CN113290958B - Graphene foam film reinforced heat conduction gasket and preparation method thereof - Google Patents
Graphene foam film reinforced heat conduction gasket and preparation method thereof Download PDFInfo
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- CN113290958B CN113290958B CN202110034374.5A CN202110034374A CN113290958B CN 113290958 B CN113290958 B CN 113290958B CN 202110034374 A CN202110034374 A CN 202110034374A CN 113290958 B CN113290958 B CN 113290958B
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- graphene foam
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 259
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 259
- 239000006260 foam Substances 0.000 title claims abstract description 242
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000000853 adhesive Substances 0.000 claims abstract description 62
- 230000001070 adhesive effect Effects 0.000 claims abstract description 62
- 230000006835 compression Effects 0.000 claims abstract description 22
- 238000007906 compression Methods 0.000 claims abstract description 22
- 239000011148 porous material Substances 0.000 claims description 120
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 62
- 239000000741 silica gel Substances 0.000 claims description 62
- 229910002027 silica gel Inorganic materials 0.000 claims description 62
- 239000012528 membrane Substances 0.000 claims description 48
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 32
- 238000005520 cutting process Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 18
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 16
- 238000007747 plating Methods 0.000 claims description 11
- -1 polydimethylsiloxane Polymers 0.000 claims description 11
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 9
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 9
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 8
- 238000004080 punching Methods 0.000 claims description 8
- 238000001465 metallisation Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 6
- 238000009832 plasma treatment Methods 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- OTKXURHKRLMLIY-UHFFFAOYSA-N [SiH3]O[SiH2]C#N Chemical compound [SiH3]O[SiH2]C#N OTKXURHKRLMLIY-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 238000007788 roughening Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 3
- 239000004925 Acrylic resin Substances 0.000 claims description 3
- 229920000178 Acrylic resin Polymers 0.000 claims description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 229920005546 furfural resin Polymers 0.000 claims description 3
- 230000000149 penetrating effect Effects 0.000 claims description 3
- 229920001568 phenolic resin Polymers 0.000 claims description 3
- 239000005011 phenolic resin Substances 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 229920002635 polyurethane Polymers 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- 238000004381 surface treatment Methods 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 238000003698 laser cutting Methods 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 239000002002 slurry Substances 0.000 claims description 2
- 230000008014 freezing Effects 0.000 claims 1
- 238000007710 freezing Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 description 55
- 230000000052 comparative effect Effects 0.000 description 18
- 238000012360 testing method Methods 0.000 description 17
- 239000010410 layer Substances 0.000 description 12
- 230000000694 effects Effects 0.000 description 10
- 238000007598 dipping method Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000002390 adhesive tape Substances 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 230000003746 surface roughness Effects 0.000 description 3
- PKMNZOFQIRXQDO-UHFFFAOYSA-N heptane;hexane Chemical compound CCCCCC.CCCCCCC PKMNZOFQIRXQDO-UHFFFAOYSA-N 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 239000002103 nanocoating Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 239000013464 silicone adhesive Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000008096 xylene Substances 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
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/18—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by features of a layer of foamed material
-
- 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
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
-
- 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
- B32B38/04—Punching, slitting or perforating
-
- 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
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
- B32B5/32—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed at least two layers being foamed and next to each other
-
- 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
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K7/00—Constructional details common to different types of electric apparatus
- H05K7/20—Modifications to facilitate cooling, ventilating, or heating
- H05K7/2039—Modifications to facilitate cooling, ventilating, or heating characterised by the heat transfer by conduction from the heat generating element to a dissipating body
-
- 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
- B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
- B32B2260/02—Composition of the impregnated, bonded or embedded layer
-
- 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
- B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
- B32B2260/04—Impregnation, embedding, or binder material
- B32B2260/046—Synthetic resin
-
- 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
- B32B2266/00—Composition of foam
- B32B2266/04—Inorganic
-
- 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
-
- 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
- B32B2307/51—Elastic
Landscapes
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The application discloses a graphene foam film reinforced heat conduction gasket and a preparation method thereof, wherein the graphene foam film reinforced heat conduction gasket comprises the following components: the heat-conducting gasket comprises a multi-layer graphene foam film and an adhesive filled in the graphene foam film and between the graphene foam film and the adhesive, wherein the graphene foam film accounts for 60-95 wt% of the total weight of the heat-conducting gasket. According to the application, the graphene is arranged in the heat conduction gasket along the thickness direction, and the gasket has good heat conduction performance in the thickness direction; the combination of the graphene foam film and the adhesive has good compressibility and compression resilience, and the application thermal resistance is small.
