aluminum powder to copper salt (Al: Cu) = mol (9:3), then placing the solution C1 mixed with the aluminum powder into a reaction kettle for hydrothermal reaction at 100 ℃, and keeping the temperature for 60 min to obtain the copper-coated aluminum powder composite material CA 1; and then uniformly mixing CA1 and diamond according to the mass ratio of m (CA1: diamond) = (9:1) to obtain an FCA1 mixed material, co-firing the FCA1 at 660 ℃ under a vacuum condition, preserving heat for 3 hours, cooling to room temperature along with a furnace, taking out, sieving, and cleaning to obtain the copper-aluminum alloy coated diamond composite. FIG. 5 shows an SEM image of a copper aluminum alloy coated diamond composite prepared by the technique of example 3; fig. 6 shows an XRD pattern of the cu-al alloy coated diamond composite prepared by the technique of this example 3, and XRD analysis shows that cu-al alloy is grown on the diamond surface.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (7)
1. A preparation method of a copper-aluminum alloy coated diamond composite is characterized in that firstly, aluminum powder and copper salt are mixed according to a certain molar ratio and then are subjected to hydrothermal reaction to obtain a copper-coated aluminum powder composite material CA 1; and then uniformly mixing CA1 and diamond according to a certain mass ratio to obtain an FCA1 mixed material, co-firing the FCA1 under a non-oxidizing atmosphere, cooling to room temperature along with a furnace, taking out, sieving, and cleaning to obtain the copper-aluminum alloy coated diamond complex.
2. The method of claim 1, wherein the copper salt is a water soluble copper salt selected from the group consisting of copper nitrate, copper sulfate, and copper chloride.
3. The method of claim 1, wherein the soluble copper salt is added with deionized water to make 0.3 mol-L-1Then, the aluminum powder and the copper salt are mixed according to mol (Al: Cu) = (8-10: 3).
4. The method for preparing the copper-aluminum alloy coated diamond composite as claimed in claim 1, wherein the hydrothermal reaction temperature is 80-120 ℃ and the hydrothermal reaction holding time is 30-90 min.
5. The method for preparing the copper-aluminum alloy coated diamond composite according to claim 1, wherein the CA1 and the diamond are uniformly mixed according to a mass ratio of m (CA1: diamond) = (2-9: 1) to obtain an FCA1 mixed material.
6. The method for preparing the copper-aluminum alloy coated diamond composite as claimed in claim 1, wherein the FCA1 mixed material is placed into a corundum crucible, co-fired at 660-800 ℃ under the non-oxidizing atmosphere condition, kept warm for 1-3 h, cooled to room temperature along with a furnace, taken out, sieved and cleaned to obtain the copper-aluminum alloy coated diamond composite.
7. The method of claim 1, wherein the non-oxidizing atmosphere is vacuum or inert gas.
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Citations (8)
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|---|---|---|---|---|
| CN102248159A (en) * | 2011-07-26 | 2011-11-23 | 北京工业大学 | Preparation method of silver-coated aluminum powder |
| CN105986158A (en) * | 2015-02-12 | 2016-10-05 | 中国科学院宁波材料技术与工程研究所 | High-thermal-conductivity diamond-metal composite material and preparation method thereof |
| CN106312056A (en) * | 2016-09-29 | 2017-01-11 | 许昌学院 | Diamond surface metallization method |
| US20170045314A1 (en) * | 2014-04-25 | 2017-02-16 | Denka Company Limited | Aluminum-diamond composite, and heat dissipating component using same |
| WO2019246321A1 (en) * | 2018-06-20 | 2019-12-26 | Desktop Metal, Inc. | Methods and compositions for the preparation of powders for binder-based three-dimensional additive metal manufacturing |
| CN111136260A (en) * | 2018-11-02 | 2020-05-12 | 江苏锋泰工具有限公司 | Diamond coating process |
| CN111318688A (en) * | 2020-03-24 | 2020-06-23 | 昆明理工大学 | Preparation method and application of aluminum-based conductive powder |
| CN112272652A (en) * | 2018-06-04 | 2021-01-26 | 积水化学工业株式会社 | Diamond particles, diamond-containing composition, and method for producing diamond particles |
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2021
- 2021-05-18 CN CN202110541761.8A patent/CN113210602B/en active Active
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| CN102248159A (en) * | 2011-07-26 | 2011-11-23 | 北京工业大学 | Preparation method of silver-coated aluminum powder |
| US20170045314A1 (en) * | 2014-04-25 | 2017-02-16 | Denka Company Limited | Aluminum-diamond composite, and heat dissipating component using same |
| CN105986158A (en) * | 2015-02-12 | 2016-10-05 | 中国科学院宁波材料技术与工程研究所 | High-thermal-conductivity diamond-metal composite material and preparation method thereof |
| CN106312056A (en) * | 2016-09-29 | 2017-01-11 | 许昌学院 | Diamond surface metallization method |
| CN112272652A (en) * | 2018-06-04 | 2021-01-26 | 积水化学工业株式会社 | Diamond particles, diamond-containing composition, and method for producing diamond particles |
| WO2019246321A1 (en) * | 2018-06-20 | 2019-12-26 | Desktop Metal, Inc. | Methods and compositions for the preparation of powders for binder-based three-dimensional additive metal manufacturing |
| CN111136260A (en) * | 2018-11-02 | 2020-05-12 | 江苏锋泰工具有限公司 | Diamond coating process |
| CN111318688A (en) * | 2020-03-24 | 2020-06-23 | 昆明理工大学 | Preparation method and application of aluminum-based conductive powder |
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