CN110394521A - Diamond film high efficiency and heat radiation material and preparation method thereof - Google Patents
Diamond film high efficiency and heat radiation material and preparation method thereof Download PDFInfo
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- CN110394521A CN110394521A CN201910711380.2A CN201910711380A CN110394521A CN 110394521 A CN110394521 A CN 110394521A CN 201910711380 A CN201910711380 A CN 201910711380A CN 110394521 A CN110394521 A CN 110394521A
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- Prior art keywords
- powder
- diamond
- diamond film
- high efficiency
- heat radiation
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Classifications
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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
-
- 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 present invention is a kind of diamond film high efficiency and heat radiation material and preparation method thereof, the heat sink material from top to bottom successively includes the upper, middle and lower three parts, the freestanding diamond film that upper layer is 20-500 μm of thickness, middle layer is the weld metal zone containing bortz powder, and lower layer is diamond/copper composite material.The heat sink material the preparation method comprises the following steps: using Ag, Cu, Ti, diamond mixed powder as activated rosin flux, the aufwuchsplate of freestanding diamond film and diamond/copper composite plate weld are got up using vacuum welding, that is, obtain the diamond high efficiency and heat radiation material.Due to containing bortz powder in weld metal zone thermoresistance layer is not present, while substrate uses diamond/copper composite material, heat sink material integral heat sink function admirable, thermal conductivity is higher than 600W/(mK in heat sink material of the present invention).In addition, freestanding diamond film thickness needed for the method for the present invention is thin, it is at low cost；It is easy to operate, it can be achieved that large-scale batch production.
Description
Technical field
The present invention relates to thermal management materials and its technical field of preparation, specifically a kind of diamond film high efficiency and heat radiation material
And preparation method thereof.
Background technique
Modern electronic technology rapid development, electronic component have higher integrated level and faster running speed, device
Calorific value increases sharply, and to the heat-sinking capability of electronic package material, more stringent requirements are proposed.And the ceramic material used now
(AlN, Al2O3, SiC) and metal-base composites (Cu-W, Cu-Mo, Al-SiC) etc. be increasingly unable to satisfy and rapidly and efficiently radiate
Demand.Therefore, future electronic encapsulating material must upgrade, and realize the function of quickly removing heat.
Diamond is the highest substance of thermal conductivity in nature, and thermal conductivity is up to 2000W/(mK at room temperature), it is approximately copper
5 times, while its thermal expansion coefficient is very low, is one of optimal electronic package material.Currently in order to realizing diamond in electricity
The application in sub- encapsulating material field, the main diamond using diamond/Cu composite material is prepared into or by thickness greater than 300 μm
Thick film is welded on the mode that composite sheet is prepared into Cu substrate.For diamond/Cu composite material, thermal conductivity generally be can reach
440-500W/(mK), still distant apart from the thermal conductivity of diamond.In addition, its machinability is very poor, and electronic package material
Requirement to surface smoothness and size is very stringent, causes it using relatively difficult.It is compound for diamond thick-film/Cu welding
Piece, then there are following several respects: 1) thickness of diamond is big, and preparation cost is high, and the high rigidity of diamond keeps its polishing tired
Difficulty, polishing process is complicated, and cost further increases；2) diamond and copper welding difficulty generally use Ag-Cu-Ti activated solder
It being welded, Ti is added to form TiC as active metal, increase the wellability of diamond, however the thermal conductivity of Ti and TiC
Rate is all very low, and existing in weld seam will lead to form thermoresistance layer；3) diamond thermal conductivity is very high, and Cu thermal conductivity is only 400W/
(mK), this makes the thermal conductivity of composite soldering entirety still relatively low.
Patent of invention CN201810580016.2 discloses a kind of preparation method of diamond film-copper heat sink compound, real
Show the welding of 50 ~ 100 μm of thickness of diamond and copper, although reducing the thickness and cost of diamond film, weld seam heat
Resistance layer and the lower problem of Cu substrate thermal conductivity still have.
