CN104264000B - The high thermal conductivity aluminum matrix composite of Graphene modification and method for preparing powder metallurgy thereof - Google Patents
The high thermal conductivity aluminum matrix composite of Graphene modification and method for preparing powder metallurgy thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
Abstract
The invention provides the modified high thermal conductivity aluminum matrix composite of a kind of Graphene and method for preparing powder metallurgy thereof, described material includes reinforcement particle and aluminum substrate, and reinforcement particle and the compound interface of aluminum substrate contain high thermal conductivity graphene nanometer sheet.Described method includes: reinforcement particle strong acid solution is soaked by (1), then cleans to neutral, drying by deionized water, removes surface impurity, obtain the reinforcement particle of activation process；(2) the reinforcement particle of activation process is joined in graphene dispersing solution, by mechanical agitation or ultrasonic disperse, at its Surface coating graphene nanometer sheet, prepare the reinforcement particle that Graphene is modified；(3) the reinforcement particle that Graphene is modified is mixed with aluminum substrate powder, by pressed compact and sintering, prepare the high thermal conductivity aluminum matrix composite that Graphene is modified.Composite chemical stability prepared by the present invention is good, and thermal conductivity is high, can be used as the thermal management materials of high power semi-conductor components and parts.
Description
Technical field
The present invention relates to metal-base composites technical field, use Graphene to reinforcement in particular it relates to a kind of
Grain carries out surface modification, and then uses the method that PM technique prepares high thermal conductivity aluminum matrix composite again.
Background technology
In recent years, for adapting to the growth requirement of electronic technology, high heat conduction, low bulk Metal Substrate as thermal management materials are multiple
The research of condensation material achieves huge progress.Particle enhanced aluminum-based composite material is light owing to having aluminum substrate and reinforcement particle
Matter, highly thermally conductive, the overall merit of low bulk, become the ideal chose of future electronic encapsulating material.But, select at present
Reinforcement particle be mainly carbon family or the highly heat-conductive material Han carbons, such as: carborundum, diamond, exfoliated graphite particles etc.,
These particles and aluminum substrate poor compatibility, thus Material cladding interface prepared by low temperature cannot form effectively combination, material is combined
Close poor performance, cannot apply；And when at high temperature processing, particle again easily and aluminium generation interfacial reaction, generates bar-shaped or sheet
Shape Al4C3Phase.On the one hand, due to Al4C3Thermal conductivity is low, and the generation of this product phase can significantly reduce the heat of composite
Conductance；On the other hand, Al4C3Poor chemical stability, easily there is chemical reaction when meeting acid, alkali, water even alcohols and
Decompose, cause aluminum matrix composite chemical stability to reduce；Additionally, Al4C3Fragility is big, and it is once formed in interface
Continuous film, easily causes compound interface cracking to cause material failure.Owing to there are the problems referred to above, high thermal conductivity aluminum matrix is combined
Material is severely limited in the popularization and application of field of heat management.Therefore, the boundary that particle is good with aluminum substrate can be realized
Face combines, and can suppress again Al simultaneously4C3The generation of phase, is the key preparing high heat conduction particle reinforced aluminum matrix composites.
Particle is carried out surface process, such as: coating surface, is the main Research Thinking solving this problem.
Literature search to prior art finds, at particle surface plating W (or its carbide), Ti (or its carbide)
It is to improve compound interface to combine, suppress Al4C3The technical way generated mutually.Document 1 " Enhanced thermal
Conductivity in diamond/aluminum composites with a tungsten interface nanolayer " (pass through W
Nano-coating improves the heat conductivility of diamond/aluminum composite) (Materials and Design 47 (2013) 160-166)
Combine by improving diamond/aluminum compound interface at the W nano-deposit that diamond surface plating thickness is 100-400nm, press down
Al processed4C3Generate mutually, its diamond volume content prepared be 40% heat conductivity can be carried by 496W/mK
High to 599W/mK；Document 2 " Thermal conductivity and microstructure of Al/diamond composites
With Ti-coated diamond particles consolidated by spark plasma sintering " (plasma sintering plates
The thermal conductivity of Ti diamond/aluminum composite and microstructure) (Journal of Composite Materials 46 (2012)
1127-1136) by the Ti metal level that diamond particle surfaces plated thickness is 0.5 μm, improving the boundary of diamond and aluminium
Face combines, and the heat conductivity making diamond volume content be 40% is brought up to 433W/mK by 325W/mK.So
And, document 3 " A predictive model for interfacial thermal conductance in surface metallized
Diamond aluminum matrix composites " (the interface thermal conductance prediction mould of surface metalation diamond/aluminum composite
Type) (Materials and Design 55 (2014) 257-262) " thickness of coating is to Ti-coated diamond/aluminium composite wood with document 4
The impact of material thermal conductivity " (China YouSe Acta Metallurgica Sinica, 23 (2013) 802-808) card in terms of theory and test two the most respectively
Real: particle surface plating W, the Ti such as heat conductivity increases with interface thickness of coating and drastically declines, diamond
Though can improve interface cohesion and the thermal conductivity of composite Deng more non-plating particle, but it still differs relatively big with theoretical value, its
The subject matter existed is: (1) compared with reinforced particulate, aluminum substrate, the thermal conductivity of boundary layer the lowest (as W,
Ti is respectively 178W/mK and 21.9W/mK)；(2) thickness of coating is too big (generally greater than 100nm), because of coating
The composite material interface thermal resistance introduced and increase is relatively big, causes heat conductivity and theoretical value at a distance of the biggest；(3)
The thickness of particle surface coating and the more difficult control of uniformity, interface modification effect is undesirable.
