CN108587570A - Insulating phase-change heat conduction material and preparation method thereof - Google Patents
Insulating phase-change heat conduction material and preparation method thereof Download PDFInfo
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- CN108587570A CN108587570A CN201810246002.7A CN201810246002A CN108587570A CN 108587570 A CN108587570 A CN 108587570A CN 201810246002 A CN201810246002 A CN 201810246002A CN 108587570 A CN108587570 A CN 108587570A
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- boron nitride
- change heat
- conductive material
- heat conductive
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- 239000000463 material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 79
- 229910052582 BN Inorganic materials 0.000 claims abstract description 73
- 238000009413 insulation Methods 0.000 claims abstract description 39
- 239000000725 suspension Substances 0.000 claims abstract description 33
- 239000004020 conductor Substances 0.000 claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 14
- 229920000642 polymer Polymers 0.000 claims abstract description 12
- 239000012188 paraffin wax Substances 0.000 claims abstract description 9
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 8
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 8
- 239000003063 flame retardant Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 59
- 239000002071 nanotube Substances 0.000 claims description 46
- 239000000203 mixture Substances 0.000 claims description 24
- 235000019441 ethanol Nutrition 0.000 claims description 22
- 239000000945 filler Substances 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 238000012856 packing Methods 0.000 claims description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- 239000010439 graphite Substances 0.000 claims description 10
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims description 9
- WFXRJNDIBXZNJK-KVVVOXFISA-N azanium;(z)-octadec-9-enoate Chemical compound N.CCCCCCCC\C=C/CCCCCCCC(O)=O WFXRJNDIBXZNJK-KVVVOXFISA-N 0.000 claims description 9
- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 8
- 230000008018 melting Effects 0.000 claims description 8
- -1 acyl Imines Chemical class 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical group [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- XDVOLDOITVSJGL-UHFFFAOYSA-N 3,7-dihydroxy-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound O1B(O)OB2OB(O)OB1O2 XDVOLDOITVSJGL-UHFFFAOYSA-N 0.000 claims description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 3
- 229910021538 borax Inorganic materials 0.000 claims description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004327 boric acid Substances 0.000 claims description 3
- 229910052796 boron Inorganic materials 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 230000004048 modification Effects 0.000 claims description 3
- 238000012986 modification Methods 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 239000004328 sodium tetraborate Substances 0.000 claims description 3
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 229920000090 poly(aryl ether) Polymers 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 230000009467 reduction Effects 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 229920000570 polyether Polymers 0.000 claims 1
- 229920000573 polyethylene Polymers 0.000 claims 1
- 230000008859 change Effects 0.000 abstract description 19
- 238000002156 mixing Methods 0.000 abstract description 6
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract 1
- FVFJGQJXAWCHIE-UHFFFAOYSA-N [4-(bromomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CBr)C=C1 FVFJGQJXAWCHIE-UHFFFAOYSA-N 0.000 abstract 1
- 230000017525 heat dissipation Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 20
- 238000013019 agitation Methods 0.000 description 17
- 239000000047 product Substances 0.000 description 15
- 238000001816 cooling Methods 0.000 description 12
- 229920001903 high density polyethylene Polymers 0.000 description 12
- 239000004700 high-density polyethylene Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- 239000004697 Polyetherimide Substances 0.000 description 9
- 229920001601 polyetherimide Polymers 0.000 description 9
- 238000010792 warming Methods 0.000 description 8
- 230000009466 transformation Effects 0.000 description 7
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 6
- 230000004323 axial length Effects 0.000 description 6
- 229910052810 boron oxide Inorganic materials 0.000 description 6
- 238000000748 compression moulding Methods 0.000 description 6
- 230000007704 transition Effects 0.000 description 6
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 5
- 238000002604 ultrasonography Methods 0.000 description 5
- MOWNZPNSYMGTMD-UHFFFAOYSA-N oxidoboron Chemical class O=[B] MOWNZPNSYMGTMD-UHFFFAOYSA-N 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 206010037660 Pyrexia Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000012782 phase change material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/34—Waxes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/40—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes epoxy resins
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/42—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes polyesters; polyethers; polyacetals
- H01B3/427—Polyethers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/44—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the field of heat dissipation materials for electronic products, in particular to an insulating phase change heat conduction material and a preparation method thereof. The insulating phase-change heat-conducting material comprises a boron nitride suspension, paraffin, a polymer and an antioxidant, wherein the boron nitride suspension is prepared by mixing raw materials including ammonium oleate, a flame retardant and three-dimensional reticular expansion boron nitride. The three-dimensional mesh-shaped expanded boron nitride of the insulation phase-change heat conduction material is expanded boron nitride with a continuous three-dimensional mesh structure inside, provides a uniform and continuous heat conduction network for the whole heat conduction material, has better heat conduction performance compared with the use of common nanometer boron nitride powder, has excellent insulation performance, can be used in electronic products with higher insulation performance, and does not influence signals of the electronic products.
