CN108819360A - A kind of graphene heat conducting film/heat conductive silica gel film composite material of stratiform alternating structure and preparation method thereof - Google Patents
A kind of graphene heat conducting film/heat conductive silica gel film composite material of stratiform alternating structure and preparation method thereof Download PDFInfo
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- CN108819360A CN108819360A CN201810365178.4A CN201810365178A CN108819360A CN 108819360 A CN108819360 A CN 108819360A CN 201810365178 A CN201810365178 A CN 201810365178A CN 108819360 A CN108819360 A CN 108819360A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 133
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 115
- 239000002131 composite material Substances 0.000 title claims abstract description 69
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 239000000741 silica gel Substances 0.000 title claims abstract description 66
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 66
- 108010025899 gelatin film Proteins 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000003292 glue Substances 0.000 claims abstract description 23
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 23
- 239000010703 silicon Substances 0.000 claims abstract description 23
- 239000001913 cellulose Substances 0.000 claims abstract description 18
- 229920002678 cellulose Polymers 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 49
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 43
- 239000000243 solution Substances 0.000 claims description 28
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 20
- 229910000077 silane Inorganic materials 0.000 claims description 20
- 239000011259 mixed solution Substances 0.000 claims description 15
- 239000003638 chemical reducing agent Substances 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 14
- 229960004756 ethanol Drugs 0.000 claims description 11
- 239000000835 fiber Substances 0.000 claims description 11
- 239000012065 filter cake Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 8
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 6
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 6
- 229920002554 vinyl polymer Polymers 0.000 claims description 6
- 150000001336 alkenes Chemical class 0.000 claims description 5
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 230000004048 modification Effects 0.000 claims description 4
- 238000012986 modification Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 238000007711 solidification Methods 0.000 claims description 4
- 230000008023 solidification Effects 0.000 claims description 4
- 229910017083 AlN Inorganic materials 0.000 claims description 3
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 3
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 3
- 229930003268 Vitamin C Natural products 0.000 claims description 3
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 3
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 3
- 229940071870 hydroiodic acid Drugs 0.000 claims description 3
- 235000019154 vitamin C Nutrition 0.000 claims description 3
- 239000011718 vitamin C Substances 0.000 claims description 3
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 2
- 229910052582 BN Inorganic materials 0.000 claims description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 239000002041 carbon nanotube Substances 0.000 claims description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 2
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- 239000012279 sodium borohydride Substances 0.000 claims description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 2
- 239000004575 stone Substances 0.000 claims description 2
- KBQVDAIIQCXKPI-UHFFFAOYSA-N 3-trimethoxysilylpropyl prop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C=C KBQVDAIIQCXKPI-UHFFFAOYSA-N 0.000 claims 1
- 239000005977 Ethylene Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 claims 1
- 239000000945 filler Substances 0.000 claims 1
- -1 silicane alkane Chemical class 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 10
- 239000006185 dispersion Substances 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 6
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 9
- 230000017525 heat dissipation Effects 0.000 description 7
- 238000006722 reduction reaction Methods 0.000 description 6
- 229920002379 silicone rubber Polymers 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000002121 nanofiber Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 description 2
- 238000011946 reduction process Methods 0.000 description 2
- 239000004945 silicone rubber Substances 0.000 description 2
- 230000001360 synchronised effect Effects 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- XLVKXZZJSTWDJY-UHFFFAOYSA-N [SiH4].[Si] Chemical compound [SiH4].[Si] XLVKXZZJSTWDJY-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/005—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
- B32B9/007—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile comprising carbon, e.g. graphite, composite carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B3/00—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form
- B32B3/26—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids ; characterised by an apertured layer
- B32B3/266—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids ; characterised by an apertured layer characterised by an apertured layer, the apertures going through the whole thickness of the layer, e.g. expanded metal, perforated layer, slit layer regular cells B32B3/12
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/02—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by a sequence of laminating steps, e.g. by adding new layers at consecutive laminating stations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/16—Drying; Softening; Cleaning
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
- B32B2307/202—Conductive
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
- B32B2307/206—Insulating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/302—Conductive
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/50—Properties of the layers or laminate having particular mechanical properties
- B32B2307/582—Tearability
- B32B2307/5825—Tear resistant
Landscapes
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Carbon And Carbon Compounds (AREA)
- Cooling Or The Like Of Semiconductors Or Solid State Devices (AREA)
Abstract
A kind of graphene heat conducting film/heat conductive silica gel film composite material of stratiform alternating structure and preparation method thereof, it is related to a kind of graphene/heat conductive silica gel composite material and preparation method.The present invention is to solve the graphene dispersion in existing graphene/heat conductive silica gel composite material is difficult, it is difficult to the technical issues of forming the thermal conducting path of steady and continuous.Composite material of the invention is made of graphene heat conducting film and thermal conductive silicon glue film, and graphene heat conducting film and thermal conductive silicon glue film are alternately arranged.Preparation method of the invention：One, graphene heat conducting film is prepared；Two, heat conductive silica gel is prepared；Three, graphene heat conducting film/heat conductive silica gel film composite material of stratiform alternating structure is prepared.The present invention prepares graphene heat conducting film using nano-cellulose and the compound method of graphene, graphene/heat conductive silica gel film composite material that stratiform alternating structure is formed using interface tech composite heat-conducting pellosil, meets the needs of fields such as Aeronautics and Astronautics, electric are to High-performance heat conduction material.
