CN108179302A - A kind of preparation method of high heat-conductive diamond/carbon/carbon-copper composite material - Google Patents
A kind of preparation method of high heat-conductive diamond/carbon/carbon-copper composite material Download PDFInfo
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- CN108179302A CN108179302A CN201810089819.8A CN201810089819A CN108179302A CN 108179302 A CN108179302 A CN 108179302A CN 201810089819 A CN201810089819 A CN 201810089819A CN 108179302 A CN108179302 A CN 108179302A
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- 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
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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- 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
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/1015—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform
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- 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
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/1015—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform
- C22C1/1021—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform the preform being ceramic
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C9/00—Alloys based on copper
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Abstract
A kind of preparation method of high heat-conductive diamond/carbon/carbon-copper composite material, is related to a kind of preparation method of composite material.The purpose of the present invention is to solve existing diamond carbon/carbon-copper composite material preparation method can not realize the near-net-shape of large scale thin slice exemplar, high quality, be prepared on a large scale the problem of.Preparation method：Bortz powder is fitted into jolt ramming in mold and makes precast body, precast body is placed in crucible, and fine copper or blocky copper alloy are positioned over precast body top, vacuumized, and heat up molten copper under inert gas shielding, pressure impregnation, pressurize cooling, and release finally demoulds.Advantageous effect：The method of the present invention can realize high efficiency volume production, high mechanical properties, and high yield rate can prepare large scale thin slice exemplar, and exemplar thermal conductivity improves, and manufacturing cost is low, and impurity content is few, and molding die and crucible can be reused.The present invention is suitable for preparing high heat-conductive diamond/carbon/carbon-copper composite material.
Description
Technical field
The present invention relates to a kind of preparation methods of composite material.
Background technology
With the continuous improvement of chip integration, Electronic Packaging develops to miniaturization, lightweight and high performance direction, makes
The operating temperature for obtaining circuit constantly rises, and the constantly increase of system unit volume heat generation rate leads to system job insecurity.In order to obtain
Obtain stable performance, it is necessary to improve radiating condition, thus Electronic Packaging is constantly promoted in the importance of field of microelectronics, along with
The demand of New Materials for Electric Packing is also being continuously increased.High quality diamond is to be currently known the highest object of thermal conductivity in the world
Matter can reach 1800-2000W/ (mK), and be insulator at room temperature, also with the spies such as dielectric constant is low, coefficient of thermal expansion is low
Point, but single diamond is not easy to make encapsulating material, and cost is very high, it is comparatively ideal to be made as metal-base composites.
Metallic copper has excellent an electric conductivity and heat conductivility, and the thermal conductivity of metallic copper is 404W/ (mK), coefficient of thermal expansion 16.8
×10-6/K；There is diamond/copper based composites thermal conductivity to be higher than conventional metallic alloys and aluminium nitride ceramics material, thermal expansion
The advantages that coefficient matches with semi-conducting material, is corrosion-resistant in seawater salt mist environment, therefore suitable for electricity such as phased-array radars
Son encapsulation and thermal management materials.
Difficult point prepared by diamond/copper based composites is：(1) wetability of diamond and copper is poor, gold at 1150 DEG C
The angle of wetting of hard rock and copper is 145 °；(2) diamond does not have solid phase reaction with copper high temperature, and carbon does not have solid solubility in copper,
Therefore, it is difficult to be sintered out fine and close composite material.By Modified Diamond, carbide is such as added in, it can be with one
The new problem for increasing interface resistance is brought again while determining the wetability of degree improvement diamond and copper, but be modified, and influences Buddha's warrior attendant
The thermal conductivity and coefficient of thermal expansion of stone/Cu-base composites.(3) diamond graphitization problem, in air, diamond 773K with
Under may be graphitized completely.Under vacuum condition, part graphitization phenomenon takes place in 970K-1670K diamonds, when temperature is higher than
2070K, diamond are graphitized completely.
The main preparation methods of existing diamond reinforced Cu-matrix compound material have：Pressure infiltration method/high pressure infiltration method,
SPS spark plasma sinterings method, powder metallurgic method, gas pressure infiltration method etc..The Guo Hong subjects of Beijing Non-Ferrous Metal Research General Academy
The thermal conductivity 620W/mK for the Diamond/CuCr0.8 composite materials that group is prepared with pressure infiltration method.It is set needed for pressure infiltration method
Standby is vacuum hotpressing infiltration stove, and the pressure of gas needed for pressure infiltration method is megapascal (MPa) grade.Beijing Non-Ferrous Metal Research General Academy
Guo Hong seminars also using high pressure infiltration method prepare Diamond/CuCr0.8 composite materials, thermal conductivity reach 700W/mK, this
Method makes part diamond realize glomerocryst, but diamond fraction crushes in the method preparation process, can be to stability of material and can
It is impacted by property, required equipment is special equipment, and specially cubic press, required pressure are Ji Pa (GPa) grades.
And the composite material prepared is confined to experiment small size exemplar, is not easy to realize large-scale mass production.Beijing University of Science ＆ Technology goes into business into factory etc.
