CN105755307B - A kind of alveolate texture enhancing composite and preparation method - Google Patents
A kind of alveolate texture enhancing composite and preparation method Download PDFInfo
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- CN105755307B CN105755307B CN201610161186.8A CN201610161186A CN105755307B CN 105755307 B CN105755307 B CN 105755307B CN 201610161186 A CN201610161186 A CN 201610161186A CN 105755307 B CN105755307 B CN 105755307B
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Abstract
A kind of alveolate texture enhancing composite and preparation method, the composite is made up of cellular backing material, high heat conduction film layer, matrix material and high heat conduction particle, cellular backing material is metal, highly heat-conductive material can be diamond, graphene, the single substance in CNT or a variety of compound, and matrix material is high-thermal conductive metal material or polymeric material.Composite of the present invention is upwardly formed continuous quick conductive passage along alveolate texture side, and axially has preferably orientation heat conductivility along honeycomb, can realize to a certain extent higher to hot differentiated control, stock utilization.In addition, honeycomb has the characteristics of strong designability, steady quality, high-strength light, can meet the needs of fields such as space flight and aviation, ship, communications and transportation are to high performance light heat exchanging material.Suitable for industrial applications.
Description
Technical field
The invention discloses a kind of alveolate texture enhancing composite and preparation method, belong to composite technology of preparing
Field.
Background technology：
Modern science and technology is maked rapid progress, and let us enjoys while convenience of its achievement institute band, is also the work band of scientific research
Increasing challenge is carried out.With the fast development of electronics and information industry, variation, superelevation is integrated, is miniaturized, opposite sex chemical conversion
The development course of electronic device.When the river rises the boat goes up for requirement nature to encapsulating material, and all kinds of Heat Conduction Materials are also come out one after another.From base
Body divides, and has Metal Substrate, ceramic base, polymer matrix etc.；Divide from reinforcement, there is diamond, graphene, CNT etc.；From
The structure of reinforcement is divided, and has zero dimension graininess, one dimension fibre or wire, two-dimensional slice shape, three-dimensional network shape and a special construction
Deng.Patent CN105239026A proposes a kind of one-dimensional diamond reinforced aluminum matrix composites and preparation method thereof patent, in aluminium
Be distributed the diamond array that is made up of some one-dimensional diamond wires in matrix, one-dimensional diamond wire be surface modified diamond line simultaneously
With aluminum substrate metallurgical binding；Heat transfer efficiency is further lifted by adding diamond particles formation connection in series-parallel composite heat-conducting structure.
Patent CN105220049A proposes a kind of sheet diamond reinforced metal-base composite material and preparation method, in parent metal
Diamond wafers are provided with, diamond wafers and parent metal are metallurgical binding；Patent CN105112754A proposes one kind three
Network diamond framework enhancing Cu-base composites and preparation method are tieed up, composite is by metallic matrix (Al, Cu, Ag), three-dimensional
Network diamond framework and diamond particles composition, make the composite wood by being distributed three-dimensional network diamond framework in metallic matrix
Material is respectively provided with excellent heat conductivility along three dimensional diamond skeleton direction, and compound by adding diamond particles formation connection in series-parallel
Conductive structure further lifts heat transfer efficiency.
Compared with above-mentioned composite configuration, hexagonal honeycomb can be described as a big miracle of nature.Its structure is than any circle
Shape or the structure of square are stronger, can undertake the external force from each side.The exactly so special structure of honeycomb, the mankind are therefrom
Inspired, even if most slim material, as long as it is made honeycomb shape, very big external force can be born, and it is not variable
Shape, this not only reduces the consumption of raw material, and it can also beautify the environment.The characteristics of cellular structural material high-strength light, use
In aerospace field, it is the special requirement for answering Aero-Space science and technology and the composite of a kind of microlight-type that grows up,
Rarely has the report at highly thermally conductive aspect.
The content of the invention
It is an object of the invention to overcome the deficiency of prior art, there is provided one kind is upwardly formed continuously along alveolate texture side
Quick conductive passage, and the alveolate texture for axially having preferably orientation heat conductivility along honeycomb strengthens composite and system
Preparation Method, composite prepared by the present invention can be realized higher to hot differentiated control, stock utilization to a certain extent.
A kind of alveolate texture enhancing composite of the present invention, described composite include cellular reinforcement and matrix
Material, described matrix material are high-thermal conductive metal or polymer；The cellular reinforcement is coated with cellular substrate
Highly heat-conductive material, described highly heat-conductive material be selected from diamond film, graphene film, carbon nano-tube film, diamond/graphene film,
Kind in diamond/carbon nanotube films, graphene/carbon nano-tube film, diamond/graphene/carbon nano-tube film.