Summary of the invention
For defect of the prior art, it is an object of the invention to provide the modified high thermal conductivity aluminum matrix of a kind of Graphene and be combined
Material and method for preparing powder metallurgy thereof, can obtain that thermal conductivity is higher, chemical stability more preferably, without interfacial reaction phase
High heat conduction particle reinforced aluminum matrix composites, it is simple to it is in the popularization and application of field of heat management.
For realizing object above, the present invention by the following technical solutions:
The present invention provides the high thermal conductivity aluminum matrix composite that a kind of Graphene is modified, and described composite includes reinforcement particle
With aluminum substrate, described reinforcement particle and the compound interface of aluminum substrate contain high thermal conductivity graphene nanometer sheet.
Preferably, the described highly heat-conductive material that reinforcement particle is carborundum, diamond, exfoliated graphite particles.
Preferably, the equivalent grain size of described reinforcement particle is 20-600 μm.
Preferably, described reinforcement particle volume content in whole described composite is 20-65%.The most excellent
Choosing, the volume content of described reinforcement particle is 40-60%.
Preferably, described graphene nanometer sheet is single or multiple lift Graphene.
Preferably, the thickness of described graphene nanometer sheet is 0.3-20nm.
Preferably, the sheet footpath of described graphene nanometer sheet is 0.3-20 μm.
Preferably, described aluminum substrate is fine aluminium or its alloy.
The present invention provides the method for preparing powder metallurgy of the high thermal conductivity aluminum matrix composite of a kind of Graphene modification, described side
Method uses graphene nanometer sheet that high heat conduction particle is carried out surface modification cladding, it is thus achieved that Graphene modified particles, by Graphene
Modified particles is compound with aluminum substrate obtains high thermal conductivity graphene modified particles reinforced aluminum matrix composites；
Described method comprises the steps:
(1) reinforcement particle strong acid solution is soaked, then clean to neutral, drying by deionized water, remove table
Face impurity, obtains the reinforcement particle of activation process；
(2) the reinforcement particle of activation process is joined in graphene dispersing solution, by mechanical agitation or ultrasonic disperse,
In reinforcement particle surface coated graphite alkene nanometer sheet, prepare the reinforcement particle that Graphene is modified；
(3) the reinforcement particle that Graphene is modified is mixed with aluminum substrate powder, by pressed compact and sintering, prepare graphite
The high thermal conductivity aluminum matrix composite that alkene is modified.