Description
Technical field
The present invention relates to a kind of graphene/heat conductive silica gel composite material and preparation methods.
Background technique
In recent years, with the development of economy with the progress of technology, requirement of the people to high-performance heat-conducting elastomer is increasingly
Height, such as：The sealed product of High performance electronics requires have excellent heat dissipation and insulation effect, moisture-proof dust-proof and earthquake-proof again；
Chemical industry production and the fields such as wastewater treatment require the material of heat exchange device to possess good thermally conductive, high temperature resistant and resistance to simultaneously
The performances such as chemical attack；Section components in automobile engine are up to 205 DEG C using temperature, and general purpose rubber is difficult to bear.It is thermally conductive
Silicon rubber have excellent heat dissipation, damping, chemical corrosion resistance and it is wider use temperature (- 90~250 DEG C), can in the limit and
In harsh environment keep elasticity and stability in use, be very suitable to the industries such as electronics, electric appliance, automobile and instrument elastic adhesive,
Positioning, heat dissipation, insulation and sealing use, thus are concerned in Heat Conduction Material using field.
Currently, having had already appeared the related technology of preparing of some heat-conducting silicone rubber pads or composite material both at home and abroad.
CN106280050A discloses a kind of heat-conductive composite material and preparation method thereof, and using resin as middle layer, silicone rubber pad is made
For outer layer, but composite flexibility is poor, and thermal conductivity is lower.CN106832961A discloses a kind of graphene silicon rubber heat conductive pad
Piece and preparation method thereof is prepared thermally conductive carbon film on sheet metal using chemical vapor deposition, then is dissolved sheet metal with concentrated acid, shape
At heat conductive intermediate layer, preparation process is difficult, limits large-scale production and application.
Graphene has excellent heating conduction and high-specific surface area, is the ideal heat sink material of electronic device.Graphene
There are problems, such as difficulties in dispersion in the practical application for solving heat dissipation problem, it is difficult to form the thermal conducting path of steady and continuous.
Summary of the invention
The present invention is to solve the graphene dispersion in existing graphene/heat conductive silica gel composite material is difficult, it is difficult to shape
At steady and continuous thermal conducting path the technical issues of, and provide a kind of graphene heat conducting film/heat conductive silica gel of stratiform alternating structure
Film composite material and preparation method thereof.
Graphene heat conducting film/heat conductive silica gel film composite material of stratiform alternating structure of the invention is by graphene heat conducting film
It is formed with thermal conductive silicon glue film, the graphene heat conducting film and thermal conductive silicon glue film are alternately arranged；The thickness of the thermal conductive silicon glue film
Degree is 0.1mm~10mm.