A kind of alveolate texture enhancing composite of the present invention, when described matrix material is high-thermal conductive metal, matrix material
One kind in metallic copper, aluminium, silver, copper alloy, aluminium alloy, silver alloy, copper in the copper alloy, aluminium alloy, silver alloy,
Aluminium, the weight/mass percentage composition of silver are more than or equal to 50%；Polymeric matrix is thermoplastic polymer or thermosetting polymer；The heat
Thermoplastic polymer is selected from polyethylene, polypropylene, polystyrene, polyvinyl chloride, polytetrafluoroethylene (PTFE), nylon, makrolon, poly- methyl
One kind in methyl acrylate, glycol ester, poly terephthalic acid, polyformaldehyde, polyamide, polysulfones；The thermosetting polymer
Selected from epoxy resin, phenolic resin, Lauxite, amino resins, melmac, unsaturated polyester resin, organosilicon tree
One kind in fat, silicon rubber, expanded polystyrene (EPS), polyurethane.
A kind of alveolate texture of the present invention strengthens composite, also contains high heat conduction particle in composite, the height is led
Hot particle is selected from diamond particles, CNT, Graphene powder, graphene coated diamond particles, CNT cladding Buddha's warrior attendant
At least one of stone particle.
A kind of present invention alveolate texture enhancing composite, in composite, the volume fraction of cellular reinforcement is
5-70%, matrix material volume fraction are 30-95%, and high heat conduction grain volume fraction is 0-50%, each component volume basis it
With for 100%.
A kind of present invention alveolate texture enhancing composite, cellular backing material be selected from metallic copper, titanium, tungsten, molybdenum,
One kind in one kind or acid bronze alloy, titanium-base alloy, molybdenum-base alloy in chromium, nickel, the acid bronze alloy, titanium-base alloy, molybdenum base
Copper, titanium, the weight/mass percentage composition of molybdenum are more than or equal to 50% in alloy.
A kind of alveolate texture of the present invention strengthens composite, and at least one cellular reinforcement is included in composite；
Or
Include multiple cellular reinforcements in composite, cellular reinforcement is sheet or strip, described strip or
The cellular reinforcement of sheet is compound with matrix material in the form of an array；Or described strip or the cellular reinforcement alternating heap of sheet
It is folded compound with matrix material；Cellular reinforcement in composite is identical or different.
The present invention a kind of alveolate texture enhancing composite, in cellular reinforcement, by the honeycomb that section is hexagon
Or rectangle honeycomb is arranged in order composition, the thickness of cellular reinforcement is 0.01~10mm, 0.01~5mm of pore wall thickness.
A kind of preparation method of alveolate texture enhancing composite of the present invention, comprises the steps：
The first step：Prepare cellular reinforcement
By the cleaning of alveolate texture substrate, drying；Highly heat-conductive material is deposited in diamond surface using chemical vapor deposition；
Highly heat-conductive material graphite, diamond, graphene, the deposition process parameters of CNT are：
Graphene CVD deposition parameter is：It is 0.5-80% that carbonaceous gas, which accounts for all gas mass flow percentage in stove,；It is raw
Long temperature is 400-1200 DEG C, and growth air pressure is 5-105Pa；
CNT CVD deposition parameter is：It is 5-50% that carbonaceous gas, which accounts for all gas mass flow percentage in stove,；It is raw
Long temperature is 400-1300 DEG C, and growth air pressure is 103-105Pa；
Diamond CVD deposition parameter is：It is 0.5-10% that carbonaceous gas, which accounts for all gas mass flow percentage in stove,；It is raw
Long temperature is 600-1000 DEG C, and growth air pressure is 103-104Pa；
By to applying plasma and induced by magnetic field, and regulation carbon throughput, growth temperature, life in real time in CVD deposition stove
Long air pressure, realize highly heat-conductive material diamond/graphene, diamond/carbon nanotube, diamond/graphene/carbon nano-tube film
CVD deposition, deposition parameter are：
Graphene CVD deposition parameter is：It is 0.5-80% that carbonaceous gas, which accounts for all gas mass flow percentage in stove,；It is raw
Long temperature is 400-1200 DEG C, and growth air pressure is 5-105Pa；Plasma electric current density 0-50mA/cm2；Magnetic field is strong in deposition region
Spend for 100 Gausses to 30 teslas；
CNT CVD deposition parameter is：It is 5-50% that carbonaceous gas, which accounts for all gas mass flow percentage in stove,；It is raw
Long temperature is 400-1300 DEG C, and growth air pressure is 103-105Pa；Plasma electric current density 0-30mA/cm2；Magnetic field in deposition region
Intensity is 100 Gausses to 30 teslas；
Diamond CVD deposition parameter is：It is 0.5-10% that carbonaceous gas, which accounts for all gas mass flow percentage in stove,；It is raw
Long temperature is 600-1000 DEG C, grows air pressure 103-104Pa；
Highly heat-conductive material thickness is 0.34nm-1mm；
Second step：Cellular reinforcement and matrix progress is compound, obtain alveolate texture enhancing Metal Substrate or polymer
Based composites；
Cellular reinforcement and metallic matrix compound tense, use is cold-rolled sintered, hot pressed sintering, plasma agglomeration, molten without pressure
Ooze, pressure infiltration, a kind of technology in casting carry out it is compound；
Cellular reinforcement and polymeric matrix compound tense, using dipping curing molding, injection moulding, compressing, rolling
A kind of technology being moulded into type, injection molding, extrusion moulding, laminated into type, flow casting molding carries out compound.