Description
Technical field
The present invention relates to electronic product radiating Material Fields, and in particular to a kind of insulation phase-change heat conductive material and its preparation side
Method.
Background technology
With the fast development of electronics technology and intelligent consumption electronic product, electronic product working efficiency is continuously improved, work(
Can be more and more stronger and stronger with performance, while the energy that its each component generates at work is also continuously improved, work
Temperature steeply rises, and the fever of product has become one of the problem of can not ignore, will be to the stability of electronic product, reliability
It causes to seriously threaten with service life.Heat is interpreted as the restrictive factor of electronic system progressive development.
Thermal interfacial material is a kind of material being commonly used to IC package and electronic radiation, and main function is to fill up two kinds of materials
The micropore and rough hole that surface generates when engagement or contact, reduce the impedance that heat is transmitted, and improve thermal diffusivity.Phase transformation
Heat Conduction Material is a kind of heat sink material better than common thermal interfacial material, utilizes phase change characteristics, can not only utmostly fill
Interface void reduces thermal resistance, and absorption and release by thinking change process heat, prevents device temperature moment from steeply rising,
Electronic device is protected, is prolonged the service life.
But the insulation performance of phase-change heat conductive material is poor, cannot expire in requiring insulation performance relatively high electronic device
Sufficient requirement, and because its electric conductivity can also weaken or shield the signal of electronic product, influence properties of product.Therefore, develop
Go out a kind of insulation phase-change heat conductive material, but existing insulation phase-change heat conductive material is by being formed using a variety of insulating polymers
Composite material, heat conductivility is poor, and the heat conductivility of material is greatly limited under the premise of realizing insulation performance.
Invention content
It is such exhausted technical problem to be solved by the invention is to provide a kind of insulation phase-change heat conductive material and preparation method thereof
Edge phase-change heat conductive material has more excellent heat conductivility relative to existing insulation phase-change heat conductive material, and ensures simultaneously excellent
Different insulating properties.
Used technical solution is to solve above-mentioned technical problem:
The present invention provides a kind of insulation phase-change heat conductive material, including boron nitride suspension, paraffin, polymer and antioxidant,
The boron nitride suspension is mixed to prepare by the raw material including oleic acid ammonia, fire retardant and three-dimensional netted expansion boron nitride, and described three
It is 20~120m that tie up netted expansion boron nitride, which be specific surface area,2/ g, the boron nitride powder that allowance for expansion is 100~220mL/g, institute
State boron nitride suspension:Paraffin:Polymer:The mass ratio of antioxidant is (1-5):(1-8):(1-7):(0.01-1).
Preferably, further include modified Nano tube packing, the modified Nano tube packing is by nanotube filler, Dopamine hydrochloride
It is made with silane coupling agent, solvent hybrid reaction, the modified Nano tube packing accounts for the quality of the insulation phase-change heat conductive material
Score is 5%-20%.It is preferred that a diameter of 5-100nm of nanotube filler, length is 50nm-1 μm.
