CN115094411A - Gradient diamond/metal composite material and preparation method thereof - Google Patents
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- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
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- B22F1/14—Treatment of metallic powder
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- 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
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- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
- C23C24/103—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
- C23C24/106—Coating with metal alloys or metal elements only
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- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
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- H—ELECTRICITY
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
- H01L23/3735—Laminates or multilayers, e.g. direct bond copper ceramic substrates
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Abstract
The invention discloses a gradient diamond metal composite material and a preparation method thereof. The gradient diamond/metal composite material comprises an upper metal surface layer, a lower metal surface layer, a diamond metal subsurface layer, a diamond metal core layer and a diamond metal subsurface layer, wherein the diamond metal subsurface layer, the diamond metal core layer and the diamond metal subsurface layer are sequentially arranged between the upper metal surface layer and the lower metal surface layer, and the particle size (D50) of diamond particles in the diamond metal subsurface layer is controlled to be 30-50 mu m; the diamond metal core layer contains coarse diamond particles and fine diamond particles, the particle size (D50) of the coarse diamond particles is controlled to be 100-300 mu m, and the particle size (D50) of the fine diamond particles in the core layer is controlled to be 30-50 mu m. The preparation method comprises the following steps: (1) preparing raw materials of a surface layer, a subsurface layer and a core layer, and respectively filling the raw materials into three independent nozzles of laser cladding equipment. (2) And covering the alloy substrate with a metal foil, and pressing by using a blank holder. (3) And carrying out laser cladding on the surface of the metal foil in a vacuum environment to form each layer in sequence. (4) And (5) after cladding is finished, machining.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a gradient diamond/metal composite material easy to machine and weld and a preparation method thereof.
Background
With the development of semiconductor technology, chip heat dissipation has become a bottleneck problem recognized in the industry. Diamond is the material with the highest thermal conductivity known in nature, and currently, diamond and diamond/metal composite materials are widely applied to manufacturing chip heat sinks. As a chip heat sink material, the material is required to have the characteristics of high heat conductivity and adaptive expansion coefficient with a chip material. The higher the thermal conductivity is, the more beneficial the heat dissipation of the chip is, and the content of the diamond in the composite material is in direct proportion to the thermal conductivity. The better the adaptability of the thermal expansion coefficient and the chip material is, the more beneficial the stress control is, and the content of diamond in the composite material is in inverse proportion to the thermal expansion coefficient. In order to obtain higher thermal conductivity and lower thermal expansion coefficient, the content of diamond in the composite material is continuously increased. The diamond is used as a heat conduction reinforcement to form a composite material with metal, and the rule generally exists that the larger the volume fraction of the diamond, the larger the heat conductivity of the composite material is, the smaller the expansion coefficient is, and vice versa. When the copper/diamond composite material is used as a heat sink, diamond with smaller grain size is needed because the surface with extremely low roughness (Sa < 1 μm) needs to be obtained. In addition, the metal heat sink material is also required to have good solderability because it needs to be connected to a chip or other component. The present solution to solderability is achieved primarily by apparent metallization of the material. And the higher the content of diamond, the poorer the metallization capability of the composite material, and the greater the welding difficulty. It can be seen that there is a significant contradiction between the current application requirements of copper/diamond composites, namely, the contradiction between thermal conductivity, coefficient of expansion, and surface processability, weldability.
As shown in fig. 2, the general processing paths for the copper/diamond composite heat sink are: infiltration or powder metallurgy produces a billet (a) → laser machining profile (b) → grinding surface (c) → surface metallization (d). It can be seen that the thermal conductivity, expansion coefficient and workability of the material have solidified at the blank preparation stage.
As described above, it is urgently needed to break through the limitations of the original blank preparation method, solve the problems of insufficient surface precision processability and large welding difficulty on the premise of keeping the characteristics of high thermal conductivity and low expansion of the original material, and pave the way for industrial batch application of diamond/metal composite materials.
Disclosure of Invention
It is an object of the present invention to provide a gradient diamond/metal composite which is easy to machine and weld.
Another object of the present invention is to provide a method for preparing the gradient diamond/metal composite material.