Preferably, described aluminum substrate is fine aluminium or its alloy, and the equivalent grain size of initial described aluminum substrate powder is
20-600μm。
The principle of the present invention:
The reinforcement particle of highly heat-conductive material is after strong acid activating processes, and particle surface impurity is removed and generates one
The active points of determined number；And use mechanical agitation or ultrasonic disperse, water or ethanol medium add appropriate surface and changes
After property agent, graphene nanometer sheet can be changed into homodisperse metastable state, graphene nanometer sheet and decentralized medium by reunion state
Form metastable state dispersion liquid；Graphene nanometer sheet in metastable state dispersion liquid has higher unstability trend, with activation process
After reinforcement particle mixing after, be aided with mechanical agitation or sonic oscillation, metastable state is destroyed, and the surface added changes
Property agent can suppress graphene nanometer sheet reunion each other, after promoting graphene nanometer sheet unstability, being attached to activation process
Reinforcement particle surface, and by particle surface active site adsorb pinning, graphene nanometer sheet is firmly attached to by force
Acid activation particle surface, i.e. prepares the reinforcement particle that Graphene is modified.The special laminated structure of graphene nanometer sheet with
Nano-scale, is aided with the surface modifier inhibitory action to again reuniting between it, makes graphene nanometer sheet be prone at particle
Dispersion on surface is uniform, thickness is homogeneous；By the thickness of graphene nanometer sheet used by adjusting and surface modifier kind,
The number of processes etc. of Graphene modified particles, can the thickness of flexible modulation particle surface coated graphite alkene nanometer sheet.Use pressure
Base and sintering method, by Graphene modified particles and fine aluminium or aluminium alloy compound, can prepare high thermal conductivity graphene modified
High heat conduction particle reinforced aluminum matrix composites.At high temperature there is high chemical stability due to Graphene, in routine
It is difficult to and metallic aluminium generation chemical reaction under the conditions of technology of preparing, introduces a layer graphene nanometer sheet at diamond surface, can
Avoid high heat conduction particle to contact with the direct of aluminium, thus avoid the interfacial reaction of itself and aluminum substrate；Simultaneously because Graphene tool
Have a high thermal conductivity (3000-5200W/mK), therefore be not introduced into Graphene or use the particle of conventional metals plated film
Reinforced aluminum matrix composites is compared, and the introducing of Graphene can significantly reduce compound interface thermal resistance, improves heat conductivity.
Compared with prior art, the present invention has a following beneficial effect:
(1) the reinforcement particle that Graphene is modified both can avoid the reaction of itself and aluminium, can reduce again compound interface thermal resistance,
Composite is made to have higher thermal conductivity；
(2) Graphene is special laminated structure and nano-scale so that it is be prone to and absorption dispersed at particle surface,
Thickness and the uniformity of Graphene easily regulate and control.
Accompanying drawing explanation
The detailed description made non-limiting example with reference to the following drawings by reading, other of the present invention is special
Levy, purpose and advantage will become more apparent upon:
Fig. 1 is the preparation technology flow chart of the embodiment of the present invention.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.Following example will assist in those skilled in the art
Member is further appreciated by the present invention, but limits the present invention the most in any form.It should be pointed out that, the common skill to this area
For art personnel, without departing from the inventive concept of the premise, it is also possible to make some deformation and improvement.These broadly fall into
Protection scope of the present invention.
The high thermal conductivity aluminum matrix composite of the present invention a kind of Graphene presented below modification and method for preparing powder metallurgy thereof,
The method uses graphene nanometer sheet that high heat conduction particle is carried out surface modification cladding, it is thus achieved that Graphene modified particles, by stone
Ink alkene modified particles is combined with aluminum substrate and obtains the aluminum matrix composite that high thermal conductivity graphene is modified.Owing to Graphene chemistry is steady
Qualitative height, thickness are little, thermal conductivity is high, can effectively prevent high enhanced thermal conduction body particle (such as carborundum, diamond, sheet
Graphite granule etc.) and aluminum substrate generation chemical reaction, it is to avoid generate Al4C3Deng deleterious interfacial product, it is ensured that strengthen
There is between body particle and aluminum substrate high interface thermal conductance.So, the composite chemical stability of preparation is good, and thermal conductivity is high,
Can be used as the thermal management materials of high power semi-conductor components and parts.
In following example, the concentration of the described graphene dispersing solution of employing is 5.0mg/ml, Graphene, reinforcement
The detail parameters of particle and aluminum substrate is as shown in table 1.Pressed compact can use the prior aries such as mold pressing, isostatic pressed at 50-400MPa
Under pressure suppress, sintering can use vacuum-sintering, vacuum pressure sintering, protective atmosphere sintering, gas pressure sintering, etc.
The prior aries such as gas ions sintering, microwave sintering are at a temperature of 450-650 DEG C or load 30-300MPa axial compressive force simultaneously
Carrying out, the sample size of preparation is Ф 12.7 × 3.0mm, tests for thermal conductivity.The room temperature thermal conductivity (TC) of material
Calculated, wherein by formula λ=α × ρ × c: α is room temperature thermal diffusion coefficient, use Germany Nai Chi company LFA447
Equipment is recorded by the laser method of shining；ρ is the density of material, uses Archimedes's drainage to record；C is composite
Specific heat capacity.The thermal conductivity be given in embodiment is room temperature test result.What table 1 was given is the technique in each embodiment
Parameter and final material property.