The radiating requirements of future electronic encapsulating material, diamond/Cu can not be adapted in order to solve current material heat dissipation performance
Composite processing difficulty is high, and heat dissipation performance differs greatly with diamond, and welding prepares diamond film-copper heat sink material to Buddha's warrior attendant
The problems such as stone thickness requirement is high, and solder layer will form thermoresistance layer and simple copper-based bottom weak heat-dissipating, urgent need research and development novel low-cost,
Diamond-Cu composite heat dissipation material with excellent heat dispersion performance.
Summary of the invention
The purpose of the invention is to make up the defect of the prior art, future can not be adapted to by solving current material heat dissipation performance
The radiating requirements of electronic package material, realize the utilization of this heat sink material haveing excellent performance of diamond, and provide a kind of Buddha's warrior attendant
Stone film high efficiency and heat radiation material and preparation method thereof.
The present invention is achieved through the following technical solutions:
A kind of diamond film high efficiency and heat radiation material from top to bottom successively includes the upper, middle and lower three parts；Wherein, upper layer
For 20-500 μm of thickness of freestanding diamond film, using as heat source contact layer；Middle layer is the weld metal zone containing bortz powder, with
As heat conduction layer；Lower layer is diamond/copper composite material, using as heat conduction layer.
Freestanding diamond film is prepared using CVD method as a preferred technical solution,.
Further, the present invention also provides the preparation method of above-mentioned diamond film high efficiency and heat radiation material, specifically include as
Lower step:
1) using centainly match Ag powder, Cu powder, Ti powder, bortz powder mixed powder as activated rosin flux, using borax as helping weldering
Agent is modulated into paste flux, and is brushed on the surface of diamond/copper composite material；
2) growth of freestanding diamond film is placed on the surface of diamond/copper composite material down, and diamond from
Implement downward pressure on support membrane to it, then uses vacuum drying oven by freestanding diamond film and diamond/copper composite material
High temperature is heated to be welded to get the diamond film high efficiency and heat radiation material.
When making activated rosin flux as a preferred technical solution, first by Ag powder, Cu powder and Ti powder be uniformly mixed obtained Ag,
Cu, Ti mixed powder, wherein the quality of Ag powder accounts for the 55-70% of mixed powder gross mass, and it is total that the quality of Cu powder accounts for mixed powder
The 20-30% of quality；The quality of Ti powder accounts for the 10-15% of mixed powder gross mass；Then bortz powder and Ag, Cu, Ti are mixed again
It closes powder and is uniformly mixed obtained Ag, Cu, Ti, bortz powder mixed powder, wherein the quality of bortz powder accounts for Ag, Cu, Ti, gold
The 10-30% of emery mixed powder gross mass.
The granularity of bortz powder is 0.1-100 μm as a preferred technical solution,.
The pressure implemented on freestanding diamond film as a preferred technical solution, is 0.1-10Mpa.
When welding in vacuum drying oven as a preferred technical solution, holding temperature is 700-950 DEG C, soaking time 5-
30min。
Beneficial effects of the present invention are as follows:
1) novel diamond film high efficiency and heat radiation material of the invention, by freestanding diamond film layer, containing the weld metal zone of bortz powder
Layer and diamond/Cu composite material base bottom are constituted, containing with high thermal conductivity and relatively low thermel expansion system in trilaminate material
Several diamonds can greatly improve the heat-sinking capability of entire heat sink material, and the thermal conductivity of heat sink material of the present invention is up to 600W/
(mK) more than；Wherein, freestanding diamond film can be effectively conducted the heat of heat source generation, weld seam layer as heat source contact layer
The heat conduction layer constituted with diamond/Cu composite layer can more efficiently conduct heat while not send out due to increasing diamond
Raw biggish deflection；Weld seam layer containing bortz powder can effectively improve the situation that conventional weld layer forms thermal resistance.
2) present invention prepares relatively thin freestanding diamond film using CVD method and can meet the requirements, using surface smoothness
Higher monocrystalline silicon or other materials are ok as diamond growth substrate, do not need to throw diamond after removing substrate
Light processing, or only need simple polishing treatment that can meet smoothness requirements, the preparation and polishing of the diamond substantially reduced
Cost.
