CN105755307A - Reinforced composite adopting honeycomb structure and preparation method - Google Patents
Reinforced composite adopting honeycomb structure and preparation method Download PDFInfo
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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Abstract
The invention discloses a reinforced composite adopting a honeycomb structure and a preparation method. The composite comprises a honeycomb substrate material, a high-thermal-conductivity film layer, a matrix material and high-thermal-conductivity particles, wherein the honeycomb substrate material is metal; the high-thermal-conductivity material is a single substance or a combination of multiple substances of diamond, graphene and carbon nanotubes; the matrix material is a high-thermal-conductivity metal material or a polymer material. A continuous rapid thermal conduction channel is formed in the composite in the honeycomb structure direction, the composite has better directional thermal conduction performance in the axial direction of the honeycomb, graded management of heat can be realized to a certain extent, and the material utilization rate is higher. Besides, the honeycomb structure has the characteristics of high designability, stable quality, high strength and light weight, can meet the demands for high-performance light radiating materials in the fields such as aerospace, ships, transportation and the like and is suitable for industrial application.
Description
Technical field
The invention discloses a kind of alveolate texture reinforced composite and preparation method, belong to technical field of composite preparation.
Background technology:
Making rapid progress of modern science and technology, let us enjoy that its achievement is with convenient simultaneously, also the work for scientific research brings increasing challenge.Along with the fast development of electronics and information industry, variation, the superelevation development course being melted into electronic device integrated, microminiaturized, different in nature.To the requirement of encapsulating material, natural when the river rises the boat goes up, and all kinds of Heat Conduction Materials are also come out one after another.Divide from matrix, have Metal Substrate, ceramic base, polymer-matrix etc.；Divide from reinforcement, have diamond, Graphene, CNT etc.；Divide from the structure of reinforcement, have zero dimension graininess, one dimension fibre or wire, two-dimensional slice shape, three-dimensional network shape and special construction etc..Patent CN105239026A proposes a kind of one-dimensional diamond reinforced aluminum matrix composites and preparation method thereof patent, aluminum substrate is distributed the diamond array being made up of some one-dimensional diamond wires, one-dimensional diamond wire be surface modified diamond line and with aluminum substrate metallurgical binding；Heat transfer efficiency is promoted further by adding diamond particles formation connection in series-parallel composite heat-conducting structure.Patent CN105220049A proposes a kind of lamellar diamond reinforced metal-base composite material and preparation method, is provided with diamond wafers in parent metal, and diamond wafers and parent metal are metallurgical binding；Patent CN105112754A proposes a kind of three-dimensional network diamond framework and strengthens Cu-base composites and preparation method, composite is made up of metallic matrix (Al, Cu, Ag), three-dimensional network diamond framework and diamond particles, make this composite be respectively provided with the heat conductivility of excellence along three dimensional diamond skeleton direction by metallic matrix is distributed three-dimensional network diamond framework, and promote heat transfer efficiency further by adding diamond particles formation connection in series-parallel composite heat-conducting structure.
Compared with above-mentioned composite configuration, hexagonal Nidus Vespae can be described as a big miracle of nature.Its structure is stronger than any circular or foursquare structure, can undertake the external force from each side.The structure that honeycomb is so special just, the mankind are therefrom inspired, even if the most slim material, as long as it is made honeycomb shape, can bear very big external force, and be unlikely to deform, this not only reduces raw-material consumption, and can also beautify the environment.The feature of cellular structural material high-strength light, is used for aerospace field, and it is the composite of a kind of microlight-type answered the special requirement of Aero-Space science and technology and grow up, and rarely has the report in highly thermally conductive.
Summary of the invention
It is an object of the invention to overcome the deficiency of prior art, there is provided a kind of and be upwardly formed continuous print quick conductive passage along alveolate texture side, and axially there is alveolate texture reinforced composite and the preparation method of better directed heat conductivility along honeycomb, composite prepared by the present invention can realize the administration by different levels to heat to a certain extent, and stock utilization is higher.
One alveolate texture reinforced composite of the present invention, described composite includes cellular reinforcement and matrix material, and described matrix material is high-thermal conductive metal or polymer；Described cellular reinforcement is to be coated with highly heat-conductive material on cellular substrate, described highly heat-conductive material kind in diamond film, graphene film, carbon nano-tube film, diamond/graphene film, diamond/carbon nanotube films, graphene/carbon nano-tube film, diamond/graphene/carbon nano-tube film.