In order to achieve the purpose, the invention adopts the following technical scheme:
the gradient diamond/metal composite material is characterized by comprising an upper metal surface layer, a lower metal surface layer, a diamond metal subsurface layer, a diamond metal core layer and a diamond metal subsurface layer, wherein the diamond metal subsurface layer, the diamond metal core layer and the diamond metal subsurface layer are sequentially arranged between the upper metal surface layer and the lower metal surface layer, and the particle size (D50) of diamond particles in the diamond metal subsurface layer is controlled to be 30-50 microns; the diamond metal core layer contains coarse diamond particles and fine diamond particles, the particle size (D50) of the coarse diamond particles is controlled to be 100-300 mu m, and the particle size (D50) of the fine diamond particles in the core layer is controlled to be 30-50 mu m.
Further, the metal is copper or aluminum.
Furthermore, the upper and lower metal surface layers can be designed to have different thicknesses according to actual effects, the original thickness of the metal on the surface layer connected with the chip is controlled to be 1-2 mm, and the original thickness of the metal on the surface layer connected with other heat dissipation structures is controlled to be 1-5 mm.
Further, the volume fraction of diamond in the diamond metal subsurface layer is controlled to be 50% -60%, and the thickness of each diamond metal subsurface layer is 0.2 mm-1 mm.
Further, the volume fraction of diamond in the diamond metal core layer is controlled to be 65% -70%, and the thickness of the diamond metal core layer is 0.2-2 mm. Preferably, the volume fraction ratio of the coarse-grain diamond to the fine-grain diamond in the diamond metal core layer is 2-4.
A preparation method of a gradient diamond/metal composite material comprises the following steps:
(1) selecting metal powder raw materials, and controlling the particle size (D50) of metal powder particles to be 50-150 mu m; mixing part of metal powder and subsurface layer with diamond according to the requirements to obtain subsurface layer raw material; mixing part of the metal powder with the diamond for the core layer according to the requirements to obtain a core layer raw material; respectively arranged in three independent nozzles of laser cladding equipment.
(2) Covering a metal foil with the chemical composition consistent with that of the metal powder on the alloy substrate, wherein the thickness of the foil is 0.05-0.5 mm, and pressing the foil tightly by using a blank holder.
(3) Performing laser cladding on the surface of the metal foil in a vacuum environment, sequentially cladding a metal surface layer, a diamond metal subsurface layer, a diamond metal core layer, a diamond metal subsurface layer and a metal surface layer, and adjusting the thickness of each layer by controlling the number of cladding layers. In the cladding process, the metal powder is melted and then is solidified and connected to form a continuous matrix, and the diamond is distributed in the subsurface layer and the core layer according to the preset shape without changing the shape.
(4) And after the cladding is finished, taking down the block material obtained by cladding together with the metal foil, and cutting the circumference by adopting laser to obtain the appearance profile. And grinding and polishing the outer surface of the metal foil serving as a reference surface for controlling the size in the thickness direction to obtain the composite material with the upper surface and the lower surface uniformly covered with the metal layer, so that welding and packaging can be performed without surface metallization.
The invention has the beneficial effects that:
the gradient diamond/metal composite material provided by the invention is provided with three functional layers, wherein the metal surface layer bears the precision processing and welding of the material packaging surface; the subsurface layer is used for preventing the large-particle diamond of the core part from flowing to the surface layer to influence the processing; the core layer has the functions of increasing the overall thermal conductivity of the material and reducing the expansion coefficient of the material as much as possible. The design concept ensures that the machinability and weldability of the material are greatly improved on the premise of not reducing the thermal conductivity and the expansion coefficient of the composite material, thereby greatly reducing the processing flow of the diamond metal composite material, simultaneously reducing the processing difficulty and the cost, improving the adaptability of the diamond metal composite material as a heat sink material, and further exploring the performance potential of the diamond/metal composite material.
In addition, the gradient diamond/metal composite material is prepared by utilizing the characteristic that the laser cladding forming technology can accurately control additive components and sizes, the preparation process is simple and convenient, and the raw materials and the processing cost are not greatly increased. The material prepared by the invention can be widely applied to chips of high-power electronic components and laser heat sinks.
Drawings
Fig. 1 is a schematic view of the gradient diamond/metal composite material of the present invention and its processing.
Fig. 2 is a schematic view of a conventional diamond/metal composite and a process for manufacturing the same.
Detailed Description
The present invention is further described in detail below with reference to the drawings and examples, but the scope of the present invention is not limited thereto.
As shown in fig. 1(b), the gradient diamond/metal composite material of the present invention comprises, in order from top to bottom, an upper metal surface layer 1, a diamond metal subsurface layer 2, a diamond metal core layer 3, a diamond metal subsurface layer 4, and a lower metal surface layer 5.
