CN111889676A - Method for preparing diamond copper-based composite material by additive manufacturing process - Google Patents

Method for preparing diamond copper-based composite material by additive manufacturing process Download PDF

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CN111889676A
CN111889676A CN202010784749.5A CN202010784749A CN111889676A CN 111889676 A CN111889676 A CN 111889676A CN 202010784749 A CN202010784749 A CN 202010784749A CN 111889676 A CN111889676 A CN 111889676A
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composite material
diamond
powder
plating
carbide
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CN111889676B (en
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苏振华
朱嘉琦
曹文鑫
代兵
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Harbin Institute of Technology
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Harbin Institute of Technology
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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
    • B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
    • 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
    • B22F3/1003—Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007—Atmosphere
    • 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
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • B22F3/15—Hot isostatic pressing
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
    • 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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/18—Pretreatment of the material to be coated
    • C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
    • C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
    • C23C18/1886—Multistep pretreatment
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/31—Coating with metals
    • C23C18/38—Coating with copper
    • C23C18/40—Coating with copper using reducing agents
    • C23C18/405—Formaldehyde
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

Abstract

The invention discloses a method for preparing a diamond copper-based composite material by an additive manufacturing process, and relates to a method for preparing a diamond copper-based composite material. The invention aims to solve the problem that the prior art can not prepare the diamond copper-based composite material with high thermal conductivity, high density and complex shape. The method comprises the following steps: firstly, preparing plated diamond powder; secondly, mixing; thirdly, selecting laser melting; fourthly, cold isostatic pressing technology; fifthly, sintering; sixthly, hot isostatic pressing technology; or the method comprises the following steps: firstly, preparing plated diamond powder; secondly, mixing; thirdly, selecting laser melting; fourthly, sintering; and fifthly, hot isostatic pressing technology. The invention is used for preparing the diamond copper-based composite material by the additive manufacturing process.

Description

Method for preparing diamond copper-based composite material by additive manufacturing process
Technical Field
The invention relates to a method for preparing a diamond copper-based composite material.
Background
Nowadays, the miniaturization and integration of electrical devices are rapidly progressing, and the power density of electrical devices is inevitably increasing. How to effectively thermally manage electrical devices has been a research hotspot today. The general study directions fall into two categories: firstly, high-efficiency heat management materials such as metal (aluminum, copper and the like) and diamond enhanced heat conduction metal matrix composite materials are searched; and secondly, the optimal heat dissipation structure is found through numerical simulation by optimizing the heat dissipation structure, so that the heat dissipation efficiency is improved, and meanwhile, due to the high-speed development of the additive manufacturing field, the special heat dissipation structure can be directly formed through an additive manufacturing technology.
The diamond reinforced metal-based composite material is better in heat-conducting property by using a copper-based composite material. The heat conductivity of the diamond reinforced copper-based composite material can be greatly improved by virtue of the good heat conductivity of the matrix and the high heat conductivity of diamond. The existing mature processes such as SPS, high-pressure auxiliary infiltration and the like can obtain the diamond copper-based composite material with high thermal conductivity and high density, but the process adaptability is poor, the complex shape cannot be formed, and only parts with simple shapes such as sheets, blocks and the like can be obtained. Meanwhile, due to the higher doping amount of the diamond, the material cannot be further processed in a later processing mode. This makes the preparation of diamond copper-based composite materials with high thermal conductivity, high density and complex shape almost an unrealizable problem. This is also the biggest obstacle that currently limits the applications of composite materials.
Disclosure of Invention
The invention provides a method for preparing a diamond copper-based composite material by an additive manufacturing process, aiming at solving the problem that the prior art cannot prepare the diamond copper-based composite material with high thermal conductivity, high density and complex shape.