People also report a kind of high heat conduction, low thermal coefficient of expansion diamond composite and preparation method thereof, using high temperature height
Infiltration method is pressed, needs to carry out super-pressure melting infiltration sintering under 500~2000 DEG C and 2~8GPa of pressure, the method also belongs to one
Kind high pressure infiltration method.What gold of University of Science ＆ Technology, Beijing walks slowly like a woman et al. diamond/copper boron prepared by the high temperature and pressure infiltration process of report, gold
Hard rock/copper zirconium composite material also belongs to a kind of high pressure infiltration method.Cubic apparatus equipment internal cavity volume is limited to, using high-voltage fuse
The yield that the method for oozing prepares diamond/copper based composites is relatively low.Discharge plasma sintering (SPS) technique have heating rate it is fast,
The advantages that short preparation period, but composite material consistency prepared by the method is relatively low, therefore thermal conductivity is not high, and is difficult to prepare
Thickness is less than the sheet metal specimens of 1mm.Two pressure heads are electrode up and down during discharge sintering, and sample is excessively thin to be equivalent to short circuit,
It can not complete temperature, time, pressure controlled sintering process.Protective atmosphere can be filled when generally preparing material with the method, is protected
Atmosphere can remain in material internal, have a large amount of closed pore holes, and then lead to that density is low and there is a hole at interface, therefore composite material
Thermal conductivity is low.The reaction time of powder metallurgic method is longer, and the ball milling of powder metallurgic method mixes powder and is readily incorporated impurity in the process, thus
It is prepared by the high-quality for being difficult to realize diamond/copper based composites；Powder metallurgic method and other methods especially gas pressure infiltration side
Method is compared, and bortz powder is not tightly packed in powder metallurgic method, thus is difficult to prepare high-volume fractional diamond/copper base compound
Material.Diamond/copper composite material prepared by powder metallurgic method is compared with material prepared by gas pressure infiltration method, identical diamond
In the case of particle size and volume fraction, thermal conductivity is relatively low.In conclusion the preparation side of existing diamond/copper composite material
Method can not realize the near-net-shape of large scale thin slice exemplar and be difficult to realize high quality and be prepared on a large scale.
Invention content
Preparation method the purpose of the present invention is to solve existing diamond/copper composite material can not realize that large scale is thin
The near-net-shape of piece exemplar, high quality, the problem of being prepared on a large scale, provide a kind of high heat-conductive diamond/Cu-base composites
Preparation method.
The preparation method of high heat-conductive diamond/Cu-base composites of the present invention carries out according to the following steps：
Step 1：It weighs surface and is coated with the diamond original powder of film plating layer and be fitted into molding die and carry out jolt ramming processing,
Make precast body；Precast body is positioned in crucible, blocky fine copper or blocky copper alloy are positioned over precast body top in crucible,
Crucible is positioned in gas pressure infiltration stove；
Or diamond original powder is taken to be fitted into molding die and carries out jolt ramming processing, make precast body；Precast body is placed
In crucible, blocky copper alloy is positioned over precast body top in crucible, crucible is positioned in gas pressure infiltration stove；
Molding die is placed on supersonic oscillations plate during jolt ramming processing, vibrate 5 under the frequency of 20~30kHz~
15 minutes；
The material of the film plating layer is W, Cr, Mo or Ti；50~5000nm of thickness of the film plating layer；
The bortz powder original powder or surface are coated with a diameter of 50~400 μm of the diamond original powder of film plating layer；
The material of the molding die is high purity graphite or isostatic pressing formed graphite；
The material of the crucible is high purity graphite or isostatic pressing formed graphite；
The diamond original powder of the bulk fine copper or blocky copper alloy and jolt ramming treated surface is coated with film plating layer
Mass ratio is (0.85~2.07)：1；
The mass ratio of bulk copper alloy and the jolt ramming treated diamond original powder is (0.85~2.07)：1；
The material of the bulk copper alloy is copper zirconium alloy, chromiumcopper, copper-titanium alloy or Cu-B alloy；
Wherein, since copper is nonwetting with graphite, crucible and molding die contacted at high temperature under high pressure with copper solution
It is injury-free in journey, therefore molding die and crucible can be reused；
Step 2：It is 0.1~1Pa by gas pressure infiltration stove evacuation to vacuum degree；
Wherein, the purpose vacuumized is residual gas in discharge precast body；
Step 3：Gas pressure infiltration stove is warming up to more than blocky fine copper or blocky copper alloy fusing point under inert gas shielding
100~250 DEG C and keep the temperature 1h~3h；The inert gas pressure is 0.1~1MPa；
The purpose that 0.1~1MPa inert gases are passed through in copper or copper alloy fusion process is to prevent the copper of melting or copper from closing
Golden excessive vaporization and lose, the evaporation behavior of copper or copper alloy is related with air pressure, and pressure is higher, and evaporation rate is slower；In inertia
Fine copper or copper alloy is made to melt and be kept molten by under gas atmosphere, while copper or copper alloy melt flow downwardly into earthenware
Precast body is encased and completely cuts off gas by crucible；
Step 4：Inert gas and pressurize are passed through into gas pressure infiltration stove, pressurize terminates postcooling, release and demoulding, i.e.,
It completes；
The air pressure of the inert gas is 1~10MPa；The time of the pressurize is 10min~3h；The cooling velocity is
3~5 DEG C/min；
Wherein, be passed through high-pressure inert gas into gas pressure infiltration stove and pressurize make melting fine copper or copper alloy melt from into
Type mould gate is flowed into inside molding die and is penetrated into the gap of diamond powder.