Graphene heat conducting film/heat conductive silica gel film composite material preparation method of stratiform alternating structure of the invention be by with
What lower step carried out：
One, graphene heat conducting film is prepared：Using high-speed mixer by graphene oxide water solution, reducing agent and nanofiber
Plain uniformly mixing 5min~10min, is then sonicated 20min~60min, then quiet under conditions of temperature is 60 DEG C~90 DEG C
Reduction reaction 2h~6h is set, is filtered on composite fibre miillpore filter, with second alcohol and water, alternately washing filter cake to filtrate is neutrality,
Filter cake is 80 DEG C~120 DEG C dry 2h~6h in temperature after washing, and composite fibre miillpore filter and filter cake are removed, graphite is obtained
Alkene heat conducting film；
The concentration of the graphene oxide water solution is 0.1mg/mL~10mg/mL, and the graphene oxide is water-soluble
Graphene oxide in liquid with a thickness of 1nm~20nm；
The diameter of the nano-cellulose is 2nm~20nm, and length is 1 μm~5 μm；
Graphene oxide, reducing agent and nano-cellulose in the graphene oxide water solution press the group of mass fraction
At as follows：Graphene oxide in graphene oxide water solution is 100 parts, and nano-cellulose is 5 parts~25 parts, reducing agent 10
Part~100 parts；
Two, heat conductive silica gel is prepared：
1, modified heat filling：The dehydrated alcohol mixed solution and heat filling of silane coupling agent I are added to high speed together
1min~15min is mixed in mixing machine, then dry 2h~6h under conditions of temperature is 80 DEG C~120 DEG C, obtains modification
Heat filling；Silane coupling agent I and the volume ratio of dehydrated alcohol are in the dehydrated alcohol mixed solution of the silane coupling agent I
1:(2~10)；The quality of silane coupling agent I and heat filling in the dehydrated alcohol mixed solution of the silane coupling agent I
Than for (1~5):100；
2, using vacuum machine blender by two-component liquid silica gel and modified heat filling mixing 10min~60min,
Obtain heat conductive silica gel；The mass ratio of the two-component liquid silica gel and modified heat filling is 1:(3~10)；Described is double
The viscosity of component liquid silica gel is 50cP~1000cP；
Three, graphene heat conducting film/heat conductive silica gel film composite material of stratiform alternating structure is prepared：
1, the silane surface of graphene heat conducting film is modified：Graphene heat conducting film is immersed to the ethanol solution of silane coupling agent II
In be standing and soaking 2min~20min, then dry 0.5h~2h under conditions of temperature is 60 DEG C~90 DEG C, obtains silane surface
Modified graphene heat conducting film；The volume of silane coupling agent II and dehydrated alcohol in the ethanol solution of the silane coupling agent II
Than being 1:(1~5)；
2, heat conductive silica gel is spread using heat conductive silica gel and silane surface modified graphene heat conducting film alternately arranged mode
Open up in the surface of the modified graphene heat conducting film of silane surface, suppressed and formed a film with calender, then solidification temperature be 80 DEG C~
Solidify 5min~120min under conditions of 150 DEG C, obtains graphene heat conducting film/thermal conductive silicon glue film composite wood of stratiform alternating structure
Material；In the graphene of the stratiform alternating structure/heat conductive silica gel film composite material thermal conductive silicon glue film with a thickness of 0.1mm~
10mm。
The present invention replaces composite construction with thermal conductive silicon glue film using graphene heat conducting film and obtains multilayered thermally-conductive composite material,
Two kinds of membrane materials are combined by interface modification with being crosslinked, solves a layer interface resistance for structure heat-conductive composite material
The problem of with boundary strength, has effectively played the graphene high-efficiency capacity of heat transmission, realizes efficient uniform heat dissipation, takes full advantage of and lead
The characteristic of hot material silica gel composite realizes the regulation of heat-conductive composite material electric conductivity and adhesive property.With graphene/nanometer
Cellulose is layer skeleton, improves the tear resistance and mechanical property of heat conducting film.Pass through the structure of multilayered thermally-conductive composite material
Design, obtains the heat-conductive composite material of the multifunctional alls such as enhancing, high-efficiency heat conduction, tear-proof, conduction, insulation, bonding, energy
Enough meet the needs of fields such as electric and electronic, new energy are to thermal interfacial material, heat-conducting insulation material, heat-conductive composite material etc..
Graphene heat conducting film/heat conductive silica gel film composite material of stratiform alternating structure provided by the present invention has green ring
The excellent feature of guarantor, simple process, good heat conductivity, mechanical performance.