3) operation of the present invention is simple, it is only necessary to by diamond film and diamond/Cu composite material external pressure under vacuum conditions
Under the conditions of heat welding, can form novel diamond film-copper high efficiency and heat radiation material of meet demand, extensive batch easy to accomplish
Quantization production.
Detailed description of the invention
Attached drawing herein is used to provide to further explanation of the invention, constitutes part of this application, of the invention shows
Meaning property embodiment and its explanation are used to explain the present invention, not constitute improper limitations of the present invention.
Fig. 1 is the structural schematic diagram of diamond film high efficiency and heat radiation material of the present invention.
Fig. 2 is that diamond film high efficiency and heat radiation material of the present invention prepares schematic diagram.
In figure: 1- freestanding diamond film, the weld metal zone 2-, 3- diamond/copper composite material, 4- paste flux, 5- weight.
Specific embodiment
In order to make those skilled in the art better understand the present invention, below in conjunction with reference attached drawing and in conjunction with the embodiments to this
Further clear, complete explanation is made in invention.It should be noted that in the absence of conflict, embodiment in the application and
Feature in embodiment can be combined with each other.
The present invention provides a kind of diamond film high efficiency and heat radiation material, structure is constructed as shown in Figure 1, from top to bottom successively
Including the upper, middle and lower three parts；Wherein, upper layer is 20-500 μm of thickness of diamond being prepared by CVD method
Self-supported membrane 1, using as heat source contact layer；Middle layer is the weld metal zone 2 containing bortz powder, using as heat conduction layer；Lower layer is
Diamond/copper composite material 3, using as heat conduction layer.
The present invention also provides the preparation methods of above-mentioned diamond film high efficiency and heat radiation material, as shown in Fig. 2, specifically include as
Lower step:
1) using centainly match Ag powder, Cu powder, Ti powder, bortz powder mixed powder as activated rosin flux, using borax as helping weldering
Agent is modulated into paste flux, and brushes 4 meaning of appended drawing reference in the surface of diamond/copper composite material 3, i.e. Fig. 2
Paste flux；When making activated rosin flux, Ag powder, Cu powder and Ti powder are first uniformly mixed obtained Ag, Cu, Ti mixed powder, wherein
The quality of Ag powder accounts for the 55-70% of mixed powder gross mass, and the quality of Cu powder accounts for the 20-30% of mixed powder gross mass；Ti powder
Quality accounts for the 10-15% of mixed powder gross mass；Then bortz powder is uniformly mixed again with Ag, Cu, Ti mixed powder and is made
Ag, Cu, Ti, bortz powder mixed powder, wherein the quality of bortz powder accounts for Ag, Cu, Ti, the total matter of bortz powder mixed powder
The 10-30% of amount, the granularity of bortz powder are 0.1-100 μm；
2) growth of freestanding diamond film 1 is placed on to the diamond/copper composite material 3 for having brushed paste flux 4 down
Surface, and implement downward pressure to it on freestanding diamond film 1, the pressure of implementation is 0.1-10Mpa, specific implementation
When on freestanding diamond film 1 place weight 5；Then use vacuum drying oven by freestanding diamond film 1 and diamond/copper
Composite material 3 is heated to high temperature and is welded, and holding temperature is 700-950 DEG C, soaking time 5-30min；Last institute to obtain the final product
The diamond film high efficiency and heat radiation material stated.
Below in conjunction with several specific products and its preparation embodiment, heat sink material of the present invention is further described:
Embodiment 1
A kind of diamond film high efficiency and heat radiation material from top to bottom successively includes the upper, middle and lower three parts；Wherein, upper layer
For 20 μm of thickness of freestanding diamond film 1 being prepared by CVD method, using as heat source contact layer；Middle layer is to contain gold
The weld metal zone 2 of emery, using as heat conduction layer；Lower layer is diamond/copper composite material 3, using as heat conduction layer.