In the preparation process of the gradient diamond/metal composite material of the invention, the lower metal surface layer 5 is welded with the prefabricated metal foil. The metal is copper or aluminum, and the particle size (D50) of diamond particles in the metal subsurface layer of the diamond is controlled to be 30-50 mu m; the diamond metal core layer contains coarse diamond particles and fine diamond particles, the particle size (D50) of the coarse diamond particles is controlled to be 100-300 mu m, and the particle size (D50) of the fine diamond particles in the core layer is controlled to be 30-50 mu m. After cladding, as shown in fig. 1(a) to 1(b), the thickness and surface roughness of the upper and lower metal surface layers are regulated and controlled by grinding and polishing processes with the outer surface of the metal foil as a reference surface. In the gradient diamond/metal composite material, the upper metal surface layer and the lower metal surface layer can be welded with a chip material.
In the gradient diamond/metal composite material, the upper metal surface layer and the lower metal surface layer can be designed to have different thicknesses according to actual effects, the original thickness of the metal of the surface layer connected with a chip is controlled to be 1-2 mm, and the original thickness of the metal of the surface layer connected with other heat dissipation structures is controlled to be 1-5 mm. The volume fraction of the diamond of the subsurface layer is controlled to be 50-60%, and the thickness of the subsurface layer is 0.2-1 mm respectively. The volume fraction of the diamond of the core layer is controlled to be 65-70%, the thickness of the core layer is 0.2-2 mm, and the volume fraction ratio of the coarse-grain diamond to the fine-grain diamond is 2-4. After the thicknesses of the upper metal layer and the lower metal layer are regulated and controlled through a grinding process, the thickness of the obtained gradient diamond/metal composite material for packaging can be 0.5-3.1 mm.
As shown in fig. 2, diamond/metal composites prepared by conventional infiltration or powder metallurgy processes require at least 4 major steps to obtain a usable heat sink material.
The diamonds in the following examples are all common industrial diamonds. In the embodiment, the surface roughness is measured by adopting an optical 3D surface profile instrument, the thermal conductivity is measured according to the standard of measuring the thermal diffusion coefficient or the thermal conductivity coefficient by using a GB/T22588-.
Example 1
Copper powder having a particle size (D50) of 80 μm and diamond powder having a particle size (D50) of 30 μm and 100 μm were selected. Uniformly mixing 30 mu m diamond powder and copper powder according to the volume ratio of 1: 1 to form a subsurface raw material; diamond powder of 30 μm or 100 μm and copper powder are mixed according to volumeUniformly mixing the raw materials in a ratio of 2: 5: 3 to form a core layer raw material; copper powder was used as a surface layer material. And covering a copper foil with the thickness of 0.05mm on the substrate, and pressing by using a blank holder. Carrying out laser cladding in a vacuum environment. And controlling parameters such as powder feeding amount, laser power, scanning speed and the like, wherein the original thickness of the lower metal surface layer close to the copper foil is 2mm, the thicknesses of the two subsurface layers are 0.3mm respectively, the thickness of the core layer is 1mm, and the original thickness of the upper metal surface layer is 2 mm. The overall spread area was 40X 40 mm. After cutting the outer contour with a laser, a 30X 30mm sample with a thickness of 4.65mm was obtained. After grinding and polishing, the thicknesses of the upper metal surface layer and the lower metal surface layer are both reduced to 0.5mm, and the surface roughness can reach less than 1.5 mu m. The final heat sink piece was 2.6X 30mm and the upper and lower surfaces were uniformly covered with copper layers. The measured thermal conductivity and thermal expansion coefficient of the heat sink sheet are 583W/mK and 7.42 multiplied by 10 respectively -6 and/K. The sample was reliably connected to the gallium nitride chip by gold-tin eutectic soldering.
Comparative example 1
Uniformly mixing diamond powder with the particle size of 30 mu m or 100 mu m and copper powder according to the volume ratio of 2: 5: 3, and preparing the copper-diamond composite material by adopting a powder metallurgy method. The blank with the thickness of 2.8 multiplied by 30.2mm is processed by laser, and then is ground to 2.6 multiplied by 30mm by fine grinding by a diamond grinding wheel, the surface roughness can only reach 5 mu m, and the further reduction can not be realized. The measured thermal conductivity and thermal expansion coefficient of the heat sink sheet are 550W/mK and 7.59 multiplied by 10 respectively -6 and/K. And sputtering the surface of the ground sample to obtain a metallic nickel coating, and then obtaining a surface gold coating through a chemical plating process. The sample was reliably connected to the gallium nitride chip by gold-tin eutectic soldering.