The present invention prepares graphene heat conducting film using nano-cellulose and the compound method of graphene, and utilizes interface tech
Composite heat-conducting pellosil forms graphene heat conducting film/heat conductive silica gel film composite material of stratiform alternating structure, meets aviation, boat
It, the demand of the fields to High-performance heat conduction material such as electric.
The invention has the advantages that：
1, the present invention provides the preparation method of stratiform heat-conductive composite material, is handed over using graphene heat conducting film and thermal conductive silicon glue film
For the mode of arrangement, it is capable of forming multilayered structure, the specific number of plies does not limit, and can decide in its sole discretion according to actual needs；
2, the present invention utilizes the heating conduction of the adjustable laminar composite of multilayered structure, passes through graphene heat conducting film
Effect can quickly spread the heat that local height is concentrated, and improve the uniformity and radiating efficiency of heat dissipation；
3, the present invention solves the dispersion of graphene using nano-cellulose, using dispersion progress synchronous with reduction
Method avoids the reunion of graphene in reduction process.
Detailed description of the invention
Fig. 1 is the graphene heat conducting film/heat conductive silica gel composite material schematic diagram for testing the stratiform alternating structure of a preparation.
Specific embodiment
Specific embodiment one：Present embodiment is a kind of graphene heat conducting film/thermal conductive silicon glue film of stratiform alternating structure
Composite material is specifically made of graphene heat conducting film and thermal conductive silicon glue film, the graphene heat conducting film and thermal conductive silicon glue film
It is alternately arranged；The thermal conductive silicon glue film with a thickness of 0.1mm~10mm.
Specific embodiment two：Present embodiment is that the graphene of one laminate alternating structure of specific embodiment is thermally conductive
Film/heat conductive silica gel film composite material preparation method, specifically carries out according to the following steps：：
One, graphene heat conducting film is prepared：Using high-speed mixer by graphene oxide water solution, reducing agent and nanofiber
Plain uniformly mixing 5min~10min, is then sonicated 20min~60min, then quiet under conditions of temperature is 60 DEG C~90 DEG C
Reduction reaction 2h~6h is set, is filtered on composite fibre miillpore filter, with second alcohol and water, alternately washing filter cake to filtrate is neutrality,
Filter cake is 80 DEG C~120 DEG C dry 2h~6h in temperature after washing, and composite fibre miillpore filter and filter cake are removed, graphite is obtained
Alkene heat conducting film；
The concentration of the graphene oxide water solution is 0.1mg/mL~10mg/mL, and the graphene oxide is water-soluble
Graphene oxide in liquid with a thickness of 1nm~20nm；
The diameter of the nano-cellulose is 2nm~20nm, and length is 1 μm~5 μm；
Graphene oxide, reducing agent and nano-cellulose in the graphene oxide water solution press the group of mass fraction
At as follows：Graphene oxide in graphene oxide water solution is 100 parts, and nano-cellulose is 5 parts~25 parts, reducing agent 10
Part~100 parts；
Two, heat conductive silica gel is prepared：
1, modified heat filling：The dehydrated alcohol mixed solution and heat filling of silane coupling agent I are added to high speed together
1min~15min is mixed in mixing machine, then dry 2h~6h under conditions of temperature is 80 DEG C~120 DEG C, obtains modification
Heat filling；Silane coupling agent I and the volume ratio of dehydrated alcohol are in the dehydrated alcohol mixed solution of the silane coupling agent I
1:(2~10)；The quality of silane coupling agent I and heat filling in the dehydrated alcohol mixed solution of the silane coupling agent I
Than for (1~5):100；
2, using vacuum machine blender by two-component liquid silica gel and modified heat filling mixing 10min~60min,
Obtain heat conductive silica gel；The mass ratio of the two-component liquid silica gel and modified heat filling is 1:(3~10)；Described is double
The viscosity of component liquid silica gel is 50cP~1000cP；
Three, graphene heat conducting film/heat conductive silica gel film composite material of stratiform alternating structure is prepared：
1, the silane surface of graphene heat conducting film is modified：Graphene heat conducting film is immersed to the ethanol solution of silane coupling agent II
In be standing and soaking 2min~20min, then dry 0.5h~2h under conditions of temperature is 60 DEG C~90 DEG C, obtains silane surface
Modified graphene heat conducting film；The volume of silane coupling agent II and dehydrated alcohol in the ethanol solution of the silane coupling agent II
Than being 1:(1~5)；
2, heat conductive silica gel is spread using heat conductive silica gel and silane surface modified graphene heat conducting film alternately arranged mode
Open up in the surface of the modified graphene heat conducting film of silane surface, suppressed and formed a film with calender, then solidification temperature be 80 DEG C~
Solidify 5min~120min under conditions of 150 DEG C, obtains graphene heat conducting film/thermal conductive silicon glue film composite wood of stratiform alternating structure
Material；In the graphene of the stratiform alternating structure/heat conductive silica gel film composite material thermal conductive silicon glue film with a thickness of 0.1mm~
10mm。
Specific embodiment three：Present embodiment is unlike specific embodiment two：Reduction described in step 1
Agent is hydrazine hydrate, sodium borohydride, hydroiodic acid or vitamin C.Other are identical as specific embodiment party two.