One alveolate texture reinforced composite of the present invention, when described matrix material is high-thermal conductive metal, matrix material one in metallic copper, aluminum, silver, copper alloy, aluminium alloy, silver alloy, in described copper alloy, aluminium alloy, silver alloy, copper, aluminum, silver-colored weight/mass percentage composition are be more than or equal to 50%；Polymeric matrix is thermoplastic polymer or thermosetting polymer；Described thermoplastic polymer one in polyethylene, polypropylene, polystyrene, polrvinyl chloride, politef, nylon, Merlon, polymethyl methacrylate, glycol ester, poly terephthalic acid, polyformaldehyde, polyamide, polysulfones；Described thermosetting polymer one in epoxy resin, phenolic resin, Lauxite, amino resins, melmac, unsaturated polyester resin, organic siliconresin, silicone rubber, expanded polystyrene (EPS), polyurethane.
One alveolate texture reinforced composite of the present invention, possibly together with high heat conduction particle in composite, described high heat conduction particle at least one in diamond particles, CNT, Graphene powder, graphene coated diamond particles, CNT cladding diamond granule.
One alveolate texture reinforced composite of the present invention, in composite, the volume fraction of cellular reinforcement is 5 70%, and matrix material volume fraction is 30 95%, and high heat conduction particle volume fraction is 0 50%, each volume components percent and be 100%.
One alveolate texture reinforced composite of the present invention, one in the cellular backing material a kind of or acid bronze alloy, titanium-base alloy, molybdenum-base alloy in metallic copper, titanium, tungsten, molybdenum, chromium, the nickel, copper in described acid bronze alloy, titanium-base alloy, molybdenum-base alloy, titanium, molybdenum weight/mass percentage composition be more than or equal to 50%.
One alveolate texture reinforced composite of the present invention, comprises at least one cellular reinforcement in composite；
Or
Comprising multiple cellular reinforcement in composite, cellular reinforcement is lamellar or strip, described strip or the cellular reinforcement of lamellar in the form of an array with matrix material compound；Or described strip or the cellular reinforcement of lamellar are alternately stacked and matrix material compound；Cellular reinforcement in composite is identical or different.
One alveolate texture reinforced composite of the present invention, in cellular reinforcement, is hexagonal honeycomb by cross section or rectangle honeycomb is arranged in order and constitutes, the thickness of cellular reinforcement is 0.01～10mm, pore wall thickness 0.01～5mm.
The preparation method of a kind of alveolate texture reinforced composite of the present invention, comprises the steps:
The first step: prepare cellular reinforcement
Alveolate texture substrate is cleaned, dries；Chemical vapour deposition (CVD) is adopted to deposit highly heat-conductive material at diamond surface；Highly heat-conductive material graphite, diamond, Graphene, CNT deposition process parameters be:
Graphene CVD deposition parameter is: it is 0.5-80% that carbonaceous gas accounts for all gas mass flow percentage ratio in stove；Growth 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 accounts for all gas mass flow percentage ratio in stove；Growth 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 accounts for all gas mass flow percentage ratio in stove；Growth temperature is 600-1000 DEG C, and growth air pressure is 103-104Pa；
By to applying plasma and induced by magnetic field in CVD deposition stove, and regulate carbon throughput, growth temperature, growth air pressure in real time, realizing the CVD deposition of highly heat-conductive material diamond/Graphene, diamond/carbon nanotube, diamond/graphene/carbon nano-tube film, deposition parameter is:
Graphene CVD deposition parameter is: it is 0.5-80% that carbonaceous gas accounts for all gas mass flow percentage ratio in stove；Growth temperature is 400-1200 DEG C, and growth air pressure is 5-105Pa；Plasma electric current density 0-50mA/cm2；In deposition region, magnetic field intensity is 100 Gausses to 30 teslas；
CNT CVD deposition parameter is: it is 5-50% that carbonaceous gas accounts for all gas mass flow percentage ratio in stove；Growth temperature is 400-1300 DEG C, and growth air pressure is 103-105Pa；Plasma electric current density 0-30mA/cm2；In deposition region, magnetic field intensity is 100 Gausses to 30 teslas；
Diamond CVD deposition parameter is: it is 0.5-10% that carbonaceous gas accounts for all gas mass flow percentage ratio in stove；Growth 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 are carried out compound, obtains alveolate texture and strengthens Metal Substrate or polymer matrix composite；
Cellular reinforcement and metallic matrix compound tense, adopt a kind of technology in cold-rolled sintered, hot pressed sintering, plasma agglomeration, pressureless infiltration, pressure infiltration, casting to carry out compound；
Cellular reinforcement and polymeric matrix compound tense, adopt a kind of technology in dipping curing molding, injection moulding, compressing, rotation molding, injection mo(u)lding, extrusion moulding, laminated into type, flow casting molding to carry out compound.
