CN110394521B - Diamond film high-efficiency heat dissipation material and preparation method thereof - Google Patents
Diamond film high-efficiency heat dissipation material and preparation method thereof Download PDFInfo
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- CN110394521B CN110394521B CN201910711380.2A CN201910711380A CN110394521B CN 110394521 B CN110394521 B CN 110394521B CN 201910711380 A CN201910711380 A CN 201910711380A CN 110394521 B CN110394521 B CN 110394521B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/008—Soldering within a furnace
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/19—Soldering, e.g. brazing, or unsoldering taking account of the properties of the materials to be soldered
-
- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/01—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes on temporary substrates, e.g. substrates subsequently removed by etching
-
- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
Abstract
The invention relates to a diamond film high-efficiency heat dissipation material and a preparation method thereof, the heat dissipation material sequentially comprises an upper layer, a middle layer and a lower layer from top to bottom, the upper layer is a diamond self-supporting film with the thickness of 20-500 mu m, the middle layer is a welding seam area containing diamond powder, and the lower layer is a diamond/copper composite material. The preparation method of the heat dissipation material comprises the following steps: and welding the growth surface of the diamond self-supporting film and the diamond/copper composite material by using Ag, Cu, Ti and diamond mixed powder as an active welding flux and adopting vacuum welding to obtain the diamond efficient heat dissipation material. The heat dissipation material of the invention does not have a thermal resistance layer because the welding seam area contains diamond powder, and meanwhile, the substrate adopts the diamond/copper composite material, so that the heat dissipation material has excellent overall heat dissipation performance and the heat conductivity is higher than 600W/(m.K). In addition, the diamond self-supporting film required by the method is thin in thickness and low in cost; the operation is simple, and large-scale batch production can be realized.
Description
Technical Field
The invention relates to the technical field of thermal management materials and preparation thereof, in particular to a diamond film efficient heat dissipation material and a preparation method thereof.
Background
Modern electronic technology is rapidly developed, electronic components have higher integration level and faster running speed, the heat productivity of the components is rapidly increased, and higher requirements are provided for the heat dissipation capability of electronic packaging materials. The ceramic materials (AlN, Al) used at present2O3SiC) and metal matrix composite materials (Cu-W, Cu-Mo, Al-SiC) are increasingly unable to meet the requirements of rapid and efficient heat dissipation. Therefore, future electronic packaging materials must be upgraded to realize the function of quickly removing heat.
Diamond is the substance with the highest thermal conductivity in nature, the thermal conductivity at room temperature can reach 2000W/(m.K), which is about 5 times that of copper, and the thermal expansion coefficient is very low, so that the diamond is one of the most ideal electronic packaging materials. At present, in order to realize the application of diamond in the field of electronic packaging materials, a mode of preparing a diamond/Cu composite material or preparing a composite sheet by welding a diamond thick film with the thickness of more than 300 mu m on a Cu substrate is mainly adopted. For the diamond/Cu composite material, the thermal conductivity can reach 440-500W/(m.K), and is still far away from the thermal conductivity of diamond. In addition, the workability is poor, and the requirements of the electronic packaging material on the surface finish and the size are strict, so that the application is difficult. For diamond thick film/Cu solder compacts, the following problems exist: 1) the diamond has large thickness and high preparation cost, the high hardness of the diamond makes the polishing difficult, the polishing process is complex, and the cost is further increased; 2) the welding of diamond and copper is difficult, the welding is generally carried out by adopting Ag-Cu-Ti active welding flux, Ti is added as active metal to form TiC and increase the wettability of the diamond, however, the thermal conductivity of Ti and TiC is very low, and a thermal resistance layer is formed in a welding seam; 3) diamond thermal conductivity is high, while Cu thermal conductivity is only 400W/(m · K), which makes the thermal conductivity of the composite pad as a whole still relatively low.
The invention patent CN201810580016.2 discloses a preparation method of a diamond film-copper composite radiating fin, which realizes the welding of diamond with the thickness of 50-100 μm and copper, and reduces the thickness and the cost of a diamond film, but the problems of low heat conductivity of a welding seam thermal resistance layer and a Cu substrate still exist.