A method for preparing a diamond copper-based composite material by an additive manufacturing process is carried out according to the following steps:
firstly, preparing the plated diamond powder:
plating a composite plating layer on the surface of the diamond powder by a plating process to obtain plated diamond powder;
the composite coating consists of an outer coating and an inner coating; the outer plating layer is a pure copper plating layer; the inner plating layer is a carbide plating layer or a metal simple substance plating layer;
the thickness of the carbide coating layer is 100 nm-500 nm, and the thickness of the metal simple substance coating layer is 100 nm-1 mu m;
the mass percentage content of the pure copper plating layer in the diamond powder after plating is 20-70%;
the particle size of the diamond powder is 20-400 μm;
secondly, mixing:
mechanically and uniformly mixing the plated diamond powder and pure copper powder to obtain mixed powder;
the volume ratio of the diamond powder after plating to the pure copper powder is 1 (0.1-3); the pure copper powder is pure copper powder with the particle size of 2-6 mu m or pure copper powder with the particle size of 23-53 mu m;
thirdly, selective laser melting:
in selective laser melting equipment, controlling the oxygen content to be lower than 0.1%, preheating a substrate to 20-200 ℃, carrying out laser forming by using mixed powder under the conditions that the laser power is 30-500W, the scanning speed is 1-1500 mm/s, the spot diameter is 0.05-1 mm, the substrate temperature is 20-200 ℃ and the single powder spreading thickness of the substrate is 0.1-0.4 mm, and finally stopping heating, and taking the formed composite material off the substrate after the substrate is cooled;
fourthly, cold isostatic pressing technology:
placing the formed composite material into a jacket, vacuumizing until the pressure is less than 10Pa, placing the jacketed composite material into a cold isostatic press, keeping the pressure for 2-20 min under the condition that the hydrostatic pressure is 50-400 MPa, and removing the jacket to obtain a densified composite material;
fifthly, sintering:
placing the densified composite material in a vacuum furnace, vacuumizing until the pressure is less than 1Pa, and preserving the heat for 0.5-3 h under the condition that the sintering temperature is 850-1100 ℃ to obtain the sintered composite material;
or placing the densified composite material in an atmosphere furnace, and preserving the heat for 0.5-4 h under the conditions of protecting the atmosphere and sintering the composite material at the temperature of 850-1100 ℃ to obtain the sintered composite material;
sixthly, hot isostatic pressing technology:
and under the conditions that the hot isostatic pressing temperature is 850-1050 ℃ and the hot isostatic pressing pressure is 50-200 MPa, keeping the temperature and the pressure of the sintered composite material for 0.5-4 h to obtain the diamond copper-based composite material.
A method for preparing a diamond copper-based composite material by an additive manufacturing process is carried out according to the following steps:
firstly, preparing the plated diamond powder:
plating a composite plating layer on the surface of the diamond powder by a plating process to obtain plated diamond powder;
the composite coating consists of an outer coating and an inner coating; the outer plating layer is a pure copper plating layer; the inner plating layer is a carbide plating layer or a metal simple substance plating layer;
the thickness of the carbide coating layer is 100 nm-500 nm, and the thickness of the metal simple substance coating layer is 100 nm-1 mu m;
the mass percentage content of the pure copper plating layer in the diamond powder after plating is 20-70%;
the particle size of the diamond powder is 20-400 μm;
secondly, mixing:
mechanically and uniformly mixing the plated diamond powder and pure copper powder to obtain mixed powder;
the pure copper powder is a mixture of pure copper powder with the particle size of 23-53 mu m and pure copper powder with the particle size of 2-6 mu m;
the volume ratio of the diamond powder after plating to the pure copper powder with the particle size of 23-53 mu m is 1 (0.1-3); the volume ratio of the diamond powder after plating to the pure copper powder with the grain diameter of 2-6 mu m is 1 (0.1-3);
thirdly, selective laser melting:
in selective laser melting equipment, controlling the oxygen content to be lower than 0.1%, preheating a substrate to 20-200 ℃, carrying out laser forming by using mixed powder under the conditions that the laser power is 30-500W, the scanning speed is 1-1500 mm/s, the spot diameter is 0.05-1 mm, the substrate temperature is 20-200 ℃ and the single powder spreading thickness of the substrate is 0.1-0.4 mm, and finally stopping heating, and taking the formed composite material off the substrate after the substrate is cooled;
fourthly, sintering:
placing the molded composite material in a vacuum furnace, vacuumizing until the pressure is less than 1Pa, and preserving heat for 0.5-3 h under the condition that the sintering temperature is 850-1100 ℃ to obtain the sintered composite material;
or placing the formed composite material in an atmosphere furnace, and preserving heat for 0.5-4 h under the conditions of protecting atmosphere and sintering temperature of 850-1100 ℃ to obtain the sintered composite material;
fifthly, hot isostatic pressing technology:
and under the conditions that the hot isostatic pressing temperature is 850-1050 ℃ and the hot isostatic pressing pressure is 50-200 MPa, keeping the temperature and the pressure of the sintered composite material for 0.5-4 h to obtain the diamond copper-based composite material.
The invention has the beneficial effects that: the invention can realize the molding of the complex structure of the diamond copper-based composite material with high thermal conductivity (more than 480W/mK) and relative density of more than 98 percent. The interface bonding force between the matrix and the diamond is enhanced through the inner plating layer on the surface of the diamond; and the outer pure copper plating layer realizes selective laser melting sintering bonding and avoids the agglomeration of the diamond reinforcement body. The subsequent cold isostatic pressing and sintering technology realizes the further densification of the composite material, and can change the original internal through holes into closed holes to be used for laying a cushion for the subsequent hot isostatic pressing process. The hot isostatic pressing technology realizes the final densification of the material, and simultaneously, the diamond and the matrix form stronger interface combination through the element diffusion effect in the high-temperature and high-pressure environment. Finally, the complex component of the diamond copper-based composite material with high thermal conductivity and high density is formed.