The preparation method of a kind of alveolate texture reinforced composite of the present invention, in the first step, after the cleaning of alveolate texture substrate, drying；First adopt a kind of method in plating, chemical plating, evaporation, magnetron sputtering, chemical vapour deposition (CVD), physical vapour deposition (PVD) to deposit the one in nickel, copper, tungsten, molybdenum, titanium, silver, chromium at substrate surface or after complex metal layer, then adopt chemical vapour deposition (CVD) highly heat-conductive material；Metal layer thickness is 1nm-2 μm.
The preparation method of a kind of alveolate texture reinforced composite of the present invention, after alveolate texture substrate surface prepares metal level, first it is soaked in nano-diamond powder or Graphene powder or carbon nanotube suspension and carries out ultrasonic vibration plantation seed crystal, then, adopt chemical vapour deposition (CVD) highly heat-conductive material.
The preparation method of a kind of alveolate texture reinforced composite of the present invention, cellular reinforcement and metallic matrix compound tense, first adopt the one in physical vapour deposition (PVD), chemical vapour deposition (CVD), chemical plating, plating, cellular reinforcement surface is deposited after one layer of transition zone again with metallic matrix compound, buffer layer material is selected from one or more 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 is 1nm 2 μm.
A kind of alveolate texture provided by the invention strengthens Metal Substrate or polymer matrix composite and preparation method thereof, composite is made up of cellular backing material, highly heat-conductive material, matrix material, cellular backing material can be at least one in the metals such as copper, titanium, tungsten, molybdenum, chromium and alloy thereof, highly heat-conductive material can be one or more compounds in diamond, Graphene, CNT, and matrix material can be alternatively polymeric material for high-thermal conductive metal material.In addition; matrix material can add high heat conduction particle; high heat conduction particle can high purity granular or composite particles, high purity granular can be a kind of in diamond particles, CNT, Graphene powder, and composite particles can be graphene coated diamond particles, CNT cladding diamond granule.This composite defines continuous print quick conductive passage along cellular porous Heat Conduction Material, whole Heat Conduction Material is made to become as a whole, strengthening metal-base composites relative to conventional particles, the heat transfer efficiency of reinforcement is greatly improved, and is the very potential Novel hot management material of one.Compare publication CN105239026A and CN105220049A, there is more continuous print Reinforcement structure, heat transfer efficiency has the raising of matter.Comparing patent CN105112754A, heat conduction is directivity more, axially has better directed heat conductivility along honeycomb, achieves the administration by different levels to heat to a certain extent, and stock utilization is higher.Additionally, honeycomb texture has, designability is strong, the feature of steady quality, high-strength light, can meet the field of aerospace demand to high performance light heat exchanging material.
Composite prepared by the present invention defines continuous print quick conductive passage along alveolate texture direction, and axially has better directed heat conductivility along honeycomb, can realize the administration by different levels to heat to a certain extent, and stock utilization is higher.Be suitable to industrial applications.
Detailed description of the invention
Technical scheme is further described below by specific embodiment.
Composite prepared by the embodiment of the present invention adopts laser conductometer to carry out thermal conductivity measurement.