Specific embodiment four：Unlike one of present embodiment and specific embodiment two or three：Institute in step 1
The hole for the composite fibre miillpore filter stated is 0.22 μm.Other are identical as one of specific embodiment two or three.
Specific embodiment five：Unlike one of present embodiment and specific embodiment two to four：Institute in step 2
Silane coupling agent I in the dehydrated alcohol mixed solution for the silane coupling agent I stated is vinyltriethoxysilane, vinyl three
Methoxy silane, vinyl three (beta-methoxy ethyoxyl) silane) and γ-methacryloxypropyl trimethoxy silane in
One or more of mixtures.Other are identical as one of specific embodiment two to four.
Specific embodiment six：Unlike one of present embodiment and specific embodiment two to five：Institute in step 2
The heat filling stated is in aluminium oxide, aluminium nitride, boron nitride, silicon carbide, graphene, carbon nanotube, aluminium powder, copper powder and silver powder
One or more of mixtures.Other are identical as one of specific embodiment two to five.
Specific embodiment seven：Unlike one of present embodiment and specific embodiment two to six：Institute in step 3
Silane coupling agent II in the ethanol solution for the silane coupling agent II stated is vinyltriethoxysilane, vinyl trimethoxy
Silane, vinyl three (beta-methoxy ethyoxyl) silane) and one of γ-methacryloxypropyl trimethoxy silane or
Several mixtures.Other are identical as one of specific embodiment two to six.
The present invention is verified with following tests：
Test one：This test is a kind of graphene heat conducting film/heat conductive silica gel film composite material system of stratiform alternating structure
Preparation Method specifically carries out according to the following steps：：
One, graphene heat conducting film is prepared：Using high-speed mixer by graphene oxide water solution, reducing agent and nanofiber
Plain uniformly mixing 6min, is then sonicated 40min, reduction reaction 6h is then stood under the conditions of at a temperature of 90 °C, takes 200mL
Mixed liquor filtered on composite fibre miillpore filter, with second alcohol and water alternately washing filter cake to filtrate be it is neutral, filtered after washing
Cake is 120 DEG C of dry 2h in temperature, and composite fibre miillpore filter and filter cake are removed, graphene heat conducting film is obtained；
The concentration of the graphene oxide water solution is 5mg/mL, the oxidation stone in the graphene oxide water solution
Black alkene with a thickness of 10nm；
The diameter of the nano-cellulose is 2nm~20nm, and length is 1 μm~5 μm；
The composition of graphene oxide, reducing agent and nano-cellulose in the graphene oxide water solution is as follows：Oxygen
Graphene oxide in graphite aqueous solution is 200mg, nano-cellulose 0.1g, reducing agent 0.6g；
Two, heat conductive silica gel is prepared：
1, modified heat filling：The dehydrated alcohol mixed solution and heat filling of silane coupling agent I are added to high speed together
1min is mixed in mixing machine, then dry 2h under conditions of temperature is 120 DEG C, obtains modified heat filling；The silicon
Silane coupling agent I is 0.2g, dehydrated alcohol 2mL in the dehydrated alcohol mixed solution of alkane coupling agent I；The silane coupling agent
The mass ratio of silane coupling agent I and heat filling in I dehydrated alcohol mixed solution is 1:50；
2, two-component liquid silica gel and modified heat filling mixing 30min are led using vacuum machine blender