Description
Technical Field
The application relates to the fields of heat conduction, heat dissipation, heat management materials, heat conduction interface materials and the like, in particular to a graphene reinforced heat conduction gasket.
Background
The heat conducting gasket is a heat conducting material and is mainly applied to a transfer interface between electronic equipment and a radiating fin or a product shell. The graphene has good heat conduction performance and can be used as a reinforcing material of the heat conduction gasket. The mode of adopting graphene heat conduction film reinforced heat conduction gaskets mainly comprises two modes: firstly, stacking and bonding graphene heat conducting films layer by layer through an adhesive, and then cutting the graphene heat conducting films into heat conducting gaskets to enable the graphene heat conducting films to be arranged along the thickness direction, as in patent document WO2019235983A1; secondly, the graphene heat conducting film is changed into a longitudinal arrangement from a plane direction in a folding mode, and then an adhesive is coated to form an integral structure, for example, patent document CN110491845A.
The graphene heat conduction film adopted in the two modes has higher heat conduction coefficient, but the densified structure of the graphene heat conduction film leads to higher hardness of the prepared heat conduction gasket, and the application thermal resistance of the gasket is obviously increased; meanwhile, the obtained heat-conducting gasket is void-free and poor in compression rebound resilience, and cannot achieve the effect of filling a heat-conducting interface. The graphite-like structure in the graphene heat conducting film is easy to cause layering, so that the overall mechanical stability is affected, and the risk of cracking exists; and serious consequences of thermal failure can occur under the use conditions of high temperature, high humidity, severe cold, long term and the like. In addition, the graphene heat-conducting film has a smooth surface, and often needs to be subjected to surface roughening treatment, such as nano coating or polishing roughening, so that good combination with an adhesive can be realized; the coating layer has at least two more heat resistance interfaces, and the risk of thermal failure exists under the condition of long-term aging; the mechanical property is reduced due to surface polishing, and the compression rebound performance requirement can not be met.
The matters in the background section are only those known to the inventors and do not, of course, represent prior art in the field.
Disclosure of Invention
In view of one or more of the problems with the prior art, the present application provides a graphene foam membrane-reinforced thermally conductive gasket comprising: the heat-conducting gasket comprises a multi-layer graphene foam film and an adhesive filled in the graphene foam film and between the graphene foam film and the adhesive, wherein the graphene foam film accounts for 60-95 wt% of the total weight of the heat-conducting gasket.
According to one aspect of the application, the graphene foam film comprises 75-90 wt% of the total weight of the heat-conducting gasket. In the graphene foam film reinforced heat conduction gasket to be protected, the content of the adhesive needs to be strictly controlled so as to ensure the duty ratio of the graphene foam film. Through intensive researches on graphene foam films, in combination with the action relationship of an adhesive on the graphene foam films, the inventors of the present application found that when the graphene foam films account for less than 60wt%, the heat conduction effect is poor due to too little graphene, and when the graphene foam films account for more than 95wt%, the heat conduction pad cannot be molded due to too little adhesive, and when the graphene foam films account for 60wt% to 95wt% of the total weight of the heat conduction pad, the object of the present application can be basically satisfied, and when the graphene foam films account for 75wt% to 90wt% of the total weight of the heat conduction pad, the object of the present application is most suitable.
According to one aspect of the present application, the graphene foam film has a thermal conductivity of 50W/(m·k) or more, preferably 100W/(m·k) or more.
According to one aspect of the application, the graphene foam film has a density of 0.1-0.9g/cm 3 Preferably 0.2-0.5g/cm 3 。
According to one aspect of the application, the graphene foam film has a thickness of 50-1000 μm, preferably 300-500 μm.