Embodiment one: the aluminium composite material that diamond alveolate texture strengthens
Comprise the following steps:
(1) choosing Cu cellular unit height is 1mm, first carries out surface treatment, removes cellular substrate surface greasy dirt with acetone, after removing cellular substrate surface oxide with pickling, washes removal acid solution with water, finally, and dehydrated alcohol ultrasonic cleaning；Adopting magnetically controlled sputter method to sputter W rete at honeycomb substrate surface, wherein W film thickness is 150nm；
(2) HF CVD honeycomb substrate surface depositing diamond film after modification, deposition process parameters: heated filament distance 6mm, substrate temperature 800 DEG C, hot-wire temperature 2200 DEG C, deposition pressure 3KPa, sedimentation time 60 hours, CH are adopted4/H2Volume flow ratio 1:99；Adopting magnetically controlled sputter method diamond cellular material surface sputtering Mo/Ni/Cu composite film in deposition, wherein Mo film thickness is 50nm, Ni film thickness be 50nm, Cu film thickness is 100nm；
(3) diamond cellular material in the deposition of modified mistake is put in mould; 2 times of Al-Si alloys of diamond honeycomb skeleton volume are placed on above skeleton; wherein the mass content of Si is 10%; it is then placed in heating furnace; under high pure nitrogen is protected, 870 DEG C of insulation 30min, obtain the aluminium composite material that stone alveolate texture strengthens, and the thermal conductivity of composite is 472W/mK; tensile strength 503MPa, bending strength is 47MPa.
Embodiment two: diamond/Graphene alveolate texture reinforced epoxy composite
Comprise the following steps:
(1) choosing Ni cellular unit height is 0.5mm, first carries out surface treatment, removes cellular substrate surface greasy dirt with acetone, after removing cellular substrate surface oxide with pickling, washes removal acid solution with water, finally, and dehydrated alcohol ultrasonic cleaning；Adopting magnetically controlled sputter method to sputter Mo rete at honeycomb substrate surface, wherein Mo film thickness is 250nm；
(2) HF CVD honeycomb substrate surface depositing diamond film after modification, deposition process parameters: heated filament distance 6mm, substrate temperature 850 DEG C, hot-wire temperature 2200 DEG C, deposition pressure 3KPa, sedimentation time 100 hours, CH are adopted4/H2Volume flow ratio 1:99；Adopt HF CVD growth Graphene wall, deposition parameter: H2/CH4Atmosphere, CH4Gas mass flow percentage ratio is 20%, and growth temperature is 700 DEG C, grows air pressure 5 × 105Pa, plasma electric current density 20mA/cm2, in deposition region, magnetic field intensity is 200 Gausses, and the time is 20min；Adopting chemical plating method diamond/Graphene cellular material plating Cu film in deposition, wherein Cu film thickness is 50nm, Ni film thickness be 50nm, Cu film thickness is 100nm；
(3) by volume mark epoxy resin 50%, heat conduction particle 10%, coupling agent 1%, antioxidant 0.5%, the ratio batch mixing of processing aid 2%；Diamond/Graphene cellular material is put in mould, die casting at normal temperatures, the epoxy resin batch mixing configured is expelled in mould；After injection, the program Solidification to set: 130 DEG C/2h+150 DEG C/1h+180 DEG C/2h+200 DEG C/3h.Room temperature is naturally cooled to after having solidified.Being removed from the molds sample, namely obtain composite, composite is 396W/mK along the thermal conductivity in honeycomb wall direction, tensile strength 312MPa, and bending strength is 34MPa.
Embodiment three: diamond/carbon nanotube alveolate texture strengthens Cu-base composites and preparation method thereof
Comprise the following steps:
(1) choosing Cu cellular unit height is 2mm, first carries out surface treatment, removes cellular substrate surface greasy dirt with acetone, after removing cellular substrate surface oxide with pickling, washes removal acid solution with water, finally, and dehydrated alcohol ultrasonic cleaning；Adopting magnetically controlled sputter method to sputter W rete at honeycomb substrate surface, wherein W film thickness is 150nm；
(2) HF CVD honeycomb substrate surface depositing diamond film after modification, deposition process parameters: heated filament distance 6mm, substrate temperature 800 DEG C, hot-wire temperature 2200 DEG C, deposition pressure 3KPa, sedimentation time 200 hours, CH are adopted4/H2Volume flow ratio 1:99；Adopting magnetically controlled sputter method diamond cellular material surface sputtering Mo/Ni/Cu composite film in deposition, wherein Mo film thickness is 50nm, Ni film thickness be 50nm, Cu film thickness is 100nm；Cu film surface ultrasonic acetone soln concussion absorption nano-Ni/Fe2O4Particle；Cu film surface HF CVD prepares CNT technological parameter: CH4/H2Carbonaceous gas mass flow percentage ratio is 10%；Growth temperature is 800 DEG C, and growth air pressure is 104Pa；Plasma electric current density 10mA/cm2；In deposition region, magnetic field intensity is 200 Gausses；
(3) diamond/carbon nanotube cellular material is put in mould; 2 times of Cu-Zn alloys that height is led continuous diamond enhancing volume array skeleton volume are placed on above skeleton; wherein the mass content of Zn is 20%; it is then placed in heating furnace; 1400 DEG C of insulation 30min under high pure nitrogen is protected, can be prepared by alveolate texture and strengthen carbon/carbon-copper composite material, and composite is 868W/mK along the thermal conductivity in honeycomb wall direction; tensile strength 578MPa, bending strength is 62MPa.