The preparation method of the present invention a kind of alveolate texture enhancing composite, in the first step, by alveolate texture substrate
After cleaning, drying；First using one kind in plating, chemical plating, evaporation, magnetron sputtering, chemical vapor deposition, physical vapour deposition (PVD)
After the one kind or complex metal layer of method in substrate surface deposition nickel, copper, tungsten, molybdenum, titanium, silver, chromium, then using chemical vapor deposition
Product highly heat-conductive material；Metal layer thickness is 1nm-2 μm.
A kind of preparation method of alveolate texture enhancing composite of the present invention, alveolate texture substrate surface prepare metal
After layer, first it is soaked in nano-diamond powder or Graphene powder or carbon nanotube suspension and carries out ultrasonic vibration plantation seed crystal, so
Afterwards, using chemical vapor deposition highly heat-conductive material.
A kind of preparation method of alveolate texture enhancing composite of the present invention, cellular reinforcement and metallic matrix are compound
When, first using one kind in physical vapour deposition (PVD), chemical vapor deposition, chemical plating, plating, cellular reinforcement surface is deposited
It is compound with metallic matrix again after one layer of transition zone, one or more of the buffer layer material in tungsten, molybdenum, titanium, nickel, chromium,
Or buffer layer material is selected from carbide TiC, WC, Cr7C3, NiC, Mo2One or more in C, transition region thickness are 1nm-2 μm.
A kind of alveolate texture enhancing Metal Substrate or polymer matrix composite and preparation method thereof provided by the invention, it is multiple
Condensation material is made up of cellular backing material, highly heat-conductive material, matrix material, cellular backing material can be copper, titanium, tungsten, molybdenum,
At least one of the metals and its alloy such as chromium, highly heat-conductive material can be the one or more in diamond, graphene, CNT
Compound, matrix material can be that high-thermal conductive metal material is alternatively polymeric material.In addition, high heat conduction can be added in matrix material
Particle, high heat conduction particle can high purity granular or composite particles, high purity granular can be diamond particles, CNT, Graphene powder
Middle one kind, composite particles can be graphene coated diamond particles, CNT cladding diamond particle.The composite is along honeybee
Nest shape porous conductive material forms continuous quick conductive passage, whole Heat Conduction Material is turned into an entirety, relative to biography
System particles reiforced metal-base composition, the heat transfer efficiency of reinforcement are greatly improved, and are a kind of very promising new
Thermal management materials.Compared to publication CN105239026A and CN105220049A, there is more continuous Reinforcement structure, leading
There is the raising of matter on the thermal efficiency.Compared to patent CN105112754A, heat conduction has more directionality, and it is preferably fixed axially to have along honeycomb
To heat conductivility, the differentiated control to heat is realized to a certain extent, and stock utilization is higher.In addition, honeycomb has
The characteristics of designability is strong, steady quality, high-strength light, can meet need of the field of aerospace to high performance light heat exchanging material
Ask.
Composite prepared by the present invention forms continuous quick conductive passage along alveolate texture direction, and along honeybee
Nest axially has preferably orientation heat conductivility, can realize to a certain extent higher to hot differentiated control, stock utilization.
Suitable for industrial applications.
Embodiment
Technical scheme is further described below by specific embodiment.
Composite prepared by the embodiment of the present invention carries out thermal conductivity measurement using laser conductometer.