According to one aspect of the present application, the graphene foam film includes a plurality of first pores inside and a plurality of second pores penetrating in a thickness direction. The first pore in the graphene foam film plays a role in enhancing foam compression resilience, and can also contain a certain adhesive, so that the first pore is combined with the graphene pore wall, and the compression resilience of the heat conduction gasket is further enhanced. The inventor of the application has found through research that only an adhesive is arranged between foam films, a structural member formed by bonding a plurality of layers of foam films through the adhesive is easy to delaminate, a gasket formed by cutting is easy to crack, the yield is greatly reduced, the heat conduction effect is also poor due to delamination problem, the service life is not high in practical use, and great trouble is brought to practical application. Further, when the inventor researches the process of forming the gasket by the graphene foam, comprehensive analysis is carried out on various factors, and finally, the following steps are obtained: when the thickness of the graphene foam film is lower than 50 mu m, the mechanical strength is lower, and the graphene foam film is easy to damage in the preparation process; the thickness is higher than 1000 mu m, so that the adhesive is not easy to enter the interior, and the internal bonding of the graphene foam film is poor; the density of the graphene foam film is lower than 0.1g/cm 3 When the graphene foam film is used, the graphene foam film is easy to crack, and the density is higher than 0.9g/cm 3 The pores are less, and the adhesive is not presentCan enter the interior of the graphene foam.
According to one aspect of the application, the first pores have a pore size of 10-100 μm, preferably 15-50 μm. When the pore diameter of the first pore is smaller than 10 mu m, the pore is too small, and the adhesive is influenced; if the particle size is more than 100 mu m, the graphene foam film is too fluffy, the mechanical property is poor, and the difficulty is brought to the preparation of the gasket.
According to one aspect of the application, the first pores account for 60% -95%, and most preferably 75% -90% of the volume of the graphene foam film body.
According to one aspect of the application, the second pores have a pore size of 50-500 μm, preferably 100-300 μm. When the aperture of the second pore is less than 50 μm, the up-down penetration effect is poor; if the particle size is higher than 500 mu m, the mechanical property of the graphene foam film is reduced due to larger pores; when the pore diameter of the second pore is higher than 500 mu m, the mechanical property of the graphene foam membrane is reduced and the graphene foam membrane is easy to crack due to larger pores.
According to one aspect of the application, the center-to-center spacing between adjacent pores between the second pores is 300-1000 μm, preferably 400-800 μm. The spacing between the second pores is less than 300 mu m, so that the graphene foam film is too dense and is easy to crack; if the particle diameter is more than 1000. Mu.m, the particle diameter is too large, and the penetration effect is impaired.
According to one aspect of the application, the first and second voids are filled with an adhesive.
According to one aspect of the application, the graphene foam film is graphene oxide slurry, and is formed through coating, drying and heat treatment, and first pores are formed among graphene sheets inside the graphene foam film.
According to one aspect of the present application, the graphene foam films are arranged in the thickness direction of the thermally conductive pad.
According to one aspect of the application, the thickness of the heat conducting pad is 0.1-5mm, preferably 0.25-0.5mm; .
According to one aspect of the application, the adhesive is a compressible, compression resilient adhesive.
According to one aspect of the application, the adhesive adopts epoxy resin, phenolic resin, furfural resin, polyurethane, acrylic resin and organic silica gel. Preferably, the adhesive is a silicone adhesive. Further preferably, the adhesive is selected from the group consisting of polydimethylsiloxane, alpha, omega-dihydroxypolydimethylsiloxane, polydiphenylsiloxane, alpha, omega-dihydroxypolymethyl3, 3-trifluoropropyl siloxane, cyanosiloxysilane, and alpha, omega-diethylpolydimethylsiloxane.
The preparation method of the graphene foam film reinforced heat conduction gasket comprises the following steps:
taking a graphene foam film;
punching the graphene foam film to form a plurality of second holes penetrating up and down in the thickness direction of the graphene foam film;
immersing the graphene foam film in an adhesive or an adhesive solution;
stacking and bonding the impregnated graphene foam films layer by layer to form a block, and fully curing the adhesive; and
cutting the block into a plurality of slices along the height direction of the layer stack.