In order to solve the problems that the heat dissipation performance of the existing material cannot meet the heat dissipation requirement of future electronic packaging materials, the diamond/Cu composite material is high in processing difficulty, the difference between the heat dissipation performance and diamond is large, the diamond film-copper heat dissipation material prepared by a welding method has high requirement on the thickness of diamond, a solder layer can form a thermal resistance layer, a pure copper substrate is poor in heat dissipation performance and the like, and the research and development of a novel low-cost diamond-Cu composite heat dissipation material with good heat dissipation performance are urgently needed.
Disclosure of Invention
The invention aims to make up for the defects of the prior art, solve the problem that the heat dissipation performance of the existing material cannot meet the heat dissipation requirement of the future electronic packaging material, and realize the utilization of the diamond which is a heat dissipation material with excellent performance, and provides a diamond film high-efficiency heat dissipation material and a preparation method thereof.
The invention is realized by the following technical scheme:
a diamond film high-efficiency heat dissipation material comprises an upper layer, a middle layer and a lower layer from top to bottom in sequence; wherein the upper layer is a diamond self-supporting film with the thickness of 20-500 mu m and is used as a heat source contact layer; the middle layer is a welding seam area containing diamond powder and used as a heat conduction layer; the lower layer is made of diamond/copper composite material and is used as a heat conduction layer.
As a preferred technical scheme, the diamond self-supporting film is prepared by adopting a CVD method.
Further, the invention also provides a preparation method of the diamond film high-efficiency heat dissipation material, which comprises the following steps:
1) mixing Ag powder, Cu powder, Ti powder and diamond powder in a certain ratio to obtain active flux, using borax as scaling powder, preparing the active flux into paste flux, and brushing the paste flux on the surface of the diamond/copper composite material;
2) and (2) placing the growth surface of the diamond self-supporting film downwards on the surface of the diamond/copper composite material, applying downward pressure on the diamond self-supporting film, and heating the diamond self-supporting film and the diamond/copper composite material to a high temperature by using a vacuum furnace for welding to obtain the high-efficiency diamond film heat dissipation material.
As a preferred technical scheme, when the active welding flux is manufactured, Ag powder, Cu powder and Ti powder are uniformly mixed to prepare Ag, Cu and Ti mixed powder, wherein the mass of the Ag powder accounts for 55-70% of the total mass of the mixed powder, and the mass of the Cu powder accounts for 20-30% of the total mass of the mixed powder; the mass of the Ti powder accounts for 10-15% of the total mass of the mixed powder; then uniformly mixing the diamond powder with the mixed powder of Ag, Cu and Ti to prepare the mixed powder of Ag, Cu, Ti and diamond powder, wherein the mass of the diamond powder accounts for 10-30% of the total mass of the mixed powder of Ag, Cu, Ti and diamond powder.
As a preferred technical scheme, the granularity of the diamond powder is 0.1-100 μm.
As a preferred technical scheme, the pressure applied to the diamond self-supporting film is 0.1-10 MPa.
As a preferable technical scheme, when welding is carried out in a vacuum furnace, the heat preservation temperature is 700-950 ℃, and the heat preservation time is 5-30 min.
The invention has the following beneficial effects:
1) the novel diamond film efficient heat dissipation material is composed of a diamond self-supporting film layer, a diamond powder-containing welding seam area layer and a diamond/Cu composite material substrate layer, wherein the three layers of materials contain diamonds with extremely high heat conductivity and low thermal expansion coefficient, so that the heat dissipation capacity of the whole heat dissipation material can be greatly improved, and the heat conductivity of the heat dissipation material can reach more than 600W/(m.K); the diamond self-supporting film is used as a heat source contact layer and can effectively conduct heat generated by a heat source, and the heat conduction layer formed by the welding seam layer and the diamond/Cu composite material layer can conduct heat more efficiently without generating larger deformation due to the addition of the diamond; the weld layer containing diamond powder can effectively improve the condition of forming thermal resistance of the conventional weld layer.