Embodiment four: diamond alveolate texture reinforced epoxy based composites and preparation method thereof
Comprise the following steps:
(1) choosing cellular unit height is 1.5mm, first carries out surface treatment, removes cellular substrate surface greasy dirt with acetone, after removing cellular substrate surface oxide with pickling, washes removal acid solution with water, finally, and dehydrated alcohol ultrasonic cleaning；Adopting magnetically controlled sputter method honeycomb substrate surface sputtering Ni rete after modification, wherein Ni film thickness is 1 μm；
(2) HF CVD depositing diamond film, deposition process parameters: heated filament distance 6mm, substrate temperature 850 DEG C, hot-wire temperature 2250 DEG C, deposition pressure 3KPa, sedimentation time 90 hours, CH are adopted4/H2Volume flow ratio 1:99；Adopting magnetically controlled sputter method diamond cellular material surface sputtering Mo in deposition, film thickness is 50nm；
(4) diamond cellular material is placed in the mould of extrusion process；By volume mark epoxy resin 40%, heat conduction particle 20%, coupling agent 0.8%, antioxidant 0.6%, the ratio batch mixing of processing aid 3%；Mixed matrix material is placed in the mould of Resin film infusion, inserts in the deposition modifiied in diamond cellular material, close die cavity with the vacuum bag sealing location.Then use a baking oven for heating, melt resin.Solidifying after resin permeable fiber layer under vacuum, curing process is 130 DEG C/1h+150 DEG C/1h+180 DEG C/2h+200 DEG C/2h+220 DEG C/6h.Naturally cooling to room temperature after having solidified, be removed from the molds sample, composite is 194W/mK along the thermal conductivity in honeycomb wall direction, tensile strength 271MPa, and bending strength is 30MPa.
Embodiment five: the carbon/carbon-copper composite material that diamond alveolate texture strengthens
Comprise the following steps:
(1) choosing Cu cellular unit height is 2mm, first carries out surface treatment, removes cellular substrate surface greasy dirt with acetone, after removing cellular substrate surface oxide with pickling, washes removal acid solution with water, finally, and dehydrated alcohol ultrasonic cleaning；Adopting magnetically controlled sputter method to sputter Mo rete at honeycomb substrate surface, wherein Mo film thickness is 300nm；
(2) HF CVD honeycomb substrate surface depositing diamond film after modification, deposition process parameters: heated filament distance 6mm, substrate temperature 800 DEG C, hot-wire temperature 2200 DEG C, deposition pressure 3KPa, CH are adopted4/H2Volume flow ratio 1:99, obtains diamond film thickness 100 μm；Adopting magnetically controlled sputter method diamond cellular material surface sputtering Mo/Ni/Cu composite film in deposition, wherein Mo film thickness is 50nm, Ni film thickness be 50nm, Cu film thickness is 100nm；
(3) put in mould by fixing for diamond cellular material in the deposition of modified mistake; 2 times of Cu-Zn alloys that height is led continuous diamond enhancing volume array skeleton volume are placed on above skeleton; wherein the mass content of Zn is 10%; it is then placed in heating furnace; 1350 DEG C of insulation 30min under high pure nitrogen is protected; can be prepared by two-dimensional network arrangement diamond framework reinforced aluminum matrix composites; heat conductivity respectively 687W/ (m K); tensile strength 515MPa, bending strength is 60MPa.