It the principle of the invention and has the beneficial effect that：
1st, bortz powder and mold are made precast body, forming essence by the present invention using gas pressure infiltration and near-net-shape technique
Degree is high, uniform force.Composite material is prepared using GPa stage pressures and cubic apparatus equipment compared to existing high pressure infiltration technique,
The method of the present invention pressure is small, and exemplar is protected, therefore exemplar is not caused to damage by mold, ensures exemplar in preparation process not
Underbead crack is generated, therefore prepares high yield rate, preparation efficiency is high, can realize the large scale that broad practice needs
The high quality of thin slice exemplar is prepared on a large scale production, and sample thickness prepared by the present invention is 0.5~3mm；Simultaneously compared to six faces
Equipment is pushed up, the furnace inner space of gas pressure infiltration stove that the present invention uses is larger, can by exemplar position and the design mold of rationally arranging
To realize high efficiency volume production；
2nd, the diamond/copper composite material interface combination of prior art preparation is weaker, and boundary layer has hole or boundary layer
Discontinuously, thermal conductivity and the mechanical property for leading to composite material are very low, and coefficient of thermal expansion is very high.The present invention prepares high thermal conductive diamond
During stone/carbon/carbon-copper composite material, diamond reinforcement can generate coating element carbide, diamond enhancing with coating element reaction
Body can generate alloying element carbide, therefore in diamond reinforcement and the boundary layer of matrix alloy with the element reaction in alloy
Generate fine and close and continuous carbide interface layer.The interface cohesion between reinforcement and matrix is promoted, reduces interface heat
Resistance, so as to improve the thermal conductivity of integral composite；
3rd, the composite material consistency that prepared by the present invention is higher, therefore thermal conductivity is higher；In the Buddha's warrior attendant that grain size is 100 microns
The titanium layer that mountain flour surface plating thickness is 1000 nanometers, the high heat-conductive diamond/composite copper material obtained after compound with CuCr0.5 alloys
The thermal conductivity of material is 530W/mK, and mean thermal expansion coefficients are 6.5 × 10 when environment temperature is 30~100 DEG C-6/K；
4th, the method for the present invention is under protective atmosphere by heating, prevent melting copper or copper alloy excessive vaporization and lose,
The dosage of copper or copper alloy is drastically reduced, reduces the manufacturing cost of composite material；
5th, the present invention excludes the residual gas in precast body and alloy by being vacuumized before infiltration；Then added by gas
Pressure infiltration, makes alloy melt encase precast body completely and completely cuts off gas, then under pneumatic pressure alloy fully penetrated to precast body
In；It is cooled down finally by pressurize, makes the effective feeding of process of setting, avoid occurring shrinkage cavity in composite material；
6th, without adding binding agent in the prefabricated production procedure of the present invention, impurity content is few；
7th, since copper and graphite are nonwetting, material exists for the crucible and molding die of high purity graphite or isostatic pressing formed graphite
With injury-free in copper solution contact process under high temperature and pressure, therefore molding die and crucible can be reused；
8th, it is existing when preparing diamond/copper composite material, it can cause to close if the volume fraction of diamond reinforcement is excessively high
The channel of golden melt flows is narrower, easily forms hole, thereby reduces the consistency of material, cause prepare diamond/
Carbon/carbon-copper composite material thermal conductivity and mechanical property can also decline.Since the uniform and stable control in temperature field is closed in fine copper or copper in the present invention
More than golden fusing point 100~250 DEG C, copper or copper alloy fluidity of molten are good, therefore can prepare highest and contain volume fraction and be
75% bortz powder reinforcement diamond/copper composite material, while improving the volume fraction of bortz powder reinforcement not
Institutional framework is destroyed, does not influence the thermophysical property and mechanical property of diamond/copper composite material.
Description of the drawings
Fig. 1 is the preparation process schematic diagram of high heat-conductive diamond/carbon/carbon-copper composite material component in embodiment 1；In figure, step a
For state of the copper alloy blocky in gas pressure infiltration stove when unfused, step b is when blocky copper alloy melts in gas pressure infiltration stove
State, step c are the state after blocky copper alloy solidification in gas pressure infiltration stove, and 1 represents gas pressure infiltration stove in figure, and 2 represent prefabricated
Body core model, 3 represent crucible, and 4 represent blocky copper alloy；
Fig. 2 is that high heat-conductive diamond/carbon/carbon-copper composite material is signed an undertaking with shaping mould used in component preparation process in embodiment 1
Structure schematic diagram, 1 is cast gate in figure, and 2 be mold cavity, and 3 be die main body；
Fig. 3 is high heat-conductive diamond/carbon/carbon-copper composite material Fracture scan photo prepared by embodiment 1；
Fig. 4 is the interface topography figure of high heat-conductive diamond/carbon/carbon-copper composite material prepared by embodiment 1, and 1 is chromium carbide, and 2 be carbon
Change titanium；
Fig. 5 is the three-point bending performance curve of high heat-conductive diamond/carbon/carbon-copper composite material prepared by embodiment 1 and comparative example 1
Scheme, the three-point bending performance curve for high heat-conductive diamond/carbon/carbon-copper composite material that curve 1 is prepared for embodiment 1, curve 2 are in figure
The three-point bending performance curve of diamond/copper composite material prepared by comparative example 1；
Fig. 6 is the interface topography figure of high heat-conductive diamond/carbon/carbon-copper composite material prepared by embodiment 2, and 1 is chromium carbide in figure, 2
For tungsten carbide；
Fig. 7 is high heat-conductive diamond/lateral pictorial diagram of carbon/carbon-copper composite material component prepared by embodiment 2；
Fig. 8 is high heat-conductive diamond/carbon/carbon-copper composite material component forward direction pictorial diagram prepared by embodiment 2；
Fig. 9 is the interface topography figure of high heat-conductive diamond/carbon/carbon-copper composite material prepared by embodiment 5, and 1 is chromium carbide in figure.