Further, the silane coupling agent is KH570, KH550, KH560, KH570, at least one in A151, A171
Kind.
Further, the nanotube filler is alumina nano tube, silicon oxide nanotube, aluminum nitride nanometer pipe, nitridation
At least one of boron nanotube, zinc oxide nano mitron.
Preferably, the fire retardant is polyetherimide.
Preferably, the polymer is high density polyethylene (HDPE), epoxy resin, polyarylether resin, in polytetrafluoroethylene (PTFE) extremely
Few one kind.
The present invention also provides a kind of preparation method of above-mentioned insulation phase-change heat conductive material, include the following steps:
(1) boride and expanded graphite are scattered in solvent, are dried to obtain mixture A, mixture A is placed in heating dress
In setting, and logical nitrogen reduction, extra carbon is excluded, three-dimensional netted expansion boron nitride is obtained, by oleic acid ammonia, fire retardant, three dimensional network
Shape expansion boron nitride is dissolved in solvent, and is stirred, is separated by solid-liquid separation, and solid fraction is taken to be dissolved in formation boron nitride suspension in solvent;
(2) paraffin, polymer, the boron nitride suspension is taken to be mixed to form mixed solution, and heat melting, then
Antioxidant is added and forms product B;
(3) product B is molded and is cooled down, the insulation phase-change heat conductive material is made;
(4) optional step of modified Nano tube packing, the modified Nano are added in the mixed solution described in step (2)
Tube packing is added by nanotube filler, Dopamine hydrochloride, silane coupling agent in solvent, and heating stirring, then detach, wash,
It is obtained after drying.
Preferably, heating device described in step (1) is tube furnace, nitrogen flow rate 1000mL/min, tube furnace use
Gradient-heated mode.
Preferably, the boride be boron oxide, five amine borates, borax, boric acid, pyroboric acid, at least one of.
Preferably, the solvent be methanol, ethyl alcohol, polyethylene glycol and poly- propyl alcohol at least one of.
Beneficial effects of the present invention are:
(1) the covert Heat Conduction Material of insulation of the present invention includes mixing boron nitride suspension, paraffin, polymer and antioxidant
It closes and is made, the three-dimensional netted expansion boron nitride in boron nitride suspension, which is a kind of inside, has the swollen of continuous tridimensional network
Swollen boron nitride, the heat conduction network of uniformly continuous is provided for entirety Heat Conduction Material, and comparison uses common nm-class boron nitride powder
End has better heat conductivility.
(2) using polymer and paraffin as matrix, it ensure that material has good insulating properties, can use to insulation
In the higher electronic product of performance, and the signal of electronic product will not be had an impact.And it can realize that good phase transformation is special
Property, utmostly filling interface gap, reduces thermal resistance.
Specific implementation mode
To make those skilled in the art be better understood from technical scheme of the present invention, below to insulation phase transformation of the present invention
Heat Conduction Material and preparation method thereof elaborates.
Embodiment 1
S1. three-dimensional netted expansion boron nitride is prepared:
It takes 5g boron oxides, 1g expanded graphites to be dissolved in 75ml methanol solutions, carries out magnetic agitation and mix 1h, it will be viscous after stirring
Thick mixed liquor is placed in oven and dried, and temperature is 90 DEG C, obtains the mixture B of boride and expanded graphite, the mixing that will be obtained
Object B is laid in graphite crucible, and is put into tube furnace, and under 100mL/min N2 flow velocitys, tube furnace is with the speed of 10 DEG C/min
Rate is warming up to 400 DEG C and keeps the temperature 1h, is warming up to 800 DEG C with the rate of 5 DEG C/min and keeps the temperature 2h, the rate of 5 DEG C/min is heated to
Room temperature is cooled to the furnace after 1400 DEG C of heat preservation 2.5h.After the completion of reaction, obtained product is placed in Muffle furnace, in 750 DEG C
5h is kept the temperature to exclude extra carbon, finally obtains the white powder that specific surface area is 81m2/g, allowance for expansion is 193mL/g expansions
I.e. three-dimensional netted expansion boron nitride.