Embodiment one：The aluminium composite material of diamond alveolate texture enhancing
Comprise the following steps：
(1) it is highly 1mm to choose Cu cellular units, is first surface-treated, and is removed with acetone by cellular substrate surface
Greasy dirt, after removing cellular substrate surface oxide with pickling, removal acid solution is washed with water, finally, absolute ethyl alcohol is cleaned by ultrasonic；
W film layers are sputtered in honeycomb substrate surface using magnetically controlled sputter method, wherein W film thicknesses are 150nm；
(2) the honeycomb substrate surface depositing diamond film of HF CVD after modification, deposition process parameters are used：Heated filament away from
From 6mm, 800 DEG C of substrate temperature, 2200 DEG C, deposition pressure 3KPa of hot-wire temperature, sedimentation time 60 hours, CH4/H2Volume flow
Than 1:99；Using magnetically controlled sputter method, diamond cellular material surface sputters Mo/Ni/Cu composite films, wherein Mo in deposition
Film thickness is 50nm, and Ni film thicknesses are 50nm, and Cu film thicknesses are 100nm；
(3) diamond cellular material in the deposition being modified is put into mould, by 2 times of diamond honeycomb skeleton volume
Al-Si alloys are placed on above skeleton, and wherein Si mass content is 10%, is then placed in heating furnace, are protected in high pure nitrogen
Lower 870 DEG C of insulations 30min is protected, produces the aluminium composite material of stone alveolate texture enhancing, the thermal conductivity of composite is 472W/
MK, tensile strength 503MPa, bending strength 47MPa.
Embodiment two：Diamond/graphene alveolate texture reinforced epoxy composite
Comprise the following steps：
(1) it is highly 0.5mm to choose Ni cellular units, is first surface-treated, and is removed with acetone by cellular substrate table
Face greasy dirt, after removing cellular substrate surface oxide with pickling, removal acid solution is washed with water, finally, absolute ethyl alcohol ultrasound is clear
Wash；Mo film layers are sputtered in honeycomb substrate surface using magnetically controlled sputter method, wherein Mo film thicknesses are 250nm；
(2) the honeycomb substrate surface depositing diamond film of HF CVD after modification, deposition process parameters are used：Heated filament away from
From 6mm, 850 DEG C of substrate temperature, 2200 DEG C, deposition pressure 3KPa of hot-wire temperature, sedimentation time 100 hours, CH4/H2Volume flow
Than 1:99；Graphene wall, deposition parameter are grown using HF CVD：H2/CH4Atmosphere, CH4Gas mass flow percentage is
20%, growth temperature is 700 DEG C, grows air pressure 5 × 105Pa, plasma electric current density 20mA/cm2, magnetic field is strong in deposition region
Spend for 200 Gausses, time 20min；Using chemical plating method, diamond/graphene cellular material plates Cu films in deposition, its
Middle Cu film thicknesses are 50nm, and Ni film thicknesses are 50nm, and Cu film thicknesses are 100nm；
(3) volume fraction epoxy resin 50% is pressed, heat conduction particle 10%, coupling agent 1%, antioxidant 0.5%, processing helps
The ratio batch mixing of agent 2%；Diamond/graphene cellular material is put into mould, die casting at normal temperatures, the epoxy that will have been configured
Resin batch mixing is expelled in mould；After injection, with the program Solidification of setting：130℃/2h+150℃/1h+180℃/2h+
200℃/3h.Normal temperature is naturally cooled to after the completion of solidification.Sample is removed from the molds, that is, obtains composite, composite edge
The thermal conductivity in honeycomb wall direction is 396W/mK, tensile strength 312MPa, bending strength 34MPa.
Embodiment three：Diamond/carbon nanotube alveolate texture enhancing Cu-base composites and preparation method thereof
Comprise the following steps：
(1) it is highly 2mm to choose Cu cellular units, is first surface-treated, and is removed with acetone by cellular substrate surface
Greasy dirt, after removing cellular substrate surface oxide with pickling, removal acid solution is washed with water, finally, absolute ethyl alcohol is cleaned by ultrasonic；
W film layers are sputtered in honeycomb substrate surface using magnetically controlled sputter method, wherein W film thicknesses are 150nm；
(2) the honeycomb substrate surface depositing diamond film of HF CVD after modification, deposition process parameters are used：Heated filament away from
From 6mm, 800 DEG C of substrate temperature, 2200 DEG C, deposition pressure 3KPa of hot-wire temperature, sedimentation time 200 hours, CH4/H2Volume flow
Than 1:99；Using magnetically controlled sputter method, diamond cellular material surface sputters Mo/Ni/Cu composite films, wherein Mo in deposition
Film thickness is 50nm, and Ni film thicknesses are 50nm, and Cu film thicknesses are 100nm；Cu films surface ultrasound acetone soln concussion absorption nanometer
NiFe2O4Particle；Cu films surface HF CVD prepares CNT technological parameter：CH4/H2Carbonaceous gas mass flow percentage is
10%；Growth temperature is 800 DEG C, and growth air pressure is 104Pa；Plasma electric current density 10mA/cm2；Magnetic field intensity in deposition region
For 200 Gausses；
(3) diamond/carbon nanotube cellular material is put into mould, height is led into continuous diamond strengthens volume array skeleton
2 times of Cu-Zn alloys of volume are placed on above skeleton, and wherein Zn mass content is 20%, is then placed in heating furnace, in height
The lower 1400 DEG C of insulations 30min of purity nitrogen gas shielded, you can alveolate texture enhancing carbon/carbon-copper composite material is made, composite is along honeycomb wall
The thermal conductivity in direction is 868W/mK, tensile strength 578MPa, bending strength 62MPa.