The invention provides a method for preparing a diamond copper-based composite material by an additive manufacturing process.
Detailed Description
The technical solution of the present invention is not limited to the specific embodiments listed below, and includes any combination of the specific embodiments.
The first embodiment is as follows: the method for preparing the diamond copper-based composite material by the additive manufacturing process is carried out according to the following steps:
firstly, preparing the plated diamond powder:
plating a composite plating layer on the surface of the diamond powder by a plating process to obtain plated diamond powder;
the composite coating consists of an outer coating and an inner coating; the outer plating layer is a pure copper plating layer; the inner plating layer is a carbide plating layer or a metal simple substance plating layer;
the thickness of the carbide coating layer is 100 nm-500 nm, and the thickness of the metal simple substance coating layer is 100 nm-1 mu m;
the mass percentage content of the pure copper plating layer in the diamond powder after plating is 20-70%;
the particle size of the diamond powder is 20-400 μm;
secondly, mixing:
mechanically and uniformly mixing the plated diamond powder and pure copper powder to obtain mixed powder;
the volume ratio of the diamond powder after plating to the pure copper powder is 1 (0.1-3); the pure copper powder is pure copper powder with the particle size of 2-6 mu m or pure copper powder with the particle size of 23-53 mu m;
thirdly, selective laser melting:
in selective laser melting equipment, controlling the oxygen content to be lower than 0.1%, preheating a substrate to 20-200 ℃, carrying out laser forming by using mixed powder under the conditions that the laser power is 30-500W, the scanning speed is 1-1500 mm/s, the spot diameter is 0.05-1 mm, the substrate temperature is 20-200 ℃ and the single powder spreading thickness of the substrate is 0.1-0.4 mm, and finally stopping heating, and taking the formed composite material off the substrate after the substrate is cooled;
fourthly, cold isostatic pressing technology:
placing the formed composite material into a jacket, vacuumizing until the pressure is less than 10Pa, placing the jacketed composite material into a cold isostatic press, keeping the pressure for 2-20 min under the condition that the hydrostatic pressure is 50-400 MPa, and removing the jacket to obtain a densified composite material;
fifthly, sintering:
placing the densified composite material in a vacuum furnace, vacuumizing until the pressure is less than 1Pa, and preserving the heat for 0.5-3 h under the condition that the sintering temperature is 850-1100 ℃ to obtain the sintered composite material;
or placing the densified composite material in an atmosphere furnace, and preserving the heat for 0.5-4 h under the conditions of protecting the atmosphere and sintering the composite material at the temperature of 850-1100 ℃ to obtain the sintered composite material;
sixthly, hot isostatic pressing technology:
and under the conditions that the hot isostatic pressing temperature is 850-1050 ℃ and the hot isostatic pressing pressure is 50-200 MPa, keeping the temperature and the pressure of the sintered composite material for 0.5-4 h to obtain the diamond copper-based composite material.
The beneficial effects of the embodiment are as follows:
the embodiment can realize the molding of the complex structure of the diamond copper-based composite material with high heat conductivity (more than 480W/mK) and relative density of more than 98 percent. The interface bonding force between the matrix and the diamond is enhanced through the inner plating layer on the surface of the diamond; and the outer pure copper plating layer realizes selective laser melting sintering bonding and avoids the agglomeration of the diamond reinforcement body. The subsequent cold isostatic pressing and sintering technology realizes the further densification of the composite material, and can change the original internal through holes into closed holes to be used for laying a cushion for the subsequent hot isostatic pressing process. The hot isostatic pressing technology realizes the final densification of the material, and simultaneously, the diamond and the matrix form stronger interface combination through the element diffusion effect in the high-temperature and high-pressure environment. Finally, the complex component of the diamond copper-based composite material with high thermal conductivity and high density is formed.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the carbide coating layer in the first step is titanium carbide, tungsten carbide, zirconium carbide, boron carbide, chromium carbide or molybdenum carbide; the metal simple substance plating layer in the step one is Ti, W, Zr, Cr, Mo, V or Nb. The rest is the same as the first embodiment.
The third concrete implementation mode: this embodiment is different from the first or second embodiment in that: the plating process in the first step is physical vapor deposition, chemical plating, electroplating or salt bath plating. The other is the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the diamond powder in the step one is single crystal diamond powder; the substrate in the third step is a pure copper plate. The others are the same as the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the mechanical mixing in the step two is that the planet ball mill is used for mixing for 30-60 min; the laser forming in the third step is specifically carried out according to the following steps: the first layer scans for two periods, then each layer scans for one period, the scanning directions of the layers are in an orthogonal relation, and the overlapping rate of the scanning intervals is 0-50%; and fifthly, the protective atmosphere is inert gas or reducing gas, and the reducing gas is hydrogen or methane. The rest is the same as the first to fourth embodiments.