S2. boron nitride suspension is prepared:
The polyetherimide solution of the oleic acid ammonia solution of 2wt% and 2wt% is mixed, is dissolved in ethanol solution, and
The three-dimensional netted expansion boron nitride powders of 40g, magnetic agitation 30min, rear ultrasonic disperse 2h is added, centrifuge is separated by solid-liquid separation,
It takes solid fraction that ethyl alcohol is added and obtains boron nitride suspension.
S3. take 45 DEG C of the phase transition temperature of 100 mass parts, latent heat of phase change 240J/g phase change paraffins that 100 mass are added after melting
The above-mentioned boron nitride suspension of part, the magnetic agitation 2h at 70 DEG C, the high density polyethylene (HDPE) that 100 mass parts are then added are placed on
In vacuum mixer, under 110Pa vacuum degrees, 300rpm rotating speeds, heating stirring 2h forms mixture under temperature 70 C.It will be described
Mixture melts stirring at 150 DEG C, and the antioxidant 1010 of 1 mass parts is added, and persistently stirs 1h and is placed in mold, applies about
The pressure of 10kpa, compression moulding, natural cooling cooling, demoulding obtain insulation phase-change heat conductive material.
Polyetherimide has very strong high-temperature stability, even the polyetherimide of non-reinforcing type, still has fine
Toughness and intensity.Therefore it can be provided preferably for three-dimensional netted expansion boron nitride using the superior thermal stability of polyetherimide
Heat conductivility, meanwhile, make it have excellent mechanical performance, electrical insulation capability, radiation-resistant property, high-low temperature resistant and wearability
Can, and microwaves.The present embodiment prepares the boride used in the step of three-dimensional netted expansion boron nitride and uses boron oxide,
It is that boron source prepares expansion boron nitride that five amine borates, borax, boric acid, pyroboric acid, which can also actually be selected,.
Embodiment 2
S1. three-dimensional netted expansion boron nitride is prepared:
It takes 5g boron oxides, 1g expanded graphites to be dissolved in 75ml methanol solutions, carries out magnetic agitation and mix 1h, it will be viscous after stirring
Thick mixed liquor is placed in oven and dried, and temperature is 90 DEG C, obtains the mixture B of boride and expanded graphite, the mixing that will be obtained
Object B is laid in graphite crucible, and is put into tube furnace, and under 100mL/min N2 flow velocitys, tube furnace is with the speed of 10 DEG C/min
Rate is warming up to 400 DEG C and keeps the temperature 1h, is warming up to 800 DEG C with the rate of 5 DEG C/min and keeps the temperature 2h, the rate of 5 DEG C/min is heated to
Room temperature is cooled to the furnace after 1400 DEG C of heat preservation 2.5h.After the completion of reaction, obtained product is placed in Muffle furnace, in 750 DEG C
5h is kept the temperature to exclude extra carbon, finally obtains the white powder that specific surface area is 81m2/g, allowance for expansion is 193mL/g expansions
I.e. three-dimensional netted expansion boron nitride.
S2. boron nitride suspension is prepared:
The polyetherimide solution of the oleic acid ammonia solution of 2wt% and 2wt% is mixed, is dissolved in ethanol solution, and
The three-dimensional netted expansion boron nitride powders of 40g, magnetic agitation 30min, rear ultrasonic disperse 2h is added, centrifuge is separated by solid-liquid separation,
It takes solid fraction that ethyl alcohol is added and obtains boron nitride suspension.