Specific embodiment：
Technical solution of the present invention is not limited to act specific embodiment set forth below, further includes between each specific embodiment
Arbitrary reasonable combination.
Specific embodiment one：The preparation method of present embodiment high heat-conductive diamond/carbon/carbon-copper composite material is according to the following steps
It carries out：
Step 1：It weighs surface and is coated with the diamond original powder of film plating layer and be fitted into molding die and carry out jolt ramming processing,
Make precast body；Precast body is positioned in crucible, blocky fine copper or blocky copper alloy are positioned over precast body top in crucible,
Crucible is positioned in gas pressure infiltration stove；Or diamond original powder is taken to be fitted into molding die and carries out jolt ramming processing, it makes pre-
Body processed；Precast body is positioned in crucible, blocky copper alloy is positioned over precast body top in crucible, crucible is positioned over air pressure
In infiltration furnace；
The material of the molding die is high purity graphite or isostatic pressing formed graphite；
The material of the crucible is high purity graphite or isostatic pressing formed graphite；
Step 2：It is 0.1~1Pa by gas pressure infiltration stove evacuation to vacuum degree；
Step 3：Gas pressure infiltration stove is warming up to more than blocky fine copper or blocky copper alloy fusing point under inert gas shielding
100~250 DEG C and keep the temperature 1h~3h；
The inert gas pressure is 0.1~1MPa；
Step 4：Inert gas and pressurize are passed through into gas pressure infiltration stove, pressurize terminates postcooling, release and demoulding, i.e.,
It completes；
The air pressure of the inert gas is 1~10MPa；
The time of the pressurize is 10min~3h.
It present embodiment principle and has the beneficial effect that：
1st, present embodiment uses gas pressure infiltration and near-net-shape technique, and bortz powder and mold are made precast body, into
Shape precision is high, uniform force.Composite wood is prepared using GPa stage pressures and cubic apparatus equipment compared to existing high pressure infiltration technique
Material, present embodiment method pressure is small, and exemplar is protected, therefore exemplar is not caused to damage by mold, ensures prepared by exemplar
Underbead crack is not generated in the process, therefore prepares high yield rate, and preparation efficiency is high, can realize broad practice needs
The high quality of large scale thin slice exemplar be prepared on a large scale production, sample thickness prepared by present embodiment is 0.5~3mm；Together
When compared to cubic apparatus equipment, the furnace inner space of gas pressure infiltration stove that present embodiment uses is larger, passes through exemplar of rationally arranging
Position and design mold, can realize high efficiency volume production；
2nd, the diamond/copper composite material interface combination of prior art preparation is weaker, and boundary layer has hole or boundary layer
Discontinuously, thermal conductivity and the mechanical property for leading to composite material are very low, and coefficient of thermal expansion is very high.Present embodiment prepares high heat conduction
In diamond/copper composite material, diamond reinforcement can generate coating element carbide, diamond with coating element reaction
Reinforcement can generate alloying element carbide, therefore in diamond reinforcement and the boundary of matrix alloy with the element reaction in alloy
Face layer generates fine and close and continuous carbide interface layer.The interface cohesion between reinforcement and matrix is promoted, reduces boundary
Face thermal resistance, so as to improve the thermal conductivity of integral composite；
3rd, the composite material consistency that prepared by present embodiment is higher, therefore thermal conductivity is higher；It it is 100 microns in grain size
The titanium layer that bortz powder surface plating thickness is 1000 nanometers, the high heat-conductive diamond/copper obtained after compound with CuCr0.5 alloys are multiple
The thermal conductivity of condensation material is 530W/mK, and mean thermal expansion coefficients are 6.5 × 10 when environment temperature is 30~100 DEG C-6/K；
4th, present embodiment method prevents the copper melted or copper alloy excessive vaporization and damages by being heated under protective atmosphere
It loses, drastically reduces the dosage of copper or copper alloy, reduce the manufacturing cost of composite material；
5th, present embodiment excludes the residual gas in precast body and alloy by being vacuumized before infiltration；Then pass through gas
Body osmosis makes alloy melt encase precast body completely and completely cuts off gas, then under pneumatic pressure alloy fully penetrated to pre-
In body processed；It is cooled down finally by pressurize, makes the effective feeding of process of setting, avoid occurring shrinkage cavity in composite material；
6th, without adding binding agent in the prefabricated production procedure of present embodiment, impurity content is few；
7th, since copper and graphite are nonwetting, material exists for the crucible and molding die of high purity graphite or isostatic pressing formed graphite
With injury-free in copper solution contact process under high temperature and pressure, therefore molding die and crucible can be reused；
8th, it is existing when preparing diamond/copper composite material, it can cause to close if the volume fraction of diamond reinforcement is excessively high
The channel of golden melt flows is narrower, easily forms hole, thereby reduces the consistency of material, cause prepare diamond/
Carbon/carbon-copper composite material thermal conductivity and mechanical property can also decline.Due in present embodiment the uniform and stable control in temperature field in fine copper or
More than copper alloy fusing point 100~250 DEG C, copper or copper alloy fluidity of molten are good, therefore can prepare highest and contain volume fraction
For 75% bortz powder reinforcement diamond/copper composite material, while improving the volume fraction of bortz powder reinforcement
Institutional framework is not destroyed, does not influence the thermophysical property and mechanical property of diamond/copper composite material.