Example 2
Aluminum powder with the particle size (D50) of 100 mu m and diamond powder with the particle size (D50) of 40 mu m and 200 mu m are selected. Uniformly mixing diamond powder with the particle size of 40 mu m and aluminum powder according to the volume ratio of 55: 45 to form a subsurface raw material; uniformly mixing diamond powder of 40 mu m and 200 mu m with aluminum powder according to the volume ratio of 15: 55: 30 to form a core layer raw material; aluminum powder was used as a surface layer material. And covering the aluminum foil with the thickness of 0.1mm on the substrate, and pressing the aluminum foil with a blank holder. Carrying out laser cladding in a vacuum environment. Controlling the parameters of powder feeding quantity, laser power and scanning speed,the original thickness of the lower metal surface layer of the obtained aluminum foil is 1mm, the thicknesses of the two subsurface layers are 0.5mm respectively, the thickness of the core layer is 1.2mm, and the original thickness of the upper metal surface layer is 2.5 mm. The overall spreading area was 50X 40 mm. After cutting the outer contour with a laser, a 40X 30mm sample with a thickness of 5.8mm was obtained. After grinding and polishing, the thicknesses of the upper metal surface layer and the lower metal surface layer are both reduced to 0.6 mm. The final heat sink sheet was 3.4X 40X 30mm, and the upper and lower surfaces were uniformly covered with aluminum layers. The measured thermal conductivity and thermal expansion coefficient of the heat sink sheet are 564W/mK and 7.88 multiplied by 10 respectively -6 and/K is used. And forming reliable connection with the gallium nitride chip through gold-tin eutectic welding.
Comparative example 2
Uniformly mixing diamond powder of 40 mu m and 200 mu m with aluminum powder according to the volume ratio of 15: 55: 30, and preparing the aluminum diamond composite material by adopting a powder metallurgy method. The blank with the thickness of 3.6 multiplied by 40.2 multiplied by 30.2mm is processed by laser, and then is ground to 3.4 multiplied by 40 multiplied by 30mm by fine grinding by a diamond grinding wheel, the surface roughness can only reach 8 mu m, and the further reduction can not be realized. The measured thermal conductivity and thermal expansion coefficient of the heat sink sheet are 575W/mK and 7.62 multiplied by 10 respectively -6 and/K. And (3) carrying out surface sputtering on the ground sample to obtain a metal nickel coating, and then carrying out a chemical plating process to obtain a surface gold coating. The sample was reliably connected to the gallium nitride chip by gold-tin eutectic soldering.
Example 3
Aluminum powder with the particle size (D50) of 150 mu m and diamond powder with the particle size (D50) of 50 mu m and 300 mu m are selected. Uniformly mixing 50 mu m diamond powder and aluminum powder according to the volume ratio of 6: 4 to form a subsurface raw material; uniformly mixing 50-micron and 300-micron diamond powder and aluminum powder according to the volume ratio of 15: 50: 35 to form a core layer raw material; aluminum powder was used as a surface layer material. And covering the aluminum foil with the thickness of 0.2mm on the substrate, and pressing the aluminum foil with a blank holder. Carrying out laser cladding in a vacuum environment. And controlling parameters such as powder feeding amount, laser power, scanning speed and the like, wherein the original thickness of the lower metal surface layer close to the aluminum foil is 1.5mm, the thicknesses of the two subsurface layers are respectively 0.8mm, the thickness of the core layer is 2mm, and the original thickness of the upper metal surface layer is 3 mm. The overall spreading area was 60X 50 mm. After cutting the outer contour with a laser, a 50X 40mm sample with a thickness of 8.3mm was obtained. After grinding and polishing, onThe thickness of the lower metal surface layer is reduced to 0.3 mm. The final heat sink sheet was 4.2X 50X 40mm, and the upper and lower surfaces were uniformly covered with aluminum layers. The measured thermal conductivity and thermal expansion coefficient of the heat sink sheet are 591W/mK and 7.15 multiplied by 10 respectively -6 and/K. And forming reliable connection with the gallium nitride chip through gold-tin eutectic welding.