The sixth specific implementation mode: a method for preparing a diamond copper-based composite material by an additive manufacturing process is carried out according to the following steps:
firstly, preparing the plated diamond powder:
plating a composite plating layer on the surface of the diamond powder by a plating process to obtain plated diamond powder;
the composite coating consists of an outer coating and an inner coating; the outer plating layer is a pure copper plating layer; the inner plating layer is a carbide plating layer or a metal simple substance plating layer;
the thickness of the carbide coating layer is 100 nm-500 nm, and the thickness of the metal simple substance coating layer is 100 nm-1 mu m;
the mass percentage content of the pure copper plating layer in the diamond powder after plating is 20-70%;
the particle size of the diamond powder is 20-400 μm;
secondly, mixing:
mechanically and uniformly mixing the plated diamond powder and pure copper powder to obtain mixed powder;
the pure copper powder is a mixture of pure copper powder with the particle size of 23-53 mu m and pure copper powder with the particle size of 2-6 mu m;
the volume ratio of the diamond powder after plating to the pure copper powder with the particle size of 23-53 mu m is 1 (0.1-3); the volume ratio of the diamond powder after plating to the pure copper powder with the grain diameter of 2-6 mu m is 1 (0.1-3);
thirdly, selective laser melting:
in selective laser melting equipment, controlling the oxygen content to be lower than 0.1%, preheating a substrate to 20-200 ℃, carrying out laser forming by using mixed powder under the conditions that the laser power is 30-500W, the scanning speed is 1-1500 mm/s, the spot diameter is 0.05-1 mm, the substrate temperature is 20-200 ℃ and the single powder spreading thickness of the substrate is 0.1-0.4 mm, and finally stopping heating, and taking the formed composite material off the substrate after the substrate is cooled;
fourthly, sintering:
placing the molded composite material in a vacuum furnace, vacuumizing until the pressure is less than 1Pa, and preserving heat for 0.5-3 h under the condition that the sintering temperature is 850-1100 ℃ to obtain the sintered composite material;
or placing the formed composite material in an atmosphere furnace, and preserving heat for 0.5-4 h under the conditions of protecting atmosphere and sintering temperature of 850-1100 ℃ to obtain the sintered composite material;
fifthly, hot isostatic pressing technology:
and under the conditions that the hot isostatic pressing temperature is 850-1050 ℃ and the hot isostatic pressing pressure is 50-200 MPa, keeping the temperature and the pressure of the sintered composite material for 0.5-4 h to obtain the diamond copper-based composite material.
The beneficial effects of the embodiment are as follows:
the embodiment can realize the molding of the complex structure of the diamond copper-based composite material with high heat conductivity (more than 480W/mK) and relative density of more than 98 percent. The interface bonding force between the matrix and the diamond is enhanced through the inner plating layer on the surface of the diamond; and the outer pure copper plating layer realizes selective laser melting sintering bonding and avoids the agglomeration of the diamond reinforcement body. The hot isostatic pressing technology realizes the final densification of the material, and simultaneously, the diamond and the matrix form stronger interface bonding through the element diffusion effect in the high-temperature and high-pressure environment. Finally, the complex component of the diamond copper-based composite material with high thermal conductivity and high density is formed.
The seventh embodiment: the sixth embodiment is different from the sixth embodiment in that: the carbide coating layer in the first step is titanium carbide, tungsten carbide, zirconium carbide, boron carbide, chromium carbide or molybdenum carbide; the metal simple substance plating layer in the step one is Ti, W, Zr, Cr, Mo, V or Nb. The rest is the same as the sixth embodiment.
The specific implementation mode is eight: the present embodiment differs from one of the sixth or seventh embodiments in that: the plating process in the first step is physical vapor deposition, chemical plating, electroplating or salt bath plating. The others are the same as the sixth or seventh embodiments.
When the metal simple substance plating layer in the first step is a tungsten layer, the plating process is magnetron sputtering, and the method specifically comprises the following steps: the plating target material is pure tungsten target material, the temperature in the furnace is 700-900 ℃, the plating time is 10-60 min, then the plated diamond is put into a vacuum furnace, and the temperature is kept for 0.5-2 h under the conditions that the vacuum degree is lower than 0.1Pa and the temperature is 900-1100 ℃, so as to obtain the diamond plated with the inner plating layer.