Example IV：Diamond alveolate texture reinforced epoxy based composites and preparation method thereof
Comprise the following steps：
(1) it is highly 1.5mm to choose cellular unit, is first surface-treated, and is removed with acetone by cellular substrate surface
Greasy dirt, after removing cellular substrate surface oxide with pickling, removal acid solution is washed with water, finally, absolute ethyl alcohol is cleaned by ultrasonic；
Ni film layers are sputtered using the honeycomb substrate surface of magnetically controlled sputter method after modification, wherein Ni film thicknesses are 1 μm；
(2) HF CVD depositing diamond film, deposition process parameters are used：Heated filament distance 6mm, 850 DEG C of substrate temperature, heat
2250 DEG C, deposition pressure 3KPa of temperature of silk, sedimentation time 90 hours, CH4/H2Volume flow ratio 1:99；Using magnetically controlled sputter method
Diamond cellular material surface sputters Mo, film thickness 50nm in deposition；
(4) diamond cellular material is placed in the mould of extrusion process；By volume fraction epoxy resin 40%, heat conduction
Grain 20%, coupling agent 0.8%, antioxidant 0.6%, the ratio batch mixing of processing aid 3%；Mixed matrix material is placed in resin
In the mould of film infiltration process, insert in the deposition being modified in diamond cellular material, closed with the vacuum bag of sealing positioning
Die cavity.Then heated with a baking oven, melt resin.Resin permeable fiber layer solidify afterwards under vacuum, curing process 130
℃/1h+150℃/1h+180℃/2h+200℃/2h+220℃/6h.Room temperature is naturally cooled to after the completion of solidification, is taken from mould
Go out sample, thermal conductivity of the composite along honeycomb wall direction is 194W/mK, tensile strength 271MPa, bending strength 30MPa.
Embodiment five：The carbon/carbon-copper composite material of diamond alveolate texture enhancing
Comprise the following steps：
(1) it is highly 2mm to choose Cu cellular units, is first surface-treated, and is removed with acetone by cellular substrate surface
Greasy dirt, after removing cellular substrate surface oxide with pickling, removal acid solution is washed with water, finally, absolute ethyl alcohol is cleaned by ultrasonic；
Mo film layers are sputtered in honeycomb substrate surface using magnetically controlled sputter method, wherein Mo film thicknesses are 300nm；
(2) the honeycomb substrate surface depositing diamond film of HF CVD after modification, deposition process parameters are used：Heated filament away from
From 6mm, 800 DEG C of substrate temperature, 2200 DEG C of hot-wire temperature, deposition pressure 3KPa, CH4/H2Volume flow ratio 1:99, obtain Buddha's warrior attendant
100 μm of stone film thickness；Using magnetically controlled sputter method, diamond cellular material surface sputters Mo/Ni/Cu composite films in deposition,
Wherein Mo film thicknesses are 50nm, and Ni film thicknesses are 50nm, and Cu film thicknesses are 100nm；
(3) diamond cellular material in the deposition being modified is fixed and be put into mould, height is led into continuous diamond strengthens
2 times of Cu-Zn alloys of volume array skeleton volume are placed on above skeleton, and wherein Zn mass content is 10%, are then placed in and are added
In hot stove, 1350 DEG C of insulation 30min under high pure nitrogen protection, you can two-dimensional network arrangement diamond framework enhancing aluminium base is made
Composite, heat conductivity are respectively 687W/ (mK), tensile strength 515MPa, bending strength 60MPa.