S3. modified Nano tube packing is prepared:
The a diameter of 30-40nm of 20g are weighed, axial length is the boron nitride nano-tube of 100nm, and dispersion is in ethanol, ultrasonic
30min Dopamine hydrochloride is added in ethanol solution, at room temperature ultrasound 2h.After KH570 is added, continue under the conditions of 60 DEG C
2h is reacted, reaction terminates to centrifuge modified nanotube filler, wash, dry, obtains modified boron nitride nano-tube
Filler;
S4. take 45 DEG C of the phase transition temperature of 100 mass parts, latent heat of phase change 240J/g phase change paraffins that 100 mass are added after melting
The modified Nano tube packing of the above-mentioned boron nitride suspension and 75 mass parts of part, magnetic agitation 2h, is then added 100 at 70 DEG C
The high density polyethylene (HDPE) of mass parts is placed in vacuum mixer, under 110Pa vacuum degrees, 300rpm rotating speeds, under temperature 70 C
Heating stirring 2h forms mixture.The mixture is melted to stirring at 150 DEG C, the antioxidant 1010 of 1 mass parts is added, holds
Continuous stirring 1h is placed in mold, applies the pressure of about 10kpa, compression moulding, and natural cooling cooling demoulds and obtains insulation phase transformation
Heat Conduction Material.
It is the nanotube filler of 100nm that a diameter of 30-40nm, axial length are selected in the present invention, can be with described three
Netted expansion boron nitride cooperation is tieed up, to improve the heat transfer efficiency of material, increased thermal conductivity energy.
Embodiment 3
S1. three-dimensional netted expansion boron nitride is prepared:
It takes 5g boron oxides, 1g expanded graphites to be dissolved in 75ml methanol solutions, carries out magnetic agitation and mix 1h, it will be viscous after stirring
Thick mixed liquor is placed in oven and dried, and temperature is 90 DEG C, obtains the mixture B of boride and expanded graphite, the mixing that will be obtained
Object B is laid in graphite crucible, and is put into tube furnace, and under 100mL/min N2 flow velocitys, tube furnace is with the speed of 10 DEG C/min
Rate is warming up to 400 DEG C and keeps the temperature 1h, is warming up to 800 DEG C with the rate of 5 DEG C/min and keeps the temperature 2h, the rate of 5 DEG C/min is heated to
Room temperature is cooled to the furnace after 1400 DEG C of heat preservation 2.5h.After the completion of reaction, obtained product is placed in Muffle furnace, in 750 DEG C
5h is kept the temperature to exclude extra carbon, finally obtains the white powder that specific surface area is 81m2/g, allowance for expansion is 193mL/g expansions
I.e. three-dimensional netted expansion boron nitride.
S2. boron nitride suspension is prepared:
The polyetherimide solution of the oleic acid ammonia solution of 2wt% and 2wt% is mixed, is dissolved in ethanol solution, and
The three-dimensional netted expansion boron nitride powders of 50g, magnetic agitation 30min, rear ultrasonic disperse 2h is added, centrifuge is separated by solid-liquid separation,
It takes solid fraction that ethyl alcohol is added and obtains boron nitride suspension.
S3. modified Nano tube packing is prepared:
The a diameter of 30-40nm of 10g are weighed, axial length is the aluminum nitride nanometer pipe of 120nm, and dispersion is in ethanol, ultrasonic
30min Dopamine hydrochloride is added in ethanol solution, at room temperature ultrasound 2h.After KH570 is added, continue under the conditions of 60 DEG C
2h is reacted, reaction terminates to centrifuge modified nanotube filler, wash, dry, obtains modified boron nitride nano-tube
Filler;
S4. take 45 DEG C of the phase transition temperature of 80 mass parts, latent heat of phase change 240J/g phase change paraffins that 50 mass parts are added after melting
Above-mentioned boron nitride suspension and 11 mass parts modified Nano tube packing, then 70 matter are added in the magnetic agitation 2h at 70 DEG C
The high density polyethylene (HDPE) of amount part is placed in vacuum mixer, under 110Pa vacuum degrees, 300rpm rotating speeds, under temperature 70 C plus
Thermal agitation 2h forms mixture.The mixture is melted to stirring at 150 DEG C, the antioxidant 1010 of 10 mass parts is added, holds
Continuous stirring 1h is placed in mold, applies the pressure of about 10kpa, compression moulding, and natural cooling cooling demoulds and obtains insulation phase transformation
Heat Conduction Material.