2) The invention can meet the requirement by adopting a CVD method to prepare a thinner diamond self-supporting film, can adopt monocrystalline silicon or other materials with higher surface smoothness as a diamond growth substrate, does not need polishing treatment on the diamond after removing the substrate, or can meet the requirement of smoothness only by simple polishing treatment, thereby greatly reducing the preparation and polishing cost of the diamond.
3) The method is simple to operate, the novel diamond film-copper efficient heat dissipation material meeting the requirements can be formed only by heating and welding the diamond film and the diamond/Cu composite material under the vacuum condition and external pressure condition, and large-scale batch production is easy to realize.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate exemplary embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention.
FIG. 1 is a schematic structural diagram of a diamond film high-efficiency heat-dissipating material according to the present invention.
FIG. 2 is a schematic view of the preparation of the diamond film high-efficiency heat-dissipating material of the present invention.
In the figure: 1-diamond self-supporting film, 2-welding seam area, 3-diamond/copper composite material, 4-pasty welding flux and 5-weight.
Detailed Description
In order that those skilled in the art will better understand the present invention, a more complete and complete description of the present invention is provided below in conjunction with the accompanying drawings and embodiments. It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
The invention provides a diamond film high-efficiency heat dissipation material, which has a structural structure shown in figure 1 and sequentially comprises an upper layer, a middle layer and a lower layer from top to bottom; wherein, the upper layer is a diamond self-supporting film 1 with the thickness of 20-500 μm prepared by a CVD method and is used as a heat source contact layer; the middle layer is a welding seam area 2 containing diamond powder and used as a heat conduction layer; the lower layer is a diamond/copper composite material 3 as a heat conductive layer.
The invention also provides a preparation method of the diamond film high-efficiency heat dissipation material, which comprises the following steps of:
1) mixing Ag powder, Cu powder, Ti powder and diamond powder in a certain ratio to obtain active flux, using borax as scaling powder, preparing the active flux into paste flux, and brushing the paste flux on the surface of the diamond/copper composite material 3, namely the paste flux indicated by reference numeral 4 in figure 2; when the active welding flux is manufactured, Ag powder, Cu powder and Ti powder are uniformly mixed to prepare Ag, Cu and Ti mixed powder, wherein the mass of the Ag powder accounts for 55-70% of the total mass of the mixed powder, and the mass of the Cu powder accounts for 20-30% of the total mass of the mixed powder; the mass of the Ti powder accounts for 10-15% of the total mass of the mixed powder; then uniformly mixing diamond powder with the mixed powder of Ag, Cu and Ti to prepare the mixed powder of Ag, Cu, Ti and diamond powder, wherein the mass of the diamond powder accounts for 10-30% of the total mass of the mixed powder of Ag, Cu, Ti and diamond powder, and the granularity of the diamond powder is 0.1-100 mu m;
2) placing the growth surface of the diamond self-supporting film 1 downwards on the surface of the diamond/copper composite material 3 coated with the pasty welding flux 4, applying downward pressure on the diamond self-supporting film 1, wherein the applied pressure is 0.1-10Mpa, and particularly, placing a heavy object 5 on the diamond self-supporting film 1; then, heating the diamond self-supporting film 1 and the diamond/copper composite material 3 to a high temperature by adopting a vacuum furnace for welding, wherein the heat preservation temperature is 700-; finally, the diamond film high-efficiency heat dissipation material is obtained.
The heat dissipation material of the present invention is further described below with reference to several specific examples of the product and its preparation:
example 1
A diamond film high-efficiency heat dissipation material comprises an upper layer, a middle layer and a lower layer from top to bottom in sequence; wherein, the upper layer is a diamond self-supporting film 1 with the thickness of 20 μm prepared by a CVD method and is used as a heat source contact layer; the middle layer is a welding seam area 2 containing diamond powder and used as a heat conduction layer; the lower layer is a diamond/copper composite material 3 as a heat conductive layer.