Embodiment six：Graphene alveolate texture strengthens silicon rubber composite material
Comprise the following steps：
(1) it is highly 1.5mm to choose Ni cellular units, is first surface-treated, and is removed with acetone by cellular substrate table
Face greasy dirt, after removing cellular substrate surface oxide with pickling, removal acid solution is washed with water, finally, absolute ethyl alcohol ultrasound is clear
Wash；Mo film layers are sputtered in honeycomb substrate surface using magnetically controlled sputter method, wherein Mo film thicknesses are 200nm；
(2) graphene, deposition are grown in substrate surface using plasma-assisted chemical vapour deposition in honeycomb substrate surface
During on foam framework substrate apply plasma asistance growth, and by substrate bottom add magnetic field plasma about
Beam strengthens bombardment of the plasma to foam framework surface, graphene is given birth to perpendicular to diamond surface in foam framework near surface
It is long, the bubble for a large amount of graphene walls of length of being looked unfamiliar in acquisition mesh containing a large amount of graphene coated diamond high heat conduction particles and Skeleton Table
Foam skeleton, deposition parameter are：Substrate temperature is 800 DEG C, deposition pressure 5.0kPa, CH4/H2Volume flow ratio 1:99, plasma
Current density 5mA/cm2；The orientation of growth of lower control graphene is acted under extra electric field simultaneously, makes them vertically and substrate surface
Graphene wall is formed, magnetic field intensity is 500 Gausses wherein in deposition region, obtains surface with the graphene wall array erect
Honeycomb reinforcement；
(3) using chemical plating method, graphene cellular material plates Cu films in deposition, and wherein Cu film thicknesses are 50nm；
(4) carried out using dipping solidification compound：A) silicon rubber precursor liquid is prepared：Weigh 209 silicon rubber presomas, by its with
The curing agent being furnished with during purchase is by 10:1 mass ratio mixing, gained mixture and organic solvent acetic acid ethyl ester again in mass ratio 1:
9 mixing, are vigorously agitated again about 5 minutes, and mixture is carried out into vacuumize process removes wherein bubble for 5 minutes, final to obtain silicon rubber
The acetic acid ethyl ester solution of glue presoma；B) mix：The honeycomb structural framework of graphene wall array is put into mould, then according to body
Product ratio 1:2 instill silicon rubber precursor solution, permeate it and fully infiltrate diamond macroscopic body, obtain mixture；C) at vacuum
Reason：Above-mentioned mixture is subjected to application of vacuum 2h, solvent and bubble therein is removed, silicon rubber precursor liquid is preferably filled into
In the hole of honeycomb skeleton；D) 80 DEG C, and heat preservation solidification 4h are heated to, obtains strengthening silicon rubber with graphene alveolate texture
Composite, the thermal conductivity of composite is 184W/mK, tensile strength 296MPa, bending strength 33MPa.
Embodiment seven：CNT coated graphite alkene alveolate texture strengthens PPMA composites
Comprise the following steps：
(1) it is highly 2.5mm to choose Cu cellular units, is first surface-treated, and is removed with acetone by cellular substrate table
Face greasy dirt, after removing cellular substrate surface oxide with pickling, removal acid solution is washed with water, finally, absolute ethyl alcohol ultrasound is clear
Wash；Cr film layers are sputtered in honeycomb substrate surface using magnetically controlled sputter method, wherein Cr thickness is 250nm；
(2) hot-wall cvd deposited graphite alkene film is used in honeycomb substrate surface, is specially：Heated in H2 and Ar atmosphere
To 950 DEG C (H2 and Ar flow velocitys are respectively 200 and 500mL/min in heating process, and programming rate is 33 DEG C/min), furnace temperature is treated
10min is heat-treated after rising to 950 DEG C；CH4, H2 and Ar mixed gas is passed through after the completion of heat treatment, and (gas flow rate is respectively first
Alkane 5mL/min, hydrogen 200mL/min and argon gas 500mL/min), start to grow graphene, 100 DEG C/min of cooling velocity, obtain
Graphene film average thickness is 1.7nm, that is, obtains graphene alveolate texture reinforcement；
(3) recycle magnetron sputtering to deposit one layer of nickel in graphenic surface, then sunk using plasma enhanced chemical vapor
Product acts on the orientation of growth of lower control CNT in graphenic surface catalytic growth CNT, while under extra electric field, makes
They vertically form CNT woods with graphenic surface, obtain the strengthening layer of CNT coated graphite alkene film, deposition parameter
For：Methane, hydrogen mass flow percentage is 15%；Growth temperature is 650 DEG C, growth air pressure 3000Pa；Plasma electric current density
5mA/cm2；Magnetic field intensity is 500 Gausses in deposition region, obtains CNT coated graphite alkene alveolate texture reinforcement；
(4) using chemical plating method, graphene cellular material plates Ti films in deposition, and wherein Ti film thicknesses are 30nm；
(5) carried out using dipping solidification compound：A) pMMA (poly-methyl methacrylate vinegar) precursor liquid is prepared：Weigh
20gpMMA, it is mixed with organic solvents, chloroform, be stirred vigorously 2h to PMMA and be completely dissolved, forming PMMA mass percents is
10% chloroformic solution；B) mix：Diamond three-dimensional network is put into mould, then according to volume ratio 1:5 instill PMMA's
Chloroformic solution, permeate it and fully infiltrate diamond three-dimensional network, obtain mixture；C) heat, solidify：Above-mentioned mixture is put
24h is dried in vacuo in 60 DEG C in vacuum drying oven and steams chloroform solvent, be then heated to 110 DEG C, after being incubated 1h, be down to room temperature,
The diamond with three-dimensional network skeleton structure/PMMA composites are finally given, the thermal conductivity of composite is 152W/mK,
Tensile strength 302MPa, bending strength 37MPa.