When the outer plating layer is plated in the first step, the plating process is electroless plating, and is specifically carried out according to the following steps:
a. sensitization:
placing the diamond plated with the inner plating layer in a sensitizing solution, stirring for 5-30 min, then taking out, and cleaning with deionized water to obtain a sensitized diamond;
the sensitizing solution is composed of SnCl237% by mass of HCl and H2O composition; the SnCl2The mass ratio of the HCl to 37% by mass of HCl is 1 (1.5-3); the SnCl2And H2The mass ratio of O is 1 (20-30);
b. and (3) activation:
placing the sensitized diamond in an activating solution, stirring for 5-30 min, taking out, and washing with deionized water to obtain an activated diamond;
the activating solution is PdCl2And H2O composition; the PdCl2And H2The mass ratio of O is 1 (1000-5000);
c. plating:
placing the activated diamond in a plating solution, adding 1mL of formaldehyde into every 100mL of the plating solution, stirring for 10-40 min, taking out, ultrasonically cleaning, and weighing;
the plating solution is CuSO4·H2O, EDTA disodium salt, potassium sodium tartrate and H2O, and dissolved in NaOHAdjusting the pH value of the solution to 12-13; the CuSO4·H2The mass ratio of O to EDTA disodium salt is 1 (0.8-1.2); the CuSO4·H2The mass ratio of O to potassium sodium tartrate is 1 (0.8-1.2); the CuSO4·H2The mass ratio of O to water is 1 (70-150).
If the weight increase of the plating layer does not meet the design requirement, the previous operation is continuously repeated after the plating solution is replaced.
The specific implementation method nine: this embodiment differs from one of the sixth to eighth embodiments in that: the diamond powder in the step one is single crystal diamond powder; the substrate in the third step is a pure copper plate. The others are the same as the embodiments six to eight.
The detailed implementation mode is ten: the present embodiment differs from one of the sixth to ninth embodiments in that: the mechanical mixing in the step two is that the planet ball mill is used for mixing for 30-60 min; the laser forming in the third step is specifically carried out according to the following steps: the first layer scans for two periods, then each layer scans for one period, the scanning directions of the layers are in an orthogonal relation, and the overlapping rate of the scanning intervals is 0-50%; the protective atmosphere in the fourth step is inert gas or reducing gas, and the reducing gas is hydrogen or methane. The others are the same as in the sixth to ninth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows:
a method for preparing a diamond copper-based composite material by an additive manufacturing process is carried out according to the following steps:
firstly, preparing the plated diamond powder:
plating a composite plating layer on the surface of the diamond by a plating process to obtain plated diamond powder;
the composite coating consists of an outer coating and an inner coating;
the outer plating layer is a pure copper plating layer; the inner plating layer is a carbide plating layer; the thickness of the carbide coating layer is 200 nm-500 nm;
the mass percentage content of the pure copper plating layer in the diamond powder after plating is 30 percent;
the particle size of the diamond powder is 80 μm;
secondly, mixing:
mechanically and uniformly mixing the plated diamond powder and pure copper powder to obtain mixed powder;
the volume ratio of the diamond powder to the pure copper powder after plating is 1: 1; the pure copper powder is pure copper powder with the particle size of 23-53 mu m;
thirdly, selective laser melting:
in selective laser melting equipment, introducing high-purity argon to ensure that the oxygen content in a forming cavity is lower than 0.1%, preheating a substrate to 200 ℃, carrying out laser forming by using mixed powder according to a designed shape under the conditions that the laser power is 30W, the scanning speed is 1500mm/s, the spot diameter is 0.075mm, the substrate temperature is 200 ℃ and the single powder laying thickness of the substrate is 0.1mm, and finally stopping heating, and taking the formed composite material off the substrate after the substrate is cooled;
fourthly, cold isostatic pressing technology:
placing the formed composite material into a latex sheath, vacuumizing until the pressure is 1Pa, placing the sheathed composite material into a cold isostatic press, keeping the pressure for 5min under the condition that the hydrostatic pressure is 250MPa, taking out the sheathed composite material after pressure relief, and removing the sheath to obtain a densified composite material;
fifthly, sintering:
placing the densified composite material in a vacuum furnace, vacuumizing until the pressure is less than 1Pa, and preserving heat for 2 hours at the sintering temperature of 1000 ℃ to obtain the sintered composite material;
sixthly, hot isostatic pressing technology:
and keeping the temperature and pressure of the sintered composite material for 2h under the conditions that the hot isostatic pressing temperature is 1000 ℃ and the hot isostatic pressing pressure is 120MPa, so as to obtain the diamond copper-based composite material.
The carbide coating layer in the first step is titanium carbide.