According to one aspect of the present application, the graphene foam film has a thermal conductivity of 50W/((m.K)) or more, preferably 100W/((m.K)) or more.
According to one aspect of the application, the graphene foam membrane is internally provided with a plurality of first pores, and the pore diameter of the first pores is 10-100 microns, preferably 15-50 microns.
According to one aspect of the application, the first pores account for 60% -95%, and most preferably 75% -90% of the volume of the graphene foam film body.
According to one aspect of the application, the graphene foam film has a density of 0.1-0.9g/cm 3 Preferably 0.2-0.5g/cm 3 。
According to one aspect of the application, the graphene foam film has a thickness of 50-1000 μm, preferably 300-500 μm.
According to one aspect of the application, the surface roughening treatment imparts a roughness of 4-20 μm to the graphene foam film surface.
According to one aspect of the application, the specific method for punching comprises the following steps: needle tip penetration, laser ablation, plasma punching, mechanical punching.
According to one aspect of the application, the second pores have a pore size of 50-500 μm, preferably 100-300 μm.
According to one aspect of the application, the second pores have a pore center-to-center spacing of 300-1000 μm, preferably 400-800 μm.
According to one aspect of the application, the graphene foam film is preferably surface treated.
Preferably, the surface treatment adopts at least one of surface metallization treatment and plasma treatment.
Preferably, the metallization treatment employs copper plating, nickel plating, iron plating or silver plating.
Preferably, the surface metallization treatment employs a coating thickness of 0.1-2 μm, preferably 0.5-1 μm.
Preferably, the plasma treatment is performed under an air atmosphere, a nitrogen atmosphere or an oxygen atmosphere.
Preferably, the plasma treatment, plasma power is 1-10KW, preferably 3-8KW.
According to one aspect of the application, the adhesive is a compressible, compression resilient adhesive. Preferably, the adhesive adopts epoxy resin, phenolic resin, furfural resin, polyurethane, acrylic resin and organic silica gel. Further preferably, the adhesive is a silicone gel. Further preferably, the adhesive is selected from the group consisting of polydimethylsiloxane, alpha, omega-dihydroxypolydimethylsiloxane, polydiphenylsiloxane, alpha, omega-dihydroxypolymethyl3, 3-trifluoropropyl siloxane, cyanosiloxysilane, and alpha, omega-diethylpolydimethylsiloxane.
According to one aspect of the application, the solvent of the adhesive solution is at least one of xylene, ethanol, acetone, hexane, pentane, heptane, tetrahydrofuran, N-dimethylformamide, and N-methylpyrrolidone.
According to one aspect of the application, the viscosity of the adhesive solution is 30 to 1000 mPas, preferably 100 to 500 mPas. The viscosity of the adhesive solution is lower than 30 mPa.s, and the adhesive is too little to influence the bonding effect with the graphene foam film; if the viscosity of the adhesive solution is higher than 1000 mPas, the adhesive solution is too viscous to be impregnated easily. If an adhesive is used to achieve such a viscosity, it can be used alone without the addition of a solvent. For lower viscosity adhesives, dilution with solvent may be omitted. If the polydimethyl cyclosiloxane is diluted as an adhesive, the silica gel in the silica gel solution accounts for 20-80 wt%, preferably 40-60 wt%, and is less than 20 wt%, so that the silica gel is too little to influence the bonding effect with the graphene foam film; above 80wt.%, the viscosity is too great to be impregnated.
According to one aspect of the application, the curing is performed by heating at a temperature of 150 ℃ or below or at room temperature.
According to one aspect of the application, the cutting is performed in the thickness direction of the layer stack, preferably by wire cutting, laser cutting, ultrasonic cutting, blade cutting or freeze cutting.
According to one aspect of the application, the sheet is cut to a thickness of 0.1-5mm, most preferably 0.25-0.5mm.