Specific embodiment two：The present embodiment is different from the first embodiment in that：Blocky fine copper described in step 1
Or treated that the mass ratio of diamond original powder that surface is coated with film plating layer is (0.85~2.07) for blocky copper alloy and jolt ramming：
1.Other steps and parameter are same as the specific embodiment one.
Specific embodiment three：The mass ratio of blocky copper alloy described in step 1 and jolt ramming treated diamond original powder is
(0.85~2.07)：1.Other steps and parameter are the same as one or two specific embodiments.
Specific embodiment four：Unlike one of present embodiment and specific embodiment one to three：Described in step 1
Molding die is placed on supersonic oscillations plate by jolt ramming when handling, and is vibrated 5~15 minutes under the frequency of 20~30kHz.Other
Step and one of parameter and specific embodiment one to three are identical.
Specific embodiment five：Unlike one of present embodiment and specific embodiment one to four：Described in step 1
Bortz powder original powder or surface are coated with a diameter of 50~400 μm of the diamond original powder of film plating layer.Other steps and parameter with
One of specific embodiment one to four is identical.
Specific embodiment six：Unlike one of present embodiment and specific embodiment one to five：：Described in step 1
The material of blocky copper alloy is copper zirconium alloy, chromiumcopper, copper-titanium alloy or Cu-B alloy.Other steps and parameter and specific reality
It is identical to apply one of mode one to five.
Specific embodiment seven：Unlike one of present embodiment and specific embodiment one to six：Described in step 1
The material of film plating layer is W, Cr, Mo or Ti.Other steps and one of parameter and specific embodiment one to six are identical.
Specific embodiment eight：Unlike one of present embodiment and specific embodiment one to seven：Described in step 1
50~5000nm of thickness of film plating layer.Other steps and one of parameter and specific embodiment one to seven are identical.
Specific embodiment nine：Unlike one of present embodiment and specific embodiment one to eight：Described in step 3
Gas pressure infiltration stove is warming up to more than blocky fine copper or blocky copper alloy fusing point 250 DEG C under inert gas shielding and keeps the temperature 2h.
Other steps and one of parameter and specific embodiment one to eight are identical.
Specific embodiment ten：Unlike one of present embodiment and specific embodiment one to nine：Described in step 4
Cooling velocity is 3~5 DEG C/min.Other steps and one of parameter and specific embodiment one to nine are identical.
Beneficial effects of the present invention are verified using following embodiment：
Embodiment 1：
The preparation method of the present embodiment high heat-conductive diamond/Cu-base composites carries out according to the following steps：
Step 1：It weighs surface and is coated with the diamond original powder of film plating layer and be fitted into molding die and carry out jolt ramming processing,
Make precast body；Precast body is positioned in crucible, blocky copper alloy is positioned over precast body top in crucible, crucible is placed
In gas pressure infiltration stove；
Molding die is placed on supersonic oscillations plate during the jolt ramming processing, is vibrated 10 minutes under the frequency of 28kHz；
The material of the film plating layer is Ti；
The thickness 1000nm of the film plating layer；
The surface is coated with a diameter of 100 μm of the diamond original powder of film plating layer；
The material of the molding die is high purity graphite；
The material of the crucible is high purity graphite；
Treated that the mass ratio of diamond original powder that surface is coated with film plating layer is for bulk copper alloy and the jolt ramming
1.37：1；
The chromiumcopper that the material of the bulk copper alloy is 0.5~1.1wt.% containing chromium；
Step 2：It is 1Pa by gas pressure infiltration stove evacuation to vacuum degree；
Step 3：Gas pressure infiltration stove is warming up to more than blocky fine copper or blocky copper alloy fusing point under inert gas shielding
1200 DEG C and keep the temperature 1h；The inert gas pressure is 0.1MPa；
Step 4：Inert gas and pressurize are passed through into gas pressure infiltration stove, pressurize terminates postcooling, release and demoulding, i.e.,
It completes；
The air pressure of the inert gas is 1MPa；The time of the pressurize is 1h；The cooling velocity is 3 DEG C/min；
Diamond/copper based composites density manufactured in the present embodiment is 5.53g/cm3, it is diamond intensified in composite material
Strong body volume fraction 62%, the thermal diffusion coefficient of composite material is 220.598/mm2, thermal conductivity 530W/mK, room temperature (30
DEG C) to 100 DEG C of mean thermal expansion coefficients be 6.5 × 10-6/ K, room temperature (30 DEG C) to 200 DEG C of mean thermal expansion coefficients for 6.8 ×
10-6/ K, bending strength 320MPa.