Embodiment 4
S1. three-dimensional netted expansion boron nitride is prepared:
It takes 5g boron oxides, 1g expanded graphites to be dissolved in 75ml methanol solutions, carries out magnetic agitation and mix 1h, it will be viscous after stirring
Thick mixed liquor is placed in oven and dried, and temperature is 90 DEG C, obtains the mixture B of boride and expanded graphite, the mixing that will be obtained
Object B is laid in graphite crucible, and is put into tube furnace, and under 100mL/min N2 flow velocitys, tube furnace is with the speed of 10 DEG C/min
Rate is warming up to 400 DEG C and keeps the temperature 1h, is warming up to 800 DEG C with the rate of 5 DEG C/min and keeps the temperature 2h, the rate of 5 DEG C/min is heated to
Room temperature is cooled to the furnace after 1400 DEG C of heat preservation 2.5h.After the completion of reaction, obtained product is placed in Muffle furnace, in 750 DEG C
5h is kept the temperature to exclude extra carbon, finally obtains the white powder that specific surface area is 81m2/g, allowance for expansion is 193mL/g expansions
I.e. three-dimensional netted expansion boron nitride.
S2. boron nitride suspension is prepared:
The polyetherimide solution of the oleic acid ammonia solution of 2wt% and 2wt% is mixed, is dissolved in ethanol solution, and
The three-dimensional netted expansion boron nitride powders of 50g, magnetic agitation 30min, rear ultrasonic disperse 2h is added, centrifuge is separated by solid-liquid separation,
It takes solid fraction that ethyl alcohol is added and obtains boron nitride suspension.
S3. modified Nano tube packing is prepared:
The a diameter of 30-40nm of 10g are weighed, axial length is the aluminum nitride nanometer pipe of 120nm, and dispersion is in ethanol, ultrasonic
30min Dopamine hydrochloride is added in ethanol solution, at room temperature ultrasound 2h.After KH570 is added, continue under the conditions of 60 DEG C
2h is reacted, reaction terminates to centrifuge modified nanotube filler, wash, dry, obtains modified boron nitride nano-tube
Filler;
S4. take 45 DEG C of the phase transition temperature of 80 mass parts, latent heat of phase change 240J/g phase change paraffins that 50 mass parts are added after melting
Above-mentioned boron nitride suspension and 11 mass parts modified Nano tube packing, then 70 matter are added in the magnetic agitation 2h at 70 DEG C
The epoxy resin of amount part is placed in vacuum mixer, and under 110Pa vacuum degrees, 300rpm rotating speeds are heated under temperature 70 C and stirred
It mixes 2h and forms mixture.The mixture is melted to stirring at 150 DEG C, the antioxidant 1010 of 10 mass parts is added, persistently stirs
It mixes 1h to be placed in mold, applies the pressure of about 10kpa, compression moulding, natural cooling cooling demoulds and obtains insulation heat conduction with phase change
Material.
Comparative example 1
S1. platelet boron nitride suspension is prepared:
The polyetherimide solution of the oleic acid ammonia solution of 2wt% and 2wt% is mixed, is dissolved in ethanol solution, and
It is 1-10 μm of platelet boron nitride powder that 50g grain sizes, which are added, magnetic agitation 30min, rear ultrasonic disperse 2h, and centrifuge carries out solid-liquid
Separation takes solid fraction that ethyl alcohol is added and obtains platelet boron nitride suspension.