Technological parameter in each embodiment of table 1 and material conducts heat performance
As it is shown in figure 1, method described in the present embodiment specifically includes following steps:
(1) reinforcement particle strong acid solution is soaked, then clean to neutral, drying by deionized water, remove table
Face impurity, obtains the reinforcement particle of activation process；
(2) the reinforcement particle of activation process is joined in graphene dispersing solution, by mechanical agitation or ultrasonic disperse,
In reinforcement particle surface coated graphite alkene nanometer sheet, prepare the reinforcement particle that Graphene is modified；
(3) the reinforcement particle that Graphene is modified is mixed with aluminum substrate powder, by pressed compact and sintering, prepare graphite
The high thermal conductivity aluminum matrix composite that alkene is modified.
The present invention is elaborated by below embodiment:
Embodiment 1
The diamond strong acid that granularity is 20 μm is soaked, cleans to neutrality, drying with pure water, insert Graphene
Dispersion liquid stirs 2.0 hours, fully rinses with water after leaching, it is thus achieved that Graphene modification diamond particles；By 20% body
The Graphene modification diamond particles of fraction mixes with the fine aluminium powder that purity is 99.9%, pressed compact, 630 DEG C of sintering 2
Hour preparation Graphene modification diamond reinforced aluminum matrix composites consistency be 99.2%, thermal conductivity is 335W/mK.
Embodiment 2
The diamond strong acid that granularity is 600 μm is soaked, cleans to neutrality, drying with pure water, insert graphite
Alkene dispersion liquid stirs 2.0 hours, fully rinses with water after leaching, it is thus achieved that Graphene modification diamond particles；By 65%
The Graphene modification diamond particles of volume fraction mixes with the fine aluminium that purity is 99.9%, pressed compact, and 645 DEG C of sintering 2 are little
Time the Graphene modification diamond reinforced aluminum matrix composites consistency prepared be 98.9%, thermal conductivity is 846W/mK.
Embodiment 3
The carborundum strong acid that granularity is 300 μm is soaked, cleans to neutrality, drying with pure water, insert graphite
Alkene dispersion liquid stirs 2.0 hours, fully rinses with water after leaching, it is thus achieved that Graphene carbon modified silicon carbide particle；By 45%
The Graphene carbon modified silicon carbide particle of volume fraction mixes with Al-7%Si Al alloy powder, pressed compact, and 615 DEG C of sintering 2 are little
Time the Graphene modification enhancing aluminum-base composite material by silicon carbide particles consistency prepared be 98.6%, thermal conductivity is 237
W/mK。
Embodiment 4
The graphite granule strong acid that granularity is 200 μm is soaked, cleans to neutrality, drying with pure water, insert stone
Ink alkene dispersion liquid stirs 2.0 hours, fully rinses with water after leaching, it is thus achieved that Graphene modified graphite particle；By 50%
The Graphene modified graphite particle of volume fraction mixes with Al-7%Si Al alloy powder, pressed compact, and 630 DEG C sinter 2 hours
The Graphene modified graphite particle reinforced aluminum matrix composites consistency of preparation is 99.0%, and thermal conductivity is 530W/mK.
Comparing embodiment 1
The diamond strong acid that granularity is 20 μm is soaked, cleans to neutrality, drying, by 20% volume with pure water
The diamond particles of mark mixes with the fine aluminium powder that purity is 99.9%, pressed compact, the stone of 630 DEG C of sintering preparation in 2 hours
Ink alkene modification diamond particles reinforced aluminum matrix composites consistency is 99.2%, and thermal conductivity is 283W/mK.
Comparing embodiment 2
The diamond strong acid that granularity is 600 μm is soaked, cleans to neutrality, drying with pure water, use vacuum
Hydatogenesis is deposited with 40 minutes at 750 DEG C, it is thus achieved that coating film thickness is the plated surface Ti diamond of 0.3 μm；By 65% body
The plated surface Ti diamond of fraction mixes with the fine aluminium that purity is 99.9%, pressed compact, the preparation in 2 hours of 645 DEG C of sintering
Diamond/aluminum composite consistency is 98.8%, and thermal conductivity is 598W/mK.
Comparing embodiment, compared with the present invention, processes, in phase owing to not carrying out effective Interface Control or interface modification
With under material component and preparation process condition, in comparing embodiment, the interface resistance of material is high, thermal conductivity is relatively low, typically than
The low 15-30% of high thermal conductivity aluminum matrix composite thermal conductivity prepared by the present invention.