The preparation method of the diamond film high-efficiency heat dissipation material specifically comprises the following steps:
1) mixing Ag powder, Cu powder, Ti powder and diamond powder in a certain ratio to obtain active flux, using borax as scaling powder, preparing the active flux into paste flux 4, and brushing the paste flux on the surface of the diamond/copper composite material 3; when the active welding flux is manufactured, Ag powder, Cu powder and Ti powder are uniformly mixed to prepare Ag, Cu and Ti mixed powder, wherein the mass of the Ag powder accounts for 55% of the total mass of the mixed powder, and the mass of the Cu powder accounts for 30% of the total mass of the mixed powder; the mass of the Ti powder accounts for 15 percent of the total mass of the mixed powder; then uniformly mixing diamond powder with the mixed powder of Ag, Cu and Ti to prepare the mixed powder of Ag, Cu, Ti and diamond powder, wherein the mass of the diamond powder accounts for 20 percent of the total mass of the mixed powder of Ag, Cu, Ti and diamond powder, and the granularity of the diamond powder is 0.1 mu m;
2) placing the growth surface of the diamond self-supporting film 1 downwards on the surface of the diamond/copper composite material 3, and placing a heavy object 5 on the diamond self-supporting film 1 to apply downward pressure to the diamond self-supporting film, wherein the applied pressure is 5 Mpa; then, heating the diamond self-supporting film 1 and the diamond/copper composite material 3 to a high temperature by using a vacuum furnace for welding, wherein the heat preservation temperature is 800 ℃, and the heat preservation time is 5 min; finally, the diamond film high-efficiency heat dissipation material is obtained.
Example 2
A diamond film high-efficiency heat dissipation material comprises an upper layer, a middle layer and a lower layer from top to bottom in sequence; wherein, the upper layer is a diamond self-supporting film 1 with the thickness of 230 mu m prepared by a CVD method and is used as a heat source contact layer; the middle layer is a welding seam area 2 containing diamond powder and used as a heat conduction layer; the lower layer is a diamond/copper composite material 3 as a heat conductive layer.
The preparation method of the diamond film high-efficiency heat dissipation material specifically comprises the following steps:
1) mixing Ag powder, Cu powder, Ti powder and diamond powder in a certain ratio to obtain active flux, using borax as scaling powder, preparing the active flux into paste flux 4, and brushing the paste flux on the surface of the diamond/copper composite material 3; when the active welding flux is manufactured, uniformly mixing Ag powder, Cu powder and Ti powder to prepare Ag, Cu and Ti mixed powder, wherein the mass of the Ag powder accounts for 70% of the total mass of the mixed powder, and the mass of the Cu powder accounts for 20% of the total mass of the mixed powder; the mass of the Ti powder accounts for 10 percent of the total mass of the mixed powder; then uniformly mixing diamond powder with the mixed powder of Ag, Cu and Ti to prepare the mixed powder of Ag, Cu, Ti and diamond powder, wherein the mass of the diamond powder accounts for 10 percent of the total mass of the mixed powder of Ag, Cu, Ti and diamond powder, and the granularity of the diamond powder is 55 microns;
2) placing the growth surface of the diamond self-supporting film 1 downwards on the surface of the diamond/copper composite material 3, and placing a heavy object 5 on the diamond self-supporting film 1 to apply downward pressure to the diamond self-supporting film 1, wherein the applied pressure is 10 Mpa; then, heating the diamond self-supporting film 1 and the diamond/copper composite material 3 to a high temperature by using a vacuum furnace for welding, wherein the heat preservation temperature is 950 ℃, and the heat preservation time is 15 min; finally, the diamond film high-efficiency heat dissipation material is obtained.
Example 3
A diamond film high-efficiency heat dissipation material comprises an upper layer, a middle layer and a lower layer from top to bottom in sequence; wherein, the upper layer is a diamond self-supporting film 1 with the thickness of 500 mu m prepared by a CVD method and is used as a heat source contact layer; the middle layer is a welding seam area 2 containing diamond powder and used as a heat conduction layer; the lower layer is a diamond/copper composite material 3 as a heat conductive layer.