S2. modified Nano tube packing is prepared:
The a diameter of 30-40nm of 10g are weighed, axial length is the aluminum nitride nanometer pipe of 120nm, and dispersion is in ethanol, ultrasonic
30min Dopamine hydrochloride is added in ethanol solution, at room temperature ultrasound 2h.After KH570 is added, continue under the conditions of 60 DEG C
2h is reacted, reaction terminates to centrifuge modified nanotube filler, wash, dry, obtains modified boron nitride nano-tube
Filler;
S3. take 45 DEG C of the phase transition temperature of 80 mass parts, latent heat of phase change 240J/g phase change paraffins that 50 mass parts are added after melting
Above-mentioned boron nitride suspension and 11 mass parts modified Nano tube packing, then 70 matter are added in the magnetic agitation 2h at 70 DEG C
The high density polyethylene (HDPE) of amount part is placed in vacuum mixer, under 110Pa vacuum degrees, 300rpm rotating speeds, under temperature 70 C plus
Thermal agitation 2h forms mixture.The mixture is melted to stirring at 150 DEG C, the antioxidant 1010 of 10 mass parts is added, holds
Continuous stirring 1h is placed in mold, applies the pressure of about 10kpa, compression moulding, and natural cooling cooling demoulds and obtains insulation phase transformation
Heat Conduction Material.
Comparative example 2
S1. modified Nano tube packing is prepared:
The a diameter of 30-40nm of 20g are weighed, axial length is the boron nitride nano-tube of 100nm, and dispersion is in ethanol, ultrasonic
30min Dopamine hydrochloride is added in ethanol solution, at room temperature ultrasound 2h.After KH570 is added, continue under the conditions of 60 DEG C
2h is reacted, reaction terminates to centrifuge modified nanotube filler, wash, dry, obtains modified boron nitride nano-tube
Filler;
S2. take 45 DEG C of the phase transition temperature of 100 mass parts, latent heat of phase change 240J/g phase change paraffins that 100 mass are added after melting
The modified Nano tube packing of the above-mentioned boron nitride suspension and 75 mass parts of part, magnetic agitation 2h, is then added 100 at 70 DEG C
The high density polyethylene (HDPE) of mass parts is placed in vacuum mixer, under 110Pa vacuum degrees, 300rpm rotating speeds, under temperature 70 C
Heating stirring 2h forms mixture.The mixture is melted to stirring at 150 DEG C, the antioxidant 1010 of 1 mass parts is added, holds
Continuous stirring 1h is placed in mold, applies the pressure of about 10kpa, compression moulding, and natural cooling cooling demoulds and obtains insulation phase transformation
Heat Conduction Material.It is right
Embodiment 1-4 and comparative example 1-2 insulation phase-change heat conductive materials obtained are tested for the property, and measure its heat conduction system
Number, latent heat of phase change and breakdown voltage, the results are shown in Table 1.
It the thermal coefficients of table 1 embodiment 1-4 and comparative example 1-2 insulation phase-change heat conductive materials obtained, latent heat of phase change and hits
Wear voltage
Each embodiment and comparative example can be compared and analyzed by 1 data of table.By embodiment 1, embodiment 2 and comparative example 2
It is compared, it is known that, embodiment 1 only adds boron nitride suspension, and comparative example 1 only adds nanotube filler, and embodiment 2
Boron nitride suspension and nanotube filler are added jointly, embodiment 2 all has higher relative to embodiment 1 and comparative example 2
Thermal coefficient and latent heat of phase change, heat conductivility are more excellent.It follows that a diameter of 30-40nm is selected in the present invention, it is axial long
Degree is the nanotube filler of 100nm, can be coordinated with the three-dimensional netted expansion boron nitride, and the heat conduction to improve material is imitated
Rate, increased thermal conductivity energy.Embodiment 3 and comparative example 1 are compared, it is known that, it is outstanding that comparative example 1 has used platelet boron nitride to prepare
Supernatant liquid is to be made final product, and embodiment 3 prepares boron nitride suspension under the premise of other reaction conditions and constant component
For liquid to which final product be made, the thermal coefficient and latent heat of phase change of embodiment 3 are above comparative example 1, therefore, three-dimensional netted expansion
Boron nitride provides the heat conduction network of uniformly continuous for whole Heat Conduction Material, and comparison is had using common nano boron nitride powder
Better heat conductivility can greatly improve the heat conductivility of insulation phase-change heat conductive material.