Fig. 1 is the preparation process schematic diagram of high heat-conductive diamond/carbon/carbon-copper composite material component in embodiment 1；In figure, step a
For state of the copper alloy blocky in gas pressure infiltration stove when unfused, step b is when blocky copper alloy melts in gas pressure infiltration stove
State, step c are the state after blocky copper alloy solidification in gas pressure infiltration stove, and 1 represents gas pressure infiltration stove in figure, and 2 represent prefabricated
Body core model, 3 represent crucible, and 4 represent blocky copper alloy；Fig. 2 is high heat-conductive diamond/carbon/carbon-copper composite material and component in embodiment 1
Forming die structure schematic diagram used in preparation process, 1 is cast gate in figure, and 2 be mold cavity, and 3 be die main body；Fig. 3 is
High heat-conductive diamond/carbon/carbon-copper composite material Fracture scan photo prepared by embodiment 1；It can be seen from Fig. 3 that it is adhered on diamond particles
Chromiumcopper, therefore in high heat-conductive diamond/carbon/carbon-copper composite material of the preparation of embodiment 1, titanizing improves the profit of diamond and copper
It is moist；Fig. 4 is the interface topography figure of high heat-conductive diamond/carbon/carbon-copper composite material prepared by embodiment 1, and 1 is chromium carbide, and 2 be carbonization
Titanium；As shown in Figure 4, the boundary layer of the middle diamond/copper evanohm of high heat-conductive diamond/carbon/carbon-copper composite material is by titanium carbide and carbonization
Two layers carbide of chromium is formed, and for titanium carbide layer in inside, titanium carbide crystal grain is tiny, and discontinuously, the thickness of titanium carbide layer is about 200~
700nm is grown to diamond side；On the outside, chromium carbide coarse grains, more continuously, chromium carbide layer thickness are 0.6 to the layers of chrome that is carbonized
It~1.6 μm, is grown to copper alloy side；
Comparative example 1：
The preparation method of this comparative example high heat-conductive diamond/Cu-base composites carries out according to the following steps：
Step 1：It weighs bortz powder original powder to be fitted into molding die and carry out jolt ramming processing, makes precast body；It will be prefabricated
Body is positioned in crucible, and blocky fine copper is positioned over precast body top in crucible, crucible is positioned in gas pressure infiltration stove；
Molding die is placed on supersonic oscillations plate during the jolt ramming processing, is vibrated 10 minutes under the frequency of 28kHz；
A diameter of 100 μm of the bortz powder original powder；
The material of the molding die is high purity graphite；
The material of the crucible is high purity graphite；
The mass ratio of bulk fine copper and the jolt ramming treated diamond original powder is 1.37：1；
Step 2：It is 1Pa by gas pressure infiltration stove evacuation to vacuum degree；
Step 3：Gas pressure infiltration stove is warming up to more than blocky fine copper fusing point 1200 DEG C under inert gas shielding and is kept the temperature
1h；The inert gas pressure is 0.1MPa；
Step 4：Inert gas and pressurize are passed through into gas pressure infiltration stove, pressurize terminates postcooling, release and demoulding, i.e.,
It completes；
The air pressure of the inert gas is 1MPa；The time of the pressurize is 1h；The cooling velocity is 3 DEG C/min；
Diamond/copper based composites density prepared by comparative example 1 is 5.39g/cm3, thermal diffusion coefficient 83.784/
mm2, thermal conductivity 197.567W/mK, room temperature (30 DEG C) to 100 DEG C of mean thermal expansion coefficients is 13.1 × 10-6/ K, room temperature
(30 DEG C) to 200 DEG C of mean thermal expansion coefficients are 15.4 × 10-6/ K, bending strength 56MPa.
Fig. 5 is the three-point bending performance curve of high heat-conductive diamond/carbon/carbon-copper composite material prepared by embodiment 1 and comparative example 1
Scheme, the three-point bending performance curve for high heat-conductive diamond/carbon/carbon-copper composite material that curve 1 is prepared for embodiment 1, curve 2 are in figure
The three-point bending performance curve of diamond/copper composite material prepared by comparative example 1；
Fig. 5 can be seen that the mechanics after the interface improvement of high heat-conductive diamond/carbon/carbon-copper composite material of the preparation of embodiment 1
Performance significantly improves；
Embodiment 2：
The preparation method of the present embodiment high heat-conductive diamond/Cu-base composites carries out according to the following steps：
Step 1：It weighs surface and is coated with the diamond original powder of film plating layer and be fitted into molding die and carry out jolt ramming processing,
Make precast body；Precast body is positioned in crucible, blocky copper alloy is positioned over precast body top in crucible, crucible is placed
In gas pressure infiltration stove；
Molding die is placed on supersonic oscillations plate during the jolt ramming processing, is vibrated 10 minutes under the frequency of 28kHz；
The material of the film plating layer is W；
The thickness 100nm of the film plating layer；
The surface is coated with a diameter of 100 μm of the diamond original powder of film plating layer；
The material of the molding die is high purity graphite；
The material of the crucible is high purity graphite；
Treated that the mass ratio of diamond original powder that surface is coated with film plating layer is for bulk copper alloy and the jolt ramming
1.69：1；
The chromiumcopper that the material of the bulk copper alloy is 0.5~1.1wt.% containing chromium；
Step 2：It is 1Pa by gas pressure infiltration stove evacuation to vacuum degree；
Step 3：Gas pressure infiltration stove is warming up to more than blocky fine copper or blocky copper alloy fusing point under inert gas shielding
1300 DEG C and keep the temperature 1h；The inert gas pressure is 0.1MPa；
Step 4：Inert gas and pressurize are passed through into gas pressure infiltration stove, pressurize terminates postcooling, release and demoulding, i.e.,
It completes；
The air pressure of the inert gas is 1MPa；The time of the pressurize is 1h；The cooling velocity is 3 DEG C/min；
The volume fraction 65.3% of diamond reinforcement, the density of composite material are in composite material prepared by embodiment 2
5.37g/cm3, thermal diffusion coefficient 226.478/mm2, thermal conductivity 533W/mK, coefficient of thermal expansion is 8.5 × 10-6/K；Figure
The interface topography figure of the 6 high heat-conductive diamond/carbon/carbon-copper composite materials prepared for embodiment 2,1 is chromium carbide, and 2 be tungsten carbide, and Fig. 6 can
To find out, the boundary layer of diamond/copper evanohm is by tungsten carbide in high heat-conductive diamond/carbon/carbon-copper composite material prepared by embodiment 2
It is formed with chromium carbide.Fig. 7 is high heat-conductive diamond/lateral pictorial diagram of carbon/carbon-copper composite material component prepared by embodiment 2；Fig. 8 is real
Apply high heat-conductive diamond/carbon/carbon-copper composite material component forward direction pictorial diagram of the preparation of example 2；High heat-conductive diamond/copper prepared by embodiment 2
Composite element be square sheets shape, thickness 1.54mm, square length of side 80mm.