Comparative example 3
Uniformly mixing 50-micron and 300-micron diamond powder and aluminum powder according to the volume ratio of 15: 50: 35, and preparing the aluminum diamond composite material by adopting an infiltration method. The blank with the thickness of 4.4 multiplied by 50.2 multiplied by 30.2mm is processed by laser, and then is ground to 4.2 multiplied by 50 multiplied by 40mm by fine grinding by a diamond grinding wheel, the surface roughness can only reach 12 mu m, and the further reduction can not be realized. The measured thermal conductivity and thermal expansion coefficient of the heat sink sheet are 603W/mK and 7.02 multiplied by 10 respectively -6 and/K. And sputtering the surface of the ground sample to obtain a metallic nickel coating, and then obtaining a surface gold coating through a chemical plating process. The sample was reliably connected to the gallium nitride chip by gold-tin eutectic soldering.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention thereto. It should be noted that those skilled in the art, on the basis of the teachings provided herein, may make other modifications equivalent to those already described, and should be considered within the scope of the present invention.
Claims (7)
1. The gradient diamond/metal composite material is characterized by comprising an upper metal surface layer, a lower metal surface layer, a diamond metal subsurface layer, a diamond metal core layer and a diamond metal subsurface layer, wherein the diamond metal subsurface layer, the diamond metal core layer and the diamond metal subsurface layer are sequentially arranged between the upper metal surface layer and the lower metal surface layer, and the particle size (D50) of diamond particles in the diamond metal subsurface layer is controlled to be 30-50 microns; the diamond metal core layer contains coarse diamond particles and fine diamond particles, the particle size (D50) of the coarse diamond particles is controlled to be 100-300 mu m, and the particle size (D50) of the fine diamond particles in the core layer is controlled to be 30-50 mu m.
2. The gradient diamond/metal composite of claim 1, wherein the metal is copper or aluminum.
3. The gradient diamond/metal composite material according to claim 1 or 2, wherein the original thickness of the metal of the surface layer connected to the chip is controlled to be 1 to 2mm, and the original thickness of the metal of the surface layer connected to other heat dissipation structures is controlled to be 1 to 5 mm.
4. A gradient diamond/metal composite according to claim 1 or 2, wherein the diamond volume fraction in the diamond metal sub-surface layer is controlled to be 50% to 60%, and the thickness of each diamond metal sub-surface layer is 0.2mm to 1 mm.
5. A gradient diamond/metal composite according to claim 1 or 2, wherein the diamond volume fraction in the diamond metal core layer is controlled to 65-70%, and the thickness of the diamond metal core layer is 0.2-2 mm.
6. The gradient diamond/metal composite of claim 5, wherein the ratio of the volume fractions of the coarse diamond grains and the fine diamond grains in the diamond metal core layer is 2 to 4.
7. A method of producing a gradient diamond/metal composite according to any one of claims 1 to 6, comprising the steps of:
(1) selecting metal powder raw materials, and controlling the particle size (D50) of metal powder particles to be 50-150 mu m; mixing part of metal powder and subsurface layer with diamond according to the requirements to obtain subsurface layer raw material; mixing part of the metal powder with the diamond for the core layer according to the requirements to obtain a core layer raw material; respectively loading into three independent nozzles of laser cladding equipment;
(2) covering a metal foil with the chemical composition consistent with that of the metal powder on the alloy substrate, wherein the thickness of the foil is 0.05-0.5 mm, and pressing the foil tightly by using a blank holder;
(3) performing laser cladding on the surface of the metal foil in a vacuum environment, sequentially cladding a metal surface layer, a diamond metal subsurface layer, a diamond metal core layer, a diamond metal subsurface layer and a metal surface layer, and adjusting the thickness of each layer by controlling the number of cladding layers;
(4) after cladding, taking down the block material obtained by cladding together with the metal foil, and cutting the circumference by adopting laser to obtain the outline; and grinding and polishing the outer surface of the metal foil serving as a reference surface for controlling the size in the thickness direction to obtain the composite material with the upper surface and the lower surface uniformly covered with the metal layer, so that welding and packaging can be performed without surface metallization.
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CN105755308A (en) * | 2016-04-13 | 2016-07-13 | 东莞市联洲知识产权运营管理有限公司 | Novel high-thermal-conductivity diamond/aluminum composite material and preparation method thereof |
CN107900327A (en) * | 2017-11-16 | 2018-04-13 | 北京科技大学 | A kind of method that combination 3D printing technique prepares diamond/copper composite material |
CN112222381A (en) * | 2020-09-29 | 2021-01-15 | 成都本征新材料技术有限公司 | Composite heat sink material with gradient distribution of thermal expansion coefficients and preparation method thereof |
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