The better embodiment of the present invention is illustrated above, but the present invention is not limited to the embodiment,
Those skilled in the art can also make various equivalent modifications or replacement under the premise of without prejudice to spirit of that invention, this
Equivalent modification or replacement are all contained in the application claim limited range a bit.
Claims (10)
1. a kind of insulation phase-change heat conductive material, which is characterized in that including boron nitride suspension, paraffin, polymer and antioxidant, institute
It states boron nitride suspension to be mixed to prepare by the raw material including oleic acid ammonia, fire retardant and three-dimensional netted expansion boron nitride, the three-dimensional
It is 20~120m that netted expansion boron nitride, which is specific surface area,2/ g, the boron nitride powder that allowance for expansion is 100~220mL/g, it is described
Boron nitride suspension:Paraffin:Polymer:The mass ratio of antioxidant is (1-5):(1-8):(1-7):(0.01-1).
2. insulation phase-change heat conductive material as described in claim 1, which is characterized in that further include modified Nano tube packing, it is described
Modified Nano tube packing is made by nanotube filler, Dopamine hydrochloride and silane coupling agent, solvent hybrid reaction, and the modification is received
The mass fraction that mitron filler accounts for the insulation phase-change heat conductive material is 5%-20%.
3. as claimed in claim 2 insulation phase-change heat conductive material, which is characterized in that the silane coupling agent be KH570,
At least one of KH550, KH560, KH570, A151, A171.
4. a kind of insulation phase-change heat conductive material as claimed in claim 2, which is characterized in that the nanotube filler is aluminium oxide
At least one of nanotube, silicon oxide nanotube, aluminum nitride nanometer pipe, boron nitride nano-tube, zinc oxide nano mitron.
5. insulation phase-change heat conductive material according to any one of claims 1-4, which is characterized in that the fire retardant is polyethers acyl
Imines.
6. a kind of insulation phase-change heat conductive material according to any one of claims 1-4, which is characterized in that the polymer is height
Density polyethylene, epoxy resin, polyarylether resin, at least one of polytetrafluoroethylene (PTFE).
The preparation method of phase-change heat conductive material 7. claim 1-6 any one of them insulate, which is characterized in that including following step
Suddenly:
(1) it takes boride and expanded graphite to be scattered in solvent, is dried to obtain mixture A, mixture A is placed in heating device
In, and logical nitrogen reduction excludes extra carbon, obtains three-dimensional netted expansion boron nitride, by oleic acid ammonia, fire retardant, three-dimensional netted
Expansion boron nitride is dissolved in solvent, and is stirred, is separated by solid-liquid separation, and solid fraction is taken to be dissolved in formation boron nitride suspension in solvent;
(2) it takes paraffin, polymer, the boron nitride suspension to be mixed to form mixed solution, and heat melting, is then added
Antioxidant forms product B;
(3) product B is molded and is cooled down, the insulation phase-change heat conductive material is made;
(4) optional step of modified Nano tube packing is added in the mixed solution described in step (2), the modified Nano pipe is filled out
Material is added by nanotube filler, Dopamine hydrochloride, silane coupling agent in solvent, and heating stirring, is then detached, is washed, is dry
After obtain.
8. the preparation method of insulation phase-change heat conductive material as claimed in claim 7, which is characterized in that add described in step (1)
Hot charging is set to tube furnace, nitrogen flow rate 1000mL/min, and tube furnace uses gradient-heated mode.
9. the preparation method of insulation phase-change heat conductive material as claimed in claim 7, which is characterized in that the boride is oxidation
At least one of boron, five amine borates, borax, boric acid, pyroboric acid.
10. as claimed in claim 7 insulation phase-change heat conductive material preparation method, which is characterized in that the solvent be methanol,
At least one of in ethyl alcohol, polyethylene glycol and poly- propyl alcohol.
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