Hot silica gel；The mass ratio of the two-component liquid silica gel and modified heat filling is 1:10；The two-component liquid silicon
The viscosity of glue is 200cP；
Three, graphene heat conducting film/heat conductive silica gel film composite material of stratiform alternating structure is prepared：
1, the silane surface of graphene heat conducting film is modified：Graphene heat conducting film is immersed to the ethanol solution of silane coupling agent II
In be standing and soaking 6min, then dry 1h under conditions of temperature is 80 DEG C, obtains the modified graphene heat conducting film of silane surface；
Silane coupling agent II is 0.5g, dehydrated alcohol 0.5mL in the ethanol solution of the silane coupling agent II；
2, heat conductive silica gel is spread using heat conductive silica gel and silane surface modified graphene heat conducting film alternately arranged mode
It opens up in the surface of the modified graphene heat conducting film of silane surface, is suppressed and formed a film with calender, be then 150 DEG C in solidification temperature
Under the conditions of solidify 30min, obtain graphene heat conducting film/heat conductive silica gel film composite material of stratiform alternating structure, totally 5 layers；It is described
Stratiform alternating structure graphene/heat conductive silica gel film composite material in thermal conductive silicon glue film with a thickness of 1mm；
Reducing agent described in step 1 is hydroiodic acid or vitamin C；
The hole of composite fibre miillpore filter described in step 1 is 0.22 μm；
Silane coupling agent I in the dehydrated alcohol mixed solution of silane coupling agent I described in step 2 is vinyl three
Methoxy silane；
Heat filling described in step 2 is the mixture of 6g aluminium oxide and 4g aluminium nitride；
Silane coupling agent II in the ethanol solution of silane coupling agent II described in step 3 is vinyl trimethoxy
Silane.
Fig. 1 is the graphene heat conducting film/heat conductive silica gel composite material schematic diagram for testing the stratiform alternating structure of a preparation,
1 is thermal conductive silicon glue film, and 2 be graphene heat conducting film.
This test has the advantages that：
1, this test provides the preparation method of stratiform heat-conductive composite material, is handed over using graphene heat conducting film and thermal conductive silicon glue film
For the mode of arrangement, it is capable of forming multilayered structure, the specific number of plies does not limit, and can decide in its sole discretion according to actual needs；
2, this test utilizes the heating conduction of the adjustable laminar composite of multilayered structure, passes through graphene heat conducting film
Effect can quickly spread the heat that local height is concentrated, and improve the uniformity and radiating efficiency of heat dissipation；
3, this test solves the dispersion of graphene using nano-cellulose, using dispersion progress synchronous with reduction
Method avoids the reunion of graphene in reduction process.
Claims (7)
1. a kind of graphene heat conducting film/heat conductive silica gel film composite material of stratiform alternating structure, it is characterised in that stratiform is alternately tied
Graphene heat conducting film/heat conductive silica gel film composite material of structure is made of graphene heat conducting film and thermal conductive silicon glue film, the stone
Black alkene heat conducting film and thermal conductive silicon glue film are alternately arranged；The thermal conductive silicon glue film with a thickness of 0.1mm~10mm.