The application has the following effects:
1) According to the application, the graphene foam film is used as a raw material of the heat conduction gasket, and the pores are vertically penetrated in the graphene foam film, so that the pores in the graphene foam film are communicated, the adhesive is easy to enter the graphene foam film, and the adhesive is fully combined with graphene, especially with graphene in the graphene foam film. 5-7, the graphene foam film provided by the application has the advantages of abundant pores, large pores and high porosity, effectively improves the rebound resilience of the product, and ensures the mechanical properties of the product because the walls of the pores can be tightly connected. As can be seen from fig. 7-9, the second holes are communicated with the first holes, and more adhesive is distributed in the first holes and the second holes. The heat conduction gasket reinforced by the graphene film structural material has good compressibility and compression rebound resilience.
2) The graphene foam film adopted by the application has a rough surface, and good combination can be realized by directly using an adhesive between the foam films. The surface roughness of the existing graphene guide film is 0.4-0.8 mu m, and the surface roughness of the graphene foam film used in the application is 4-10 mu m. The surface of the graphene foam film can form the surface roughness of 4-10 mu m without special treatment. Referring to fig. 1-3, the surface of the graphene foam film adopted by the application is visually rough, and after the graphene foam film is removed, the graphene foam film cannot be well separated from the two sheets due to tight adhesion.
3) And the adhesive is well combined with graphene in the graphene foam film, and the peel strength of the graphene foam film after gum dipping is compared and tested. The peeling test is used for testing the internal binding force of the film, and comprises the following steps: one side is adhered to a steel plate by a double-sided adhesive tape, the other side is adhered by a single-sided adhesive tape, and then the steel plate is placed on a peeling force tester, one end of the tester clamps the steel plate, the other end clamps the single-sided adhesive tape, and the peeling force for peeling the film is tested at an angle of 180 degrees. The test data can be used for representing the strength of the internal binding force of the film. Referring to fig. 4, a comparison graph of peel tests is shown, before and after the graphene foam film is impregnated with the adhesive. Left: the product is easier to peel before dipping, and the peeling force is 61g/25mm; right: after dipping, the product is difficult to peel, and the peeling force is 134g/25mm
4) The graphene is arranged in the heat conduction gasket along the thickness direction, and the gasket has good heat conduction performance in the thickness direction;
5) The combination of the graphene foam film and the adhesive has good compressibility and compression resilience, and the application thermal resistance is small.
Drawings
The accompanying drawings are included to provide a further understanding of the application and are incorporated in and constitute a part of this specification, illustrate the application and together with the embodiments of the application, serve to explain the application. In the drawings:
FIG. 1 is a photograph of a graphene foam film used in the present application;
FIG. 2 is a photograph of a graphene foam film used in the present application with an adhesive attached to the surface thereof;
FIG. 3 is a photograph of two graphene foam films used in the present application after being bonded together and peeled apart;
FIG. 4 is a graph of a test comparison using a peel tester;
FIG. 5 is an EMS image of a longitudinal cut section of a graphene foam membrane used in the present application;
FIG. 6 is a surface EMS image of a graphene foam membrane used in the present application after perforation;
FIG. 7 is an EMS image of a longitudinal section of a graphene foam membrane used in the present application after punching;
FIG. 8 is a surface EMS image of a graphene foam film used in the present application after perforation and dipping;
FIG. 9 is a cross-sectional EMS view of a gasket of the present application;
FIG. 10 is an enlarged view of a portion of FIG. 8;
FIG. 11 is a photograph of a block after bonding a layer of impregnated graphene foam film;
fig. 12 is a photograph of a graphene foam membrane reinforced thermal pad obtained after cutting the block of fig. 11.
Detailed Description
Hereinafter, only certain exemplary embodiments are briefly described. As will be recognized by those of skill in the pertinent art, the described embodiments may be modified in various different ways without departing from the spirit or scope of the present application. Accordingly, the drawings and description are to be regarded as illustrative in nature and not as restrictive.
In the description of the present application, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present application and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present application. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more of the described features. In the description of the present application, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
In the description of the present application, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be fixedly connected, detachably connected, or integrally connected, and may be mechanically connected, electrically connected, or may communicate with each other, for example; can be directly connected or indirectly connected through an intermediate medium, and can be communicated with the inside of two elements or the interaction relationship of the two elements. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art according to the specific circumstances.