To sum up, the present invention prepares Graphene modified particles by being coated with high thermal conductivity graphene at particle surface, and then prepares stone
The high thermal conductivity aluminum matrix composite that ink alkene is modified, the reinforcement particle in described aluminum matrix composite and the compound boundary of aluminum substrate
Containing high thermal conductivity graphene nanometer sheet on face.Graphene not only has high chemical stability, in conventional formulation techniques condition
It is difficult to and aluminum substrate generation chemical reaction down, has than the enhanced thermal conduction higher thermal conductivity of body particle simultaneously
(3000-5200W/mK), and its thickness in monolayer is only 0.34nm, even if number thickness stacked together is also only several
Nanometer.Compared with traditional particle surface metal coating (thickness is more than 100nm), stable chemical property makes graphite
Alkene nanometer sheet can protect enhanced thermal conduction body particle not with aluminum substrate generation chemical reaction, high heat conduction makes it will not be at composite
The interface resistance that middle introducing is extra, Graphene laminated structure makes it be easily spread at particle surface, is coated with simultaneously, Graphene
Thickness and the uniformity of nanometer sheet are easily controllable.Thus, the technical program can obtain that thermal conductivity is higher, chemical stability more
Well, the high heat conduction particle reinforced aluminum matrix composites without interfacial reaction phase, it is simple to it is in the popularization and application of field of heat management.
Above the specific embodiment of the present invention is described.It is to be appreciated that the invention is not limited in
Stating particular implementation, those skilled in the art can make various deformation or amendment within the scope of the claims,
This has no effect on the flesh and blood of the present invention.
Claims (9)
1. the high thermal conductivity aluminum matrix composite that a Graphene is modified, it is characterised in that described composite includes reinforcement
Particle and aluminum substrate, described reinforcement particle and the compound interface of aluminum substrate contain high thermal conductivity graphene nanometer sheet；
The described highly heat-conductive material that reinforcement particle is carborundum, diamond, exfoliated graphite particles.
The high thermal conductivity aluminum matrix composite that Graphene the most according to claim 1 is modified, it is characterised in that described increasing
The equivalent grain size of strong body particle is 20-600 μm.
The high thermal conductivity aluminum matrix composite that Graphene the most according to claim 1 is modified, it is characterised in that described increasing
Strong body particle volume content in whole described composite is 20-65%.
The high thermal conductivity aluminum matrix composite that Graphene the most according to claim 3 is modified, it is characterised in that described increasing
The volume content of strong body particle is 40-60%.
5., according to the high thermal conductivity aluminum matrix composite that the Graphene described in any one of claim 1-4 is modified, its feature exists
It is single or multiple lift Graphene in described graphene nanometer sheet.
The high thermal conductivity aluminum matrix composite that Graphene the most according to claim 5 is modified, it is characterised in that described stone
The thickness of ink alkene nanometer sheet is 0.3-20nm.
The high thermal conductivity aluminum matrix composite that Graphene the most according to claim 5 is modified, it is characterised in that described stone
The sheet footpath of ink alkene nanometer sheet is 0.3-20 μm.
8. the powder metallurgy system of the high thermal conductivity aluminum matrix composite that Graphene described in an any one of claim 1-7 is modified
Preparation Method, it is characterised in that described method comprises the steps:
(1) reinforcement particle strong acid solution is soaked, then clean to neutral, drying by deionized water, remove table
Face impurity, obtains the reinforcement particle of activation process；
(2) the reinforcement particle of activation process is joined in graphene dispersing solution, by mechanical agitation or ultrasonic disperse,
In reinforcement particle surface coated graphite alkene nanometer sheet, prepare the reinforcement particle that Graphene is modified；
(3) the reinforcement particle that Graphene is modified is mixed with aluminum substrate powder, by pressed compact and sintering, prepare graphite
The high thermal conductivity aluminum matrix composite that alkene is modified.
Prepared by the powder metallurgy of the high thermal conductivity aluminum matrix composite that a kind of Graphene the most according to claim 8 is modified
Method, it is characterised in that described aluminum substrate is fine aluminium or its alloy, the equivalent grain size of initial described aluminum substrate powder is
20-600μm。
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| CN103789564A (en) * | 2014-01-23 | 2014-05-14 | 上海交通大学 | Powder metallurgy preparation method of carbon nanotube reinforced aluminum alloy composite material |
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