The preparation method of above-mentioned diamond film high efficiency and heat radiation material, specifically comprises the following steps:
1) using centainly match Ag powder, Cu powder, Ti powder, bortz powder mixed powder as activated rosin flux, using borax as helping weldering
Agent is modulated into paste flux 4, and is brushed on the surface of diamond/copper composite material 3；When making activated rosin flux, first by Ag
Powder, Cu powder and Ti powder are uniformly mixed obtained Ag, Cu, Ti mixed powder, wherein the quality of Ag powder accounts for mixed powder gross mass
The quality of 55%, Cu powder accounts for the 30% of mixed powder gross mass；The quality of Ti powder accounts for the 15% of mixed powder gross mass；Then again will
Bortz powder is uniformly mixed with Ag, Cu, Ti mixed powder is made Ag, Cu, Ti, bortz powder mixed powder, wherein bortz powder
Quality account for Ag, Cu, Ti, bortz powder mixed powder gross mass 20%, the granularity of bortz powder is 0.1 μm；
2) growth of freestanding diamond film 1 is placed on to the surface of diamond/copper composite material 3 down, and in diamond
Weight 5 is placed on self-supported membrane 1 and implements downward pressure to it, and the pressure of implementation is 5Mpa；Then use vacuum drying oven by Buddha's warrior attendant
Stone self-supported membrane 1 is heated to high temperature with diamond/copper composite material 3 and is welded, and holding temperature is 800 DEG C, soaking time is
5min；The last diamond film high efficiency and heat radiation material to obtain the final product.
Embodiment 2
A kind of diamond film high efficiency and heat radiation material from top to bottom successively includes the upper, middle and lower three parts；Wherein, upper layer
For 230 μm of thickness of freestanding diamond film 1 being prepared by CVD method, using as heat source contact layer；Middle layer is to contain gold
The weld metal zone 2 of emery, using as heat conduction layer；Lower layer is diamond/copper composite material 3, using as heat conduction layer.
The preparation method of above-mentioned diamond film high efficiency and heat radiation material, specifically comprises the following steps:
1) using centainly match Ag powder, Cu powder, Ti powder, bortz powder mixed powder as activated rosin flux, using borax as helping weldering
Agent is modulated into paste flux 4, and is brushed on the surface of diamond/copper composite material 3；When making activated rosin flux, first by Ag
Powder, Cu powder and Ti powder are uniformly mixed obtained Ag, Cu, Ti mixed powder, wherein the quality of Ag powder accounts for mixed powder gross mass
The quality of 70%, Cu powder accounts for the 20% of mixed powder gross mass；The quality of Ti powder accounts for the 10% of mixed powder gross mass；Then again will
Bortz powder is uniformly mixed with Ag, Cu, Ti mixed powder is made Ag, Cu, Ti, bortz powder mixed powder, wherein bortz powder
Quality account for Ag, Cu, Ti, bortz powder mixed powder gross mass 10%, the granularity of bortz powder is 55 μm；
2) growth of freestanding diamond film 1 is placed on to the surface of diamond/copper composite material 3 down, and in diamond
Weight 5 is placed on self-supported membrane 1 and implements downward pressure to it, and the pressure of implementation is 10Mpa；Then use vacuum drying oven by Buddha's warrior attendant
Stone self-supported membrane 1 is heated to high temperature with diamond/copper composite material 3 and is welded, and holding temperature is 950 DEG C, soaking time is
15min；The last diamond film high efficiency and heat radiation material to obtain the final product.
Embodiment 3
A kind of diamond film high efficiency and heat radiation material from top to bottom successively includes the upper, middle and lower three parts；Wherein, upper layer
For 500 μm of thickness of freestanding diamond film 1 being prepared by CVD method, using as heat source contact layer；Middle layer is to contain gold
The weld metal zone 2 of emery, using as heat conduction layer；Lower layer is diamond/copper composite material 3, using as heat conduction layer.