It was found from the thermal conductivity and mechanical performance data that above example obtains, alveolate texture prepared by the present invention strengthens
Thermal conductivity, tensile strength, bending strength of the metal-base composites along honeycomb wall direction obtain tremendous increase, and thermal conductivity is high
Up to 868W/mK, tensile strength is up to 578MPa, and bending strength is up to 62MPa, and composite prepared by the present invention is along cellular knot
Continuous quick conductive passage is formd on structure direction, and axially there is more preferable calorifics and mechanical property along honeycomb, can be one
Determine to realize the differentiated control to heat in degree, stock utilization is higher, and combination property is apparently higher than traditional Metal Substrate or polymerization
The thermal conductivity of thing based composites.
Claims (11)
1. a kind of alveolate texture strengthens composite, it is characterised in that described composite include cellular reinforcement and
Matrix material, described matrix material are high-thermal conductive metal or polymer；The cellular reinforcement is wrapped on cellular substrate
Highly heat-conductive material is covered with, described highly heat-conductive material is selected from diamond/graphene film, diamond film/CNT, graphene
One kind in film/CNT, diamond/graphene/carbon nano-tube film；
Alveolate texture strengthens the preparation method of composite, comprises the steps：
The first step：Prepare cellular reinforcement
By the cleaning of alveolate texture substrate, drying；Highly heat-conductive material is deposited in diamond surface using chemical vapor deposition；Height is led
Hot material diamond, graphene, the deposition process parameters of CNT are：
Diamond CVD deposition parameter is：It is 0.5-10% that carbonaceous gas, which accounts for all gas mass flow percentage in stove,；Growth temperature
Spend for 600-1000 DEG C, growth air pressure is 103-104Pa；
Graphene CVD deposition parameter is：It is 0.5-80% that carbonaceous gas, which accounts for all gas mass flow percentage in stove,；Growth temperature
Spend for 400-1200 DEG C, growth air pressure is 5-105Pa；
CNT CVD deposition parameter is：It is 5-50% that carbonaceous gas, which accounts for all gas mass flow percentage in stove,；Growth temperature
Spend for 400-1300 DEG C, growth air pressure is 103-105Pa；
By to applying plasma and induced by magnetic field, and regulation carbon throughput, growth temperature, growth in real time in CVD deposition stove
Air pressure, realize highly heat-conductive material diamond/graphene, diamond/carbon nanotube, diamond/graphene/carbon nano-tube film
CVD deposition, deposition parameter are：
Diamond CVD deposition parameter is：It is 0.5-10% that carbonaceous gas, which accounts for all gas mass flow percentage in stove,；Growth temperature
Spend for 600-1000 DEG C, grow air pressure 103-104Pa；
Graphene CVD deposition parameter is：It is 0.5-80% that carbonaceous gas, which accounts for all gas mass flow percentage in stove,；Growth temperature
Spend for 400-1200 DEG C, growth air pressure is 5-105Pa；Plasma electric current density is 0.1-50mA/cm2；Magnetic field is strong in deposition region
Spend for 100 Gausses to 30 teslas；
CNT CVD deposition parameter is：It is 5-50% that carbonaceous gas, which accounts for all gas mass flow percentage in stove,；Growth temperature
Spend for 400-1300 DEG C, grow air pressure 103-105Pa；Plasma electric current density 0-30mA/cm2；Magnetic field intensity is in deposition region
100 Gausses to 30 teslas；
Highly heat-conductive material thickness is 0.34nm-1mm；
Second step：Cellular reinforcement and matrix progress is compound, obtain alveolate texture enhancing Metal Substrate or polymer matrix is answered
Condensation material；
Cellular reinforcement and metallic matrix compound tense, use is cold-rolled sintered, hot pressed sintering, plasma agglomeration, pressureless infiltration, pressure
A kind of technology in power infiltration, casting carries out compound；
Cellular reinforcement and polymeric matrix compound tense, using dipping curing molding, injection moulding, compressing, rotational moulding into
A kind of technology in type, injection molding, extrusion moulding, laminated into type, flow casting molding carries out compound.