Embodiment 3：
The preparation method of the present embodiment high heat-conductive diamond/Cu-base composites carries out according to the following steps：
Step 1：It weighs surface and is coated with the diamond original powder of film plating layer and be fitted into molding die and carry out jolt ramming processing,
Make precast body；Precast body is positioned in crucible, blocky copper alloy is positioned over precast body top in crucible, crucible is placed
In gas pressure infiltration stove；
Molding die is placed on supersonic oscillations plate during the jolt ramming processing, is vibrated 10 minutes under the frequency of 28kHz；
The material of the film plating layer is Cr；
The thickness 100nm of the film plating layer；
The surface is coated with a diameter of 100 μm of the diamond original powder of film plating layer；
The material of the molding die is high purity graphite；
The material of the crucible is high purity graphite；
Treated that the mass ratio of diamond original powder that surface is coated with film plating layer is for bulk copper alloy and the jolt ramming
2.07：1；
The chromiumcopper that the material of the bulk copper alloy is 0.5~1.1wt.% containing chromium；
Step 2：It is 1Pa by gas pressure infiltration stove evacuation to vacuum degree；
Step 3：Gas pressure infiltration stove is warming up to more than blocky fine copper or blocky copper alloy fusing point under inert gas shielding
1200 DEG C and keep the temperature 1h；The inert gas pressure is 0.1MPa；
Step 4：Inert gas and pressurize are passed through into gas pressure infiltration stove, pressurize terminates postcooling, release and demoulding, i.e.,
It completes；
The air pressure of the inert gas is 1MPa；The time of the pressurize is 10min；The cooling velocity is 3 DEG C/min；
High heat-conductive diamond/carbon/carbon-copper composite material component prepared by embodiment 3 is square sheets shape, and thickness 0.8mm is square
Length of side 100mm；The volume fraction 65% of diamond reinforcement, composite density 5.38g/cm in composite material3, thermal diffusion
Coefficient is 195.748/mm2, thermal conductivity 461W/mK, coefficient of thermal expansion is 7.5 × 10-6/K。
Embodiment 4：
The preparation method of the present embodiment high heat-conductive diamond/Cu-base composites carries out according to the following steps：
Step 1：It weighs surface and is coated with the diamond original powder of film plating layer and be fitted into molding die and carry out jolt ramming processing,
Make precast body；Precast body is positioned in crucible, blocky copper alloy is positioned over precast body top in crucible, crucible is placed
In gas pressure infiltration stove；
Molding die is placed on supersonic oscillations plate during the jolt ramming processing, is vibrated 10 minutes under the frequency of 28kHz；
The material of the film plating layer is Mo；
The thickness 100nm of the film plating layer；
The surface is coated with a diameter of 100 μm of the diamond original powder of film plating layer；
The material of the molding die is high purity graphite；
The material of the crucible is high purity graphite；
Treated that the mass ratio of diamond original powder that surface is coated with film plating layer is for bulk copper alloy and the jolt ramming
0.85：1；
The chromiumcopper that the material of the bulk copper alloy is 0.5~1.1wt.% containing chromium；
Step 2：It is 1Pa by gas pressure infiltration stove evacuation to vacuum degree；
Step 3：Gas pressure infiltration stove is warming up to more than blocky fine copper or blocky copper alloy fusing point under inert gas shielding
1300 DEG C and keep the temperature 1h；The inert gas pressure is 0.1MPa；
Step 4：Inert gas and pressurize are passed through into gas pressure infiltration stove, pressurize terminates postcooling, release and demoulding, i.e.,
It completes；
The air pressure of the inert gas is 1MPa；The time of the pressurize is 10min；The cooling velocity is 3 DEG C/min；
High heat-conductive diamond/carbon/carbon-copper composite material component prepared by embodiment 4 is square sheets shape, and thickness 1.0mm is square
Length of side 100mm；The volume fraction 65% of diamond reinforcement, composite density 5.39g/cm in composite material3, thermal diffusion
Coefficient is 182.239/mm2, thermal conductivity 430W/mK, coefficient of thermal expansion is 9.8 × 10-6/K；
Embodiment 5：
The preparation method of the present embodiment high heat-conductive diamond/Cu-base composites carries out according to the following steps：
Step 1：It weighs diamond original powder to be fitted into molding die and carry out jolt ramming processing, makes precast body；By precast body
It is positioned in crucible, blocky copper alloy is positioned over precast body top in crucible, crucible is positioned in gas pressure infiltration stove；
Molding die is placed on supersonic oscillations plate during the jolt ramming processing, is vibrated 10 minutes under the frequency of 28kHz；
A diameter of 100 μm of the diamond original powder；
The material of the molding die is high purity graphite；
The material of the crucible is high purity graphite；
Treated that the mass ratio of diamond original powder that surface is coated with film plating layer is for bulk copper alloy and the jolt ramming
1.09：1；
The chromiumcopper that the material of the bulk copper alloy is 0.5~1.1wt.% containing chromium；