2. a kind of graphene heat conducting film/heat conductive silica gel film composite material system of stratiform alternating structure as described in claim 1
Preparation Method, it is characterised in that graphene heat conducting film/heat conductive silica gel film composite material preparation method of stratiform alternating structure be by
What following steps carried out：：
One, graphene heat conducting film is prepared：It is using high-speed mixer that graphene oxide water solution, reducing agent and nano-cellulose is equal
Even mixing 5min~10min, is then sonicated 20min~60min, then stands also under conditions of temperature is 60 DEG C~90 DEG C
Original reaction 2h~6h, filters on composite fibre miillpore filter, and with second alcohol and water, alternately washing filter cake to filtrate is neutral, washing
Filter cake is 80 DEG C~120 DEG C dry 2h~6h in temperature afterwards, and composite fibre miillpore filter and filter cake are removed, graphene is obtained and leads
Hotting mask；
The concentration of the graphene oxide water solution is 0.1mg/mL~10mg/mL, in the graphene oxide water solution
Graphene oxide with a thickness of 1nm~20nm；
The diameter of the nano-cellulose is 2nm~20nm, and length is 1 μm~5 μm；
Graphene oxide, reducing agent and nano-cellulose in the graphene oxide water solution press the composition of mass fraction such as
Under：Graphene oxide in graphene oxide water solution is 100 parts, and nano-cellulose is 5 parts~25 parts, reducing agent is 10 parts~
100 parts；
Two, heat conductive silica gel is prepared：
1., modified heat filling：The dehydrated alcohol mixed solution and heat filling of silane coupling agent I are added to mixed at high speed together
1min~15min is mixed in machine, then dry 2h~6h under conditions of temperature is 80 DEG C~120 DEG C, obtains the thermally conductive of modification
Filler；The volume ratio of silane coupling agent I and dehydrated alcohol is 1 in the dehydrated alcohol mixed solution of the silane coupling agent I:(2
~10)；The mass ratio of silane coupling agent I and heat filling in the dehydrated alcohol mixed solution of the silane coupling agent I is
(1~5):100；
2., using vacuum machine blender by two-component liquid silica gel and modified heat filling mixing 10min~60min, obtain
To heat conductive silica gel；The mass ratio of the two-component liquid silica gel and modified heat filling is 1:(3~10)；Described double groups
The viscosity of part liquid silica gel is 50cP~1000cP；
Three, graphene heat conducting film/heat conductive silica gel film composite material of stratiform alternating structure is prepared：
1., the silane surface of graphene heat conducting film it is modified：Graphene heat conducting film is immersed in the ethanol solution of silane coupling agent II
It is standing and soaking 2min~20min, then dry 0.5h~2h under conditions of temperature is 60 DEG C~90 DEG C, obtains silane surface and change
The graphene heat conducting film of property；The volume ratio of silane coupling agent II and dehydrated alcohol in the ethanol solution of the silane coupling agent II
It is 1:(1~5)；
2., using heat conductive silica gel and silane surface modified graphene heat conducting film alternately arranged mode heat conductive silica gel is spread in
The surface of the modified graphene heat conducting film of silane surface, is suppressed with calender and is formed a film, and is then 80 DEG C~150 DEG C in solidification temperature
Under conditions of solidify 5min~120min, obtain graphene heat conducting film/heat conductive silica gel film composite material of stratiform alternating structure；Institute
Thermal conductive silicon glue film with a thickness of 0.1mm~10mm in the graphene for the stratiform alternating structure stated/heat conductive silica gel film composite material.
3. a kind of graphene heat conducting film/heat conductive silica gel film composite material of stratiform alternating structure according to claim 2
Preparation method, it is characterised in that reducing agent described in step 1 is hydrazine hydrate, sodium borohydride, hydroiodic acid or vitamin C.
4. a kind of graphene heat conducting film/heat conductive silica gel film composite material of stratiform alternating structure according to claim 2
Preparation method, it is characterised in that the hole of composite fibre miillpore filter described in step 1 is 0.22 μm.
5. a kind of graphene heat conducting film/heat conductive silica gel film composite material of stratiform alternating structure according to claim 2
Preparation method, it is characterised in that the silane coupling agent I in the dehydrated alcohol mixed solution of silane coupling agent I described in step 2
For vinyltriethoxysilane, vinyltrimethoxysilane, vinyl three (beta-methoxy ethyoxyl) silane) and γ-methyl
The mixture of one or more of acryloyloxypropyltrimethoxysilane.
6. a kind of graphene heat conducting film/heat conductive silica gel film composite material of stratiform alternating structure according to claim 2
Preparation method, it is characterised in that heat filling described in step 2 is aluminium oxide, aluminium nitride, boron nitride, silicon carbide, graphite
The mixture of one or more of alkene, carbon nanotube, aluminium powder, copper powder and silver powder.
7. a kind of graphene heat conducting film/heat conductive silica gel film composite material of stratiform alternating structure according to claim 2
Preparation method, it is characterised in that the silane coupling agent II in the ethanol solution of silane coupling agent II described in step 3 is ethylene
Ethyl triethoxy silicane alkane, vinyltrimethoxysilane, vinyl three (beta-methoxy ethyoxyl) silane) and γ-methacryl
The mixture of one or more of oxygroup propyl trimethoxy silicane.
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