The preparation method of the diamond film high-efficiency heat dissipation material specifically comprises the following steps:
1) mixing Ag powder, Cu powder, Ti powder and diamond powder in a certain ratio to obtain active flux, using borax as scaling powder, preparing the active flux into paste flux 4, and brushing the paste flux on the surface of the diamond/copper composite material 3; when the active welding flux is manufactured, Ag powder, Cu powder and Ti powder are uniformly mixed to prepare Ag, Cu and Ti mixed powder, wherein the mass of the Ag powder accounts for 60% of the total mass of the mixed powder, and the mass of the Cu powder accounts for 25% of the total mass of the mixed powder; the mass of the Ti powder accounts for 15 percent of the total mass of the mixed powder; then uniformly mixing diamond powder with the mixed powder of Ag, Cu and Ti to prepare the mixed powder of Ag, Cu, Ti and diamond powder, wherein the mass of the diamond powder accounts for 30 percent of the total mass of the mixed powder of Ag, Cu, Ti and diamond powder, and the granularity of the diamond powder is 100 mu m;
2) placing the growth surface of the diamond self-supporting film 1 downwards on the surface of the diamond/copper composite material 3, and placing a heavy object 5 on the diamond self-supporting film 1 to apply downward pressure to the diamond self-supporting film 1, wherein the applied pressure is 0.1 Mpa; then, heating the diamond self-supporting film 1 and the diamond/copper composite material 3 to a high temperature by using a vacuum furnace for welding, wherein the heat preservation temperature is 700 ℃, and the heat preservation time is 30 min; finally, the diamond film high-efficiency heat dissipation material is obtained.
The technical solutions in the embodiments of the present invention are clearly and completely described above, and the described embodiments are only a part of the embodiments of the present invention, but 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.
Claims (2)
1. The diamond film high-efficiency heat dissipation material is characterized by sequentially comprising an upper layer, a middle layer and a lower layer from top to bottom, wherein the upper layer is a diamond self-supporting film with the thickness of 20-500 mu m, the middle layer is a welding seam area containing diamond powder, and the lower layer is a diamond/copper composite material;
the preparation method of the diamond film high-efficiency heat dissipation material comprises the following steps: 1) mixing Ag powder, Cu powder, Ti powder and diamond powder in a certain ratio to obtain active flux, using borax as scaling powder, preparing the active flux into paste flux, and brushing the paste flux on the surface of the diamond/copper composite material; 2) placing the growth surface of the diamond self-supporting film downwards on the surface of the diamond/copper composite material, applying downward pressure on the diamond self-supporting film, wherein the applied pressure is 0.1-10Mpa, then heating the diamond self-supporting film and the diamond/copper composite material to high temperature by adopting a vacuum furnace for welding, and the heat preservation temperature is 700-950 ℃, and the heat preservation time is 5-30min, thus obtaining the high-efficiency heat dissipation material of the diamond film;
when the active welding flux is manufactured, Ag powder, Cu powder and Ti powder are uniformly mixed to prepare Ag, Cu and Ti mixed powder, wherein the mass of the Ag powder accounts for 55-70% of the total mass of the mixed powder, and the mass of the Cu powder accounts for 20-30% of the total mass of the mixed powder; the mass of the Ti powder accounts for 10-15% of the total mass of the mixed powder; then uniformly mixing the diamond powder with the mixed powder of Ag, Cu and Ti to prepare the mixed powder of Ag, Cu, Ti and diamond powder, wherein the mass of the diamond powder accounts for 10-30% of the total mass of the mixed powder of Ag, Cu, Ti and diamond powder, and the granularity of the diamond powder is 0.1-100 mu m.
2. The diamond film high efficiency heat dissipation material of claim 1, wherein: the diamond self-supporting film is prepared by adopting a CVD method.
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