The preparation method of above-mentioned diamond film high efficiency and heat radiation material, specifically comprises the following steps:
1) using centainly match Ag powder, Cu powder, Ti powder, bortz powder mixed powder as activated rosin flux, using borax as helping weldering
Agent is modulated into paste flux 4, and is brushed on the surface of diamond/copper composite material 3；When making activated rosin flux, first by Ag
Powder, Cu powder and Ti powder are uniformly mixed obtained Ag, Cu, Ti mixed powder, wherein the quality of Ag powder accounts for mixed powder gross mass
The quality of 60%, Cu powder accounts for the 25% of mixed powder gross mass；The quality of Ti powder accounts for the 15% of mixed powder gross mass；Then again will
Bortz powder is uniformly mixed with Ag, Cu, Ti mixed powder is made Ag, Cu, Ti, bortz powder mixed powder, wherein bortz powder
Quality account for Ag, Cu, Ti, bortz powder mixed powder gross mass 30%, the granularity of bortz powder is 100 μm；
2) growth of freestanding diamond film 1 is placed on to the surface of diamond/copper composite material 3 down, and in diamond
Weight 5 is placed on self-supported membrane 1 and implements downward pressure to it, and the pressure of implementation is 0.1Mpa；It then will be golden using vacuum drying oven
Hard rock self-supported membrane 1 is heated to high temperature with diamond/copper composite material 3 and is welded, and holding temperature is 700 DEG C, soaking time
For 30min；The last diamond film high efficiency and heat radiation material to obtain the final product.
The above is that technical solution in the embodiment of the present invention is clearly and completely described, described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel all other embodiment obtained without creative efforts belongs to the model that the present invention protects
It encloses.
Claims (8)
1. a kind of diamond film high efficiency and heat radiation material, which is characterized in that from top to bottom successively include the upper, middle and lower three
Point, wherein the freestanding diamond film that upper layer is 20-500 μm of thickness, middle layer are the weld metal zone containing bortz powder, and lower layer is
Diamond/copper composite material.
2. diamond film high efficiency and heat radiation material according to claim 1, it is characterised in that: freestanding diamond film uses
CVD method is prepared.
3. the preparation method of diamond film high efficiency and heat radiation material as claimed in claim 1 or 2, which is characterized in that including as follows
Step: 1) using centainly match Ag powder, Cu powder, Ti powder, bortz powder mixed powder as activated rosin flux, using borax as helping weldering
Agent is modulated into paste flux, and is brushed on the surface of diamond/copper composite material；2) by the life of freestanding diamond film
Length is placed on the surface of diamond/copper composite material down, and implements downward pressure to it on freestanding diamond film,
Then freestanding diamond film high temperature is heated to diamond/copper composite material using vacuum drying oven to weld to get described
Diamond film-copper high efficiency and heat radiation material.
4. the preparation method of diamond film high efficiency and heat radiation material according to claim 3, it is characterised in that: production activity weldering
When agent, Ag powder, Cu powder and Ti powder are first uniformly mixed obtained Ag, Cu, Ti mixed powder, wherein the quality of Ag powder accounts for mixed powder
The quality of the 55-70% of body gross mass, Cu powder accounts for the 20-30% of mixed powder gross mass；The quality of Ti powder accounts for the total matter of mixed powder
The 10-15% of amount；Then bortz powder obtained Ag, Cu, Ti, bortz powder is uniformly mixed with Ag, Cu, Ti mixed powder again to mix
Close powder, wherein the quality of bortz powder account for Ag, Cu, Ti, bortz powder mixed powder gross mass 10-30%.
5. the preparation method of diamond film high efficiency and heat radiation material according to claim 3, it is characterised in that: bortz powder
Granularity is 0.1-100 μm.
6. the preparation method of diamond film high efficiency and heat radiation material according to claim 4, it is characterised in that: bortz powder
Granularity is 0.1-100 μm.
7. the preparation method of diamond film high efficiency and heat radiation material according to claim 3, it is characterised in that: diamond props up certainly
The pressure implemented on support film is 0.1-10Mpa.
8. the preparation method of diamond film high efficiency and heat radiation material according to claim 3, it is characterised in that: welded in vacuum drying oven
When connecing, holding temperature is 700-950 DEG C, soaking time 5-30min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113084176A (en) * | 2021-04-09 | 2021-07-09 | 武汉工程大学 | Self-supporting diamond film/Cu composite heat sink material and preparation method thereof |
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| CN1258580A (en) * | 1999-12-27 | 2000-07-05 | 华南理工大学 | Active solder and its preparation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113084176B (en) * | 2021-04-09 | 2023-08-18 | 武汉工程大学 | Self-supporting diamond film/Cu composite heat sink material and preparation method thereof |
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| CN110394521B (en) | 2021-03-23 |
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