Embodiment six: Graphene alveolate texture strengthens silicon rubber composite material
Comprise the following steps:
(1) choosing Ni cellular unit height is 1.5mm, first carries out surface treatment, removes cellular substrate surface greasy dirt with acetone, after removing cellular substrate surface oxide with pickling, washes removal acid solution with water, finally, and dehydrated alcohol ultrasonic cleaning；Adopting magnetically controlled sputter method to sputter Mo rete at honeycomb substrate surface, wherein Mo film thickness is 200nm；
(2) plasma-assisted chemical vapour deposition is utilized to grow Graphene at substrate surface at honeycomb substrate surface, deposition process applies plasma asistance growth on foam framework substrate, and by adding magnetic field bottom substrate plasma confinement on the nearly surface of foam framework, the strengthening plasma bombardment to foam framework surface, Graphene is made to be perpendicular to diamond surface growth, obtain the foam framework of the amount of growing up Graphene wall of looking unfamiliar in mesh containing a large amount of graphene coated diamond height heat conduction particles and Skeleton Table, deposition parameter is: substrate temperature is 800 DEG C, deposition pressure is 5.0kPa, CH4/H2Volume flow ratio 1:99, plasma electric current density 5mA/cm2；The lower orientation of growth controlling Graphene of effect under extra electric field simultaneously, makes them vertical and substrate surface forms Graphene wall, and wherein in deposition region, magnetic field intensity is 500 Gausses, must arrive the honeycomb texture reinforcement that surface has the Graphene wall array of setting；
(3) adopting chemical plating method Graphene cellular material plating Cu film in deposition, wherein Cu film thickness is 50nm；
(4) dipping solidification is adopted to carry out compound: a) to prepare silicone rubber precursor liquid: weigh 209 silicone rubber presomas, it is mixed by the mass ratio of 10:1 with the firming agent being furnished with when buying, gained mixture and organic solvent acetic acid ethyl ester more in mass ratio 1:9 mix, it is vigorously agitated again about 5 minutes, mixture is carried out evacuation process and within 5 minutes, removes wherein bubble, the final acetic acid ethyl ester solution obtaining silicone rubber presoma；B) mixing: the honeycomb structural framework of Graphene wall array is put in mould, then according to volume ratio 1:2 instills silicone rubber precursor solution so that it is infiltration fully infiltration diamond macroscopic body, obtains mixture；C) application of vacuum: above-mentioned mixture is carried out application of vacuum 2h, removes solvent therein and bubble, makes silicone rubber precursor liquid be filled into better in the hole of honeycomb skeleton；D) heating is to 80 DEG C, and heat preservation solidification 4h, obtains having Graphene alveolate texture and strengthens silicon rubber composite material, and the thermal conductivity of composite is 184W/mK, tensile strength 296MPa, and bending strength is 33MPa.
Embodiment seven: CNT coated graphite alkene alveolate texture strengthens PPMA composite
Comprise the following steps:
(1) choosing Cu cellular unit height is 2.5mm, first carries out surface treatment, removes cellular substrate surface greasy dirt with acetone, after removing cellular substrate surface oxide with pickling, washes removal acid solution with water, finally, and dehydrated alcohol ultrasonic cleaning；Adopting magnetically controlled sputter method to sputter Cr rete at honeycomb substrate surface, wherein Cr thickness is 250nm；
(2) hot-wall cvd deposited graphite alkene film is adopted at honeycomb substrate surface, particularly as follows: heat in the atmosphere of H2 and Ar to 950 DEG C of (H2 and Ar flow velocitys respectively 200 and 500mL/min in heating process, programming rate is 33 DEG C/min), treat that furnace temperature rises to 950 DEG C of after-baking 10min；Heat treatment passes into the mixing gas (gas flow rate respectively methane 5mL/min, hydrogen 200mL/min and argon 500mL/min) of CH4, H2 and Ar after completing, start to grow Graphene, 100 DEG C/min of rate of cooling, obtaining graphene film average thickness is 1.7nm, namely obtains Graphene alveolate texture reinforcement；
(3) recycling magnetron sputtering deposits one layer of nickel at graphenic surface, then utilize plasma-assisted chemical vapour deposition at graphenic surface catalytic growth CNT, the lower orientation of growth controlling CNT of effect under extra electric field simultaneously, make them vertical and graphenic surface forms CNT woods, obtaining the strengthening layer of CNT coated graphite alkene film, deposition parameter is: methane, hydrogen mass flow percentage ratio is 15%；Growth temperature is 650 DEG C, grows air pressure 3000Pa；Plasma electric current density 5mA/cm2；In deposition region, magnetic field intensity is 500 Gausses, obtains CNT coated graphite alkene alveolate texture reinforcement；
(4) adopting chemical plating method Graphene cellular material plating Ti film in deposition, wherein Ti film thickness is 30nm；
(5) dipping solidification is adopted to carry out compound: a) to prepare pMMA (poly-methyl methacrylate vinegar) precursor liquid: weigh 20gpMMA, it is mixed with organic solvents, chloroform, it is stirred vigorously 2h to PMMA to be completely dissolved, forms the chloroformic solution that PMMA mass percent is 10%；B) mixing: diamond three-dimensional network put in mould, then according to volume ratio 1:5 instills the chloroformic solution of PMMA so that it is infiltration fully infiltration diamond three-dimensional network, obtains mixture；C) heating, solidification: above-mentioned mixture is placed in vacuum drying oven and steams chloroform solvent in 60 DEG C of vacuum drying 24h, it is then heated to 110 DEG C, after insulation 1h, it is down to room temperature, finally give the diamond/PMMA composite with three-dimensional network framing structure, the thermal conductivity of composite is 152W/mK, tensile strength 302MPa, and bending strength is 37MPa.