When the inner plating layer is plated, the plating process is salt bath plating, and is specifically carried out according to the following steps: firstly, mixing diamond powder, titanium powder, NaCl and KCl according to the mass ratio of 1:1:1:1.2, then preserving heat for 1h at the temperature of 900 ℃, taking out after the temperature is cooled, and washing with deionized water to obtain titanium carbide coated diamond;
when the outer plating layer is plated, the plating process is electroless plating, and is specifically carried out according to the following steps:
a. sensitization:
placing the diamond plated with the inner plating layer in a sensitizing solution, stirring for 15min, taking out, and cleaning with deionized water to obtain a sensitized diamond;
the sensitizing solution is composed of SnCl237% by mass of HCl and H2O composition; the SnCl2The mass ratio of the HCl to the HCl with the concentration of 37 percent by mass is 1: 2; the SnCl2And H2The mass ratio of O is 1: 25;
b. and (3) activation:
placing the sensitized diamond in an activating solution, stirring for 20min, taking out, and washing with deionized water to obtain an activated diamond;
the activating solution is PdCl2And H2O composition; the PdCl2And H2The mass ratio of O is 1: 3000;
c. plating:
placing the activated diamond in a plating solution, adding 1mL of formaldehyde into every 100mL of the plating solution, stirring for 30min, taking out, ultrasonically cleaning, and weighing;
the plating solution is CuSO4·H2O, EDTA disodium salt, potassium sodium tartrate and H2O, and adjusting the pH to 12 by using NaOH solution; the CuSO4·H2The mass ratio of O to EDTA disodium salt is 1: 1; the CuSO4·H2The mass ratio of O to potassium sodium tartrate is 1: 1; the CuSO4·H2The mass ratio of O to water is 1: 100;
if the weight increase of the plating layer does not meet the design requirement, the previous operation is continuously repeated after the plating solution is replaced.
The diamond powder in the step one is single crystal diamond powder.
The substrate in the third step is a pure copper plate.
And the mechanical mixing in the step two is that the planet ball mill is used for mixing for 30 min.
The laser forming according to the designed shape in the third step is specifically carried out according to the following steps: the first layer is scanned for two periods, then each layer is scanned for one period, the scanning directions of the layers are in an orthogonal relation, the overlapping rate of the scanning intervals is 50%, and a block body with the size of 4 multiplied by 10mm is obtained.
The density of the diamond copper-based composite material prepared in the first example is 99.2%, and the thermal conductivity is 482W/mK.
Example two:
a method for preparing a diamond copper-based composite material by an additive manufacturing process is carried out according to the following steps:
firstly, preparing the plated diamond powder:
plating a composite plating layer on the surface of the diamond by a plating process to obtain plated diamond powder;
the composite coating consists of an outer coating and an inner coating;
the outer plating layer is a pure copper plating layer; the inner plating layer is a metal simple substance plating layer;
the thickness of the metal simple substance plating layer is 0.2-0.5 μm;
the mass percentage content of the pure copper plating layer in the diamond powder after plating is 40 percent;
the particle size of the diamond powder is 200 mu m;
secondly, mixing:
mechanically and uniformly mixing the plated diamond powder and pure copper powder to obtain mixed powder;
the pure copper powder is a mixture of pure copper powder with the particle size of 23-53 mu m and pure copper powder with the particle size of 2-6 mu m;
the volume ratio of the diamond powder after plating to the pure copper powder with the particle size of 23-53 mu m is 7: 2; the volume ratio of the diamond powder after plating to the pure copper powder with the grain diameter of 2-6 mu m is 7: 1;
thirdly, selective laser melting:
in selective laser melting equipment, introducing high-purity argon to ensure that the oxygen content in a forming cavity is lower than 0.1%, preheating a substrate to 200 ℃, carrying out laser forming by using mixed powder according to a designed shape under the conditions that the laser power is 100W, the scanning speed is 1500mm/s, the spot diameter is 0.075mm, the substrate temperature is 200 ℃ and the single powder laying thickness of the substrate is 0.22mm, and finally stopping heating, and taking the formed composite material off the substrate after the substrate is cooled;
fourthly, sintering:
placing the molded composite material in a vacuum furnace, vacuumizing until the pressure is less than 1Pa, and preserving heat for 4 hours at the sintering temperature of 1040 ℃ to obtain the sintered composite material;
fifthly, hot isostatic pressing technology:
and (3) keeping the temperature and pressure of the sintered composite material for 2h under the conditions that the hot isostatic pressing temperature is 1050 ℃ and the hot isostatic pressing pressure is 170MPa, so as to obtain the diamond copper-based composite material.
The metal simple substance plating layer in the step one is a tungsten layer.
When the inner plating layer is plated, the plating process is magnetron sputtering, and is specifically carried out according to the following steps: the plating target material is pure tungsten target material, the temperature in the furnace is 800 ℃, the plating time is 40min, then the plated diamond is put into a vacuum furnace, and the temperature is kept for 30min under the conditions that the vacuum degree is lower than 0.1Pa and the temperature is 1000 ℃.