2. a kind of alveolate texture enhancing composite according to claim 1, it is characterised in that described matrix material is
During high-thermal conductive metal, the one kind of matrix material in metallic copper, aluminium, silver, copper alloy, aluminium alloy, silver alloy, the copper closes
Copper, aluminium, the weight/mass percentage composition of silver are more than or equal to 50% in gold, aluminium alloy, silver alloy；Polymeric matrix is thermoplastic polymer
Or thermosetting polymer；The thermoplastic polymer is selected from polyethylene, polypropylene, polystyrene, polyvinyl chloride, polytetrafluoroethyl-ne
In alkene, nylon, makrolon, polymethyl methacrylate, glycol ester, poly terephthalic acid, polyformaldehyde, polyamide, polysulfones
One kind；The thermosetting polymer be selected from epoxy resin, phenolic resin, Lauxite, amino resins, melmac,
One kind in unsaturated polyester resin, organic siliconresin, silicon rubber, expanded polystyrene (EPS), polyurethane.
3. a kind of alveolate texture enhancing composite according to claim 2, it is characterised in that also contain in composite
There is high heat conduction particle, the high heat conduction particle is selected from diamond particles, CNT, Graphene powder, graphene coated diamond
At least one of particle, CNT cladding diamond particle.
4. a kind of alveolate texture enhancing composite according to claim 1-3 any one, it is characterised in that compound
In material, the volume fraction of cellular reinforcement is 5-70%, and matrix material volume fraction is 30-95%, high heat conduction particle volume
Fraction is 0-50%.
A kind of 5. alveolate texture enhancing composite according to claim 1, it is characterised in that cellular backing material
One kind in one kind or acid bronze alloy, titanium-base alloy, molybdenum-base alloy in metallic copper, titanium, tungsten, molybdenum, chromium, nickel, the copper
In based alloy, titanium-base alloy, molybdenum-base alloy, copper, titanium, the weight/mass percentage composition of molybdenum are more than or equal to 50%.
6. a kind of alveolate texture enhancing composite according to claim 4, it is characterised in that included in composite
At least one cellular reinforcement.
7. a kind of alveolate texture enhancing composite according to claim 6, it is characterised in that included in composite
Multiple cellular reinforcements, cellular reinforcement are sheet or strip, and described strip or the cellular reinforcement of sheet are with array
Form is compound with matrix material；Or described strip or the cellular reinforcement of sheet be alternately stacked it is compound with matrix material；It is compound
Cellular reinforcement in material is identical or different.
A kind of 8. alveolate texture enhancing composite according to claim 7, it is characterised in that cellular reinforcement
In, it is arranged in order and is formed for the honeycomb or rectangle honeycomb of hexagon by section.
A kind of 9. alveolate texture enhancing composite according to claim 1, it is characterised in that：In the first step, by honeybee
After the cleaning of nest shape structured substrate, drying；First using plating, chemical plating, evaporation, magnetron sputtering, chemical vapor deposition, physical vapor
A kind of method in deposition is after one kind during substrate surface deposits nickel, copper, tungsten, molybdenum, titanium, silver, chromium or complex metal layer, then adopts
With chemical vapor deposition highly heat-conductive material.
A kind of 10. alveolate texture enhancing composite according to claim 9, it is characterised in that：Alveolate texture serves as a contrast
After basal surface prepares metal level, first it is soaked in nano-diamond powder or Graphene powder or carbon nanotube suspension and carries out ultrasonic shake
Plantation seed crystal is swung, then, using chemical vapor deposition highly heat-conductive material.
A kind of 11. alveolate texture enhancing composite according to any one of claim 9 or 10, it is characterised in that：
Cellular reinforcement and metallic matrix compound tense, first using in physical vapour deposition (PVD), chemical vapor deposition, chemical plating, plating
One kind, to cellular reinforcement surface deposit one layer of transition zone after it is compound with metallic matrix again, buffer layer material be selected from tungsten,
One or more in molybdenum, titanium, nickel, chromium, or buffer layer material are selected from carbide TiC, WC, Cr7C3, NiC, Mo2One kind in C
It is or a variety of.
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