Step 2：It is 1Pa by gas pressure infiltration stove evacuation to vacuum degree；
Step 3：Gas pressure infiltration stove is warming up to more than blocky fine copper or blocky copper alloy fusing point under inert gas shielding
1300 DEG C and keep the temperature 1h；The inert gas pressure is 0.1MPa；
Step 4：Inert gas and pressurize are passed through into gas pressure infiltration stove, pressurize terminates postcooling, release and demoulding, i.e.,
It completes；
The air pressure of the inert gas is 1MPa；The time of the pressurize is 10min；The cooling velocity is 3 DEG C/min；
High heat-conductive diamond/carbon/carbon-copper composite material component prepared by embodiment 5 is square sheets shape, and thickness 1.0mm is square
Length of side 100mm；The volume fraction 65% of diamond reinforcement, composite density 5.39g/cm in composite material3, thermal diffusion
Coefficient is 218.492/mm2, thermal conductivity 515W/mK, coefficient of thermal expansion is 7.2 × 10-6/K；Fig. 9 is prepared by embodiment 5
The interface topography figure of high heat-conductive diamond/carbon/carbon-copper composite material, 1 is chromium carbide in figure.
Claims (10)
1. a kind of preparation method of high heat-conductive diamond/carbon/carbon-copper composite material, it is characterised in that：This method carries out according to the following steps：
Step 1：It weighs surface and is coated with the diamond original powder of film plating layer and be fitted into molding die and carry out jolt ramming processing, make
Precast body；Precast body is positioned in crucible, blocky fine copper or blocky copper alloy are positioned over precast body top in crucible, by earthenware
Crucible is positioned in gas pressure infiltration stove；
Or diamond original powder is taken to be fitted into molding die and carries out jolt ramming processing, make precast body；Precast body is positioned over earthenware
In crucible, blocky copper alloy is positioned over precast body top in crucible, crucible is positioned in gas pressure infiltration stove；
The material of the molding die is high purity graphite or isostatic pressing formed graphite；
The material of the crucible is high purity graphite or isostatic pressing formed graphite；
Step 2：It is 0.1~1Pa by gas pressure infiltration stove evacuation to vacuum degree；
Step 3：Gas pressure infiltration stove is warming up to more than blocky fine copper or blocky copper alloy fusing point 100 under inert gas shielding
~250 DEG C and keep the temperature 1h~3h；
The inert gas pressure is 0.1~1MPa；
Step 4：Inert gas and pressurize are passed through into gas pressure infiltration stove, pressurize terminates postcooling, release and demoulding, that is, completes；
The air pressure of the inert gas is 1~10MPa；
The time of the pressurize is 10min~3h.
2. the preparation method of high heat-conductive diamond/carbon/carbon-copper composite material according to claim 1, it is characterised in that：Step 1
Treated that the mass ratio of diamond original powder that surface is coated with film plating layer is for the bulk fine copper or blocky copper alloy and jolt ramming
(0.85~2.07)：1.
3. the preparation method of high heat-conductive diamond/carbon/carbon-copper composite material according to claim 1 or 2, it is characterised in that：Step
The mass ratio of the one blocky copper alloy and jolt ramming treated diamond original powder is (0.85~2.07)：1.
4. the preparation method of high heat-conductive diamond/carbon/carbon-copper composite material according to claim 3, it is characterised in that：Step 1
Molding die is placed on supersonic oscillations plate during the jolt ramming processing, is vibrated 5~15 minutes under the frequency of 20~30kHz.
5. the preparation method of high heat-conductive diamond/carbon/carbon-copper composite material according to claim 1,2 or 4, it is characterised in that：Step
A rapid bortz powder original powder or surface are coated with a diameter of 50~400 μm of the diamond original powder of film plating layer.
6. the preparation method of high heat-conductive diamond/carbon/carbon-copper composite material according to claim 1, it is characterised in that：Step 1
The material of the bulk copper alloy is copper zirconium alloy, chromiumcopper, copper-titanium alloy or Cu-B alloy.
7. the preparation method of high heat-conductive diamond/carbon/carbon-copper composite material according to claim 1, it is characterised in that：Step 1
The material of the film plating layer is W, Cr, Mo or Ti.
8. the preparation method of high heat-conductive diamond/carbon/carbon-copper composite material according to claim 1, it is characterised in that：Step 1
50~5000nm of thickness of the film plating layer.
9. the preparation method of high heat-conductive diamond/carbon/carbon-copper composite material according to claim 1, it is characterised in that：Step 3
It is described that gas pressure infiltration stove is warming up to more than blocky fine copper or blocky copper alloy fusing point 250 DEG C under inert gas shielding and is kept the temperature
2h。
10. the preparation method of high heat-conductive diamond/carbon/carbon-copper composite material according to claim 1, it is characterised in that：Step 4
The cooling velocity is 3~5 DEG C/min.
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