When the outer plating layer is plated, the plating process is electroless plating, and is specifically carried out according to the following steps:
placing the diamond plated with the inner plating layer in a sensitizing solution, stirring for 15min, taking out, and cleaning with deionized water to obtain a sensitized diamond;
the sensitizing solution is composed of SnCl237% by mass of HCl and H2O composition; the SnCl2The mass ratio of the HCl to the HCl with the concentration of 37 percent by mass is 1: 2; the SnCl2And H2The mass ratio of O is 1: 25;
b. and (3) activation:
placing the sensitized diamond in an activating solution, stirring for 20min, taking out, and washing with deionized water to obtain an activated diamond;
the activating solution is PdCl2And H2O composition; the PdCl2And H2The mass ratio of O is 1: 3000;
c. plating:
placing the activated diamond in a plating solution, adding 1mL of formaldehyde into every 100mL of the plating solution, stirring for 30min, taking out, ultrasonically cleaning, and weighing;
the plating solution is CuSO4·H2O, EDTA disodium salt, potassium sodium tartrate and H2O, and adjusting the pH to 12 by using NaOH solution; the CuSO4·H2The mass ratio of O to EDTA disodium salt is 1: 1; the CuSO4·H2The mass ratio of O to potassium sodium tartrate is 1: 1; the CuSO4·H2The mass ratio of O to water is 1: 100;
if the weight increase of the plating layer does not meet the design requirement, the previous operation is continuously repeated after the plating solution is replaced.
The diamond powder in the step one is single crystal diamond powder.
The substrate in the third step is a pure copper plate.
And the mechanical mixing in the step two is that the planet ball mill is used for mixing for 60 min.
The laser forming according to the designed shape in the third step is specifically carried out according to the following steps: the first layer is scanned for two periods, then each layer is scanned for one period, the scanning directions of the layers are in an orthogonal relation, the overlapping rate of the scanning intervals is 50%, and a block body with the size of 4 multiplied by 10mm is obtained.
The density of the diamond copper-based composite material prepared in the first example is 98.6%, and the thermal conductivity is 673W/mK.

Claims (10)

1. A method for preparing a diamond copper-based composite material by an additive manufacturing process is characterized by comprising the following steps of:
firstly, preparing the plated diamond powder:
plating a composite plating layer on the surface of the diamond powder by a plating process to obtain plated diamond powder;
the composite coating consists of an outer coating and an inner coating; the outer plating layer is a pure copper plating layer; the inner plating layer is a carbide plating layer or a metal simple substance plating layer;
the thickness of the carbide coating layer is 100 nm-500 nm, and the thickness of the metal simple substance coating layer is 100 nm-1 mu m;
the mass percentage content of the pure copper plating layer in the diamond powder after plating is 20-70%;
the particle size of the diamond powder is 20-400 μm;
secondly, mixing:
mechanically and uniformly mixing the plated diamond powder and pure copper powder to obtain mixed powder;
the volume ratio of the diamond powder after plating to the pure copper powder is 1 (0.1-3); the pure copper powder is pure copper powder with the particle size of 2-6 mu m or pure copper powder with the particle size of 23-53 mu m;
thirdly, selective laser melting:
in selective laser melting equipment, controlling the oxygen content to be lower than 0.1%, preheating a substrate to 20-200 ℃, carrying out laser forming by using mixed powder under the conditions that the laser power is 30-500W, the scanning speed is 1-1500 mm/s, the spot diameter is 0.05-1 mm, the substrate temperature is 20-200 ℃ and the single powder spreading thickness of the substrate is 0.1-0.4 mm, and finally stopping heating, and taking the formed composite material off the substrate after the substrate is cooled;
fourthly, cold isostatic pressing technology:
placing the formed composite material into a jacket, vacuumizing until the pressure is less than 10Pa, placing the jacketed composite material into a cold isostatic press, keeping the pressure for 2-20 min under the condition that the hydrostatic pressure is 50-400 MPa, and removing the jacket to obtain a densified composite material;
fifthly, sintering:
placing the densified composite material in a vacuum furnace, vacuumizing until the pressure is less than 1Pa, and preserving the heat for 0.5-3 h under the condition that the sintering temperature is 850-1100 ℃ to obtain the sintered composite material;
or placing the densified composite material in an atmosphere furnace, and preserving the heat for 0.5-4 h under the conditions of protecting the atmosphere and sintering the composite material at the temperature of 850-1100 ℃ to obtain the sintered composite material;
sixthly, hot isostatic pressing technology:
and under the conditions that the hot isostatic pressing temperature is 850-1050 ℃ and the hot isostatic pressing pressure is 50-200 MPa, keeping the temperature and the pressure of the sintered composite material for 0.5-4 h to obtain the diamond copper-based composite material.
2. The method for preparing the diamond copper-based composite material according to the additive manufacturing process of claim 1, wherein the carbide coating layer in the step one is titanium carbide, tungsten carbide, zirconium carbide, boron carbide, chromium carbide or molybdenum carbide; the metal simple substance plating layer in the step one is Ti, W, Zr, Cr, Mo, V or Nb.