The thermal conductivity obtained from above example and mechanical performance data, alveolate texture prepared by the present invention strengthens the metal-base composites thermal conductivity along honeycomb wall direction, tensile strength, bending strength all obtains tremendous increase, thermal conductivity is up to 868W/mK, tensile strength is up to 578MPa, bending strength is up to 62MPa, composite prepared by the present invention defines continuous print quick conductive passage along alveolate texture direction, and axially there is better calorifics and mechanical property along honeycomb, the administration by different levels to heat can be realized to a certain extent, stock utilization is higher, combination property is apparently higher than the thermal conductivity of traditional Metal Substrate or polymer matrix composite.
Claims (12)
1. an alveolate texture reinforced composite, it is characterised in that described composite includes cellular reinforcement and matrix material, described matrix material is high-thermal conductive metal or polymer；Described cellular reinforcement is to be coated with highly heat-conductive material on cellular substrate, described highly heat-conductive material one in diamond film, graphene film, carbon nano-tube film, diamond/graphene film, diamond film/CNT, graphene film/CNT, diamond/graphene/carbon nano-tube film.
2. a kind of alveolate texture reinforced composite according to claim 1, it is characterized in that, when described matrix material is high-thermal conductive metal, matrix material one in metallic copper, aluminum, silver, copper alloy, aluminium alloy, silver alloy, in described copper alloy, aluminium alloy, silver alloy, copper, aluminum, silver-colored weight/mass percentage composition are be more than or equal to 50%；Polymeric matrix is thermoplastic polymer or thermosetting polymer；Described thermoplastic polymer one in polyethylene, polypropylene, polystyrene, polrvinyl chloride, politef, nylon, Merlon, polymethyl methacrylate, glycol ester, poly terephthalic acid, polyformaldehyde, polyamide, polysulfones；Described thermosetting polymer one in epoxy resin, phenolic resin, Lauxite, amino resins, melmac, unsaturated polyester resin, organic siliconresin, silicone rubber, expanded polystyrene (EPS), polyurethane.
3. a kind of alveolate texture reinforced composite according to claim 2, it is characterized in that, possibly together with high heat conduction particle in composite, described high heat conduction particle at least one in diamond particles, CNT, Graphene powder, graphene coated diamond particles, CNT cladding diamond granule.
4. a kind of alveolate texture reinforced composite according to claim 13, it is characterised in that in composite, the volume fraction of cellular reinforcement is 5 70%, and matrix material volume fraction is 30 95%, and high heat conduction particle volume fraction is 0 50%.
5. a kind of alveolate texture reinforced composite according to claim 1, it is characterized in that, one in the cellular backing material a kind of or acid bronze alloy, titanium-base alloy, molybdenum-base alloy in metallic copper, titanium, tungsten, molybdenum, chromium, nickel, in described acid bronze alloy, titanium-base alloy, molybdenum-base alloy, copper, titanium, molybdenum weight/mass percentage composition be more than or equal to 50%.
6. the cellular Heat Conduction Material reinforced composite of one according to claim 15 any one, it is characterised in that comprise at least one cellular reinforcement in composite.