3. The method for preparing the diamond copper-based composite material according to the additive manufacturing process of claim 1, wherein the plating process in the step one is physical vapor deposition, chemical vapor deposition, electroless plating, electroplating or salt bath plating.
4. The method for preparing the diamond copper-based composite material according to the additive manufacturing process of claim 1, wherein the diamond powder in the first step is single crystal diamond powder; the substrate in the third step is a pure copper plate.
5. The method for preparing the diamond copper-based composite material according to the additive manufacturing process of claim 1, wherein the mechanical mixing in the second step is mixing for 30-60 min by a planetary ball mill; the laser forming in the third step is specifically carried out according to the following steps: the first layer scans for two periods, then each layer scans for one period, the scanning directions of the layers are in an orthogonal relation, and the overlapping rate of the scanning intervals is 0-50%; and fifthly, the protective atmosphere is inert gas or reducing gas, and the reducing gas is hydrogen or methane.
6. A method for preparing a diamond copper-based composite material by an additive manufacturing process is characterized by comprising the following steps of:
firstly, preparing the plated diamond powder:
plating a composite plating layer on the surface of the diamond powder by a plating process to obtain plated diamond powder;
the composite coating consists of an outer coating and an inner coating; the outer plating layer is a pure copper plating layer; the inner plating layer is a carbide plating layer or a metal simple substance plating layer;
the thickness of the carbide coating layer is 100 nm-500 nm, and the thickness of the metal simple substance coating layer is 100 nm-1 mu m;
the mass percentage content of the pure copper plating layer in the diamond powder after plating is 20-70%;
the particle size of the diamond powder is 20-400 μm;
secondly, mixing:
mechanically and uniformly mixing the plated diamond powder and pure copper powder to obtain mixed powder;
the pure copper powder is a mixture of pure copper powder with the particle size of 23-53 mu m and pure copper powder with the particle size of 2-6 mu m;
the volume ratio of the diamond powder after plating to the pure copper powder with the particle size of 23-53 mu m is 1 (0.1-3); the volume ratio of the diamond powder after plating to the pure copper powder with the grain diameter of 2-6 mu m is 1 (0.1-3);
thirdly, selective laser melting:
in selective laser melting equipment, controlling the oxygen content to be lower than 0.1%, preheating a substrate to 20-200 ℃, carrying out laser forming by using mixed powder under the conditions that the laser power is 30-500W, the scanning speed is 1-1500 mm/s, the spot diameter is 0.05-1 mm, the substrate temperature is 20-200 ℃ and the single powder spreading thickness of the substrate is 0.1-0.4 mm, and finally stopping heating, and taking the formed composite material off the substrate after the substrate is cooled;
fourthly, sintering:
placing the molded composite material in a vacuum furnace, vacuumizing until the pressure is less than 1Pa, and preserving heat for 0.5-3 h under the condition that the sintering temperature is 850-1100 ℃ to obtain the sintered composite material;
or placing the formed composite material in an atmosphere furnace, and preserving heat for 0.5-4 h under the conditions of protecting atmosphere and sintering temperature of 850-1100 ℃ to obtain the sintered composite material;
fifthly, hot isostatic pressing technology:
and under the conditions that the hot isostatic pressing temperature is 850-1050 ℃ and the hot isostatic pressing pressure is 50-200 MPa, keeping the temperature and the pressure of the sintered composite material for 0.5-4 h to obtain the diamond copper-based composite material.
7. The method for preparing the diamond copper-based composite material according to the additive manufacturing process of claim 6, wherein the carbide coating layer in the step one is titanium carbide, tungsten carbide, zirconium carbide, boron carbide, chromium carbide or molybdenum carbide; the metal simple substance plating layer in the step one is Ti, W, Zr, Cr, Mo, V or Nb.
8. The method for preparing the diamond copper-based composite material according to the additive manufacturing process of claim 6, wherein the plating process in the step one is physical vapor deposition, chemical vapor deposition, electroless plating, electroplating or salt bath plating.
9. The method for preparing the diamond copper-based composite material according to the additive manufacturing process of claim 6, wherein the diamond powder in the first step is single crystal diamond powder; the substrate in the third step is a pure copper plate.
10. The method for preparing the diamond copper-based composite material according to the additive manufacturing process of claim 6, wherein the mechanical mixing in the second step is mixing for 30-60 min by a planetary ball mill; the laser forming in the third step is specifically carried out according to the following steps: the first layer scans for two periods, then each layer scans for one period, the scanning directions of the layers are in an orthogonal relation, and the overlapping rate of the scanning intervals is 0-50%; the protective atmosphere in the fourth step is inert gas or reducing gas, and the reducing gas is hydrogen or methane.
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