7. a kind of alveolate texture reinforced composite according to claim 6, it is characterized in that, comprising multiple cellular reinforcement in composite, cellular reinforcement is lamellar or strip, described strip or the cellular reinforcement of lamellar in the form of an array with matrix material compound；Or described strip or the cellular reinforcement of lamellar are alternately stacked and matrix material compound；Cellular reinforcement in composite is identical or different.
8. a kind of alveolate texture reinforced composite according to claim 7, it is characterised in that in cellular reinforcement, is hexagonal honeycomb by cross section or rectangle honeycomb is arranged in order and constitutes.
9. a preparation method for alveolate texture reinforced composite, comprises the steps:
The first step: prepare cellular reinforcement
Alveolate texture substrate is cleaned, dries；Chemical vapour deposition (CVD) is adopted to deposit highly heat-conductive material at diamond surface；Highly heat-conductive material graphite, diamond, Graphene, CNT deposition process parameters be:
Graphene CVD deposition parameter is: it is 0.5-80% that carbonaceous gas accounts for all gas mass flow percentage ratio in stove；Growth 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 accounts for all gas mass flow percentage ratio in stove；Growth 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 accounts for all gas mass flow percentage ratio in stove；Growth temperature is 600-1000 DEG C, and growth air pressure is 103-104Pa；
By to applying plasma and induced by magnetic field in CVD deposition stove, and regulate carbon throughput, growth temperature, growth air pressure in real time, realizing the CVD deposition of highly heat-conductive material diamond/Graphene, diamond/carbon nanotube, diamond/graphene/carbon nano-tube film, deposition parameter is:
Graphene CVD deposition parameter is: it is 0.5-80% that carbonaceous gas accounts for all gas mass flow percentage ratio in stove；Growth temperature is 400-1200 DEG C, and growth air pressure is 5-105Pa；Plasma electric current density is 0-50mA/cm2；In deposition region, magnetic field intensity is 100 Gausses to 30 teslas；
CNT CVD deposition parameter is: it is 5-50% that carbonaceous gas accounts for all gas mass flow percentage ratio in stove；Growth temperature is 400-1300 DEG C, grows air pressure 103-105Pa；Plasma electric current density 0-30mA/cm2；In deposition region, magnetic field intensity is 100 Gausses to 30 teslas；
Diamond CVD deposition parameter is: it is 0.5-10% that carbonaceous gas accounts for all gas mass flow percentage ratio in stove；Growth 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 are carried out compound, obtains alveolate texture and strengthens Metal Substrate or polymer matrix composite；
Cellular reinforcement and metallic matrix compound tense, adopt a kind of technology in cold-rolled sintered, hot pressed sintering, plasma agglomeration, pressureless infiltration, pressure infiltration, casting to carry out compound；
Cellular reinforcement and polymeric matrix compound tense, adopt a kind of technology in dipping curing molding, injection moulding, compressing, rotation molding, injection mo(u)lding, extrusion moulding, laminated into type, flow casting molding to carry out compound.
10. the preparation method of a kind of alveolate texture reinforced composite according to claim 9, it is characterised in that: in the first step, after the cleaning of alveolate texture substrate, drying；First adopt a kind of method in plating, chemical plating, evaporation, magnetron sputtering, chemical vapour deposition (CVD), physical vapour deposition (PVD) to deposit the one in nickel, copper, tungsten, molybdenum, titanium, silver, chromium at substrate surface or after complex metal layer, then adopt chemical vapour deposition (CVD) highly heat-conductive material.
11. the preparation method of a kind of alveolate texture reinforced composite according to claim 10, it is characterized in that: after alveolate texture substrate surface prepares metal level, first it is soaked in nano-diamond powder or Graphene powder or carbon nanotube suspension and carries out ultrasonic vibration plantation seed crystal, then, chemical vapour deposition (CVD) highly heat-conductive material is adopted.
12. the preparation method of a kind of alveolate texture reinforced composite according to claim 9 11, it is characterized in that: cellular reinforcement and metallic matrix compound tense, first adopt the one in physical vapour deposition (PVD), chemical vapour deposition (CVD), chemical plating, plating, cellular reinforcement surface is deposited after one layer of transition zone again with metallic matrix compound, buffer layer material is selected from one or more in tungsten, molybdenum, titanium, nickel, chromium, or buffer layer material is selected from carbide TiC, WC, Cr7C3, NiC, Mo2One or more in C.
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