In the present application, unless expressly stated or limited otherwise, a first feature "above" or "below" a second feature may include both the first and second features being in direct contact, as well as the first and second features not being in direct contact but being in contact with each other through additional features therebetween. Moreover, a first feature being "above," "over" and "on" a second feature includes the first feature being directly above and obliquely above the second feature, or simply indicating that the first feature is higher in level than the second feature. The first feature being "under", "below" and "beneath" the second feature includes the first feature being directly above and obliquely above the second feature, or simply indicating that the first feature is less level than the second feature.
The following disclosure provides many different embodiments, or examples, for implementing different features of the application. In order to simplify the present disclosure, components and arrangements of specific examples are described below. They are, of course, merely examples and are not intended to limit the application. Furthermore, the present application may repeat reference numerals and/or letters in the various examples, which are for the purpose of brevity and clarity, and which do not themselves indicate the relationship between the various embodiments and/or arrangements discussed. In addition, the present application provides examples of various specific processes and materials, but one of ordinary skill in the art will recognize the application of other processes and/or the use of other materials.
The preferred embodiments of the present application will be described below with reference to the accompanying drawings, it being understood that the preferred embodiments described herein are for illustration and explanation of the present application only, and are not intended to limit the present application.
In the following examples and comparative examples, the following methods were used to prepare the thermal conductive gaskets using graphene foam films and liquid silica gel:
a) Dipping the graphene heat-conducting foam film into liquid silica gel;
b) Stacking and bonding the graphene heat-conducting foam films subjected to glue dipping layer by layer to form a block, and fully curing the silica gel;
c) And cutting the solidified block into pieces to obtain the graphene heat-conducting foam film reinforced heat-conducting gasket.
To show the comparative effect, the thicknesses of the following example slices were taken as four thicknesses of 0.25mm, 0.5mm, 1mm and 2 mm. The following examples all employ the above methods, with the exception of specific parameters, which are described in detail below.
The following examples, all were tested for thermal conductivity and applied thermal resistance by ASTM D5470 at 20 psi; the thermal pads were tested for their compression resilience at 50% strain by ASTM D575.
Example 1:
in this example, the graphene foam film accounts for 60wt.%, the liquid silica gel 40wt.%;
graphene foam film thermal conductivity 50W/(m K);
graphene foam film thickness 50 μm and density 0.1g/cm 3 ;
The average pore diameter of the inner pores of the graphene foam membrane is 10 mu m, the pore diameters of the upper and lower through holes are 50 mu m, and the center-to-center distance of the through holes is 300 mu m;
the liquid silica gel is polydimethyl cyclosiloxane, and is diluted to have the viscosity of 1000 mPa.s by adopting heptane;
curing temperature is 150 ℃;
through testing, the porosity of the sample is 90%, the heat conductivity coefficient is 29W/(m K), and the thermal resistance and compression rebound resilience of samples with different thicknesses are as follows:
example 2:
in this example, graphene foam film was 95wt.%, liquid silica gel was 5wt.%;
graphene foam film thermal conductivity 460W/(m K);
graphene foam film thickness 1000 μm and density 0.9g/cm 3 ;
The average pore diameter of the internal pores of the graphene foam membrane is 100 mu m, the pore diameters of upper and lower through holes are 500 mu m, and the center distance of the through holes is 1000 mu m;
the liquid silica gel is polydimethylsiloxane, and hexane is adopted to dilute the liquid silica gel to the viscosity of 30 mPa.s;
curing temperature is 120 ℃;
through testing, the porosity of the sample is 50%, the heat conductivity coefficient is 326W/(m K), and the thermal resistance and compression rebound resilience of samples with different thicknesses are as follows:
example 3:
in this example, graphene foam film was 75wt.%, liquid silica gel 25wt.%;
graphene foam film thickness 300 μm and density 0.2g/cm 3 ;
The thermal conductivity of the graphene foam film is 102W/(m K);
the average pore diameter of the internal pores of the graphene foam membrane is 15 mu m, the pore diameters of the upper and lower through holes are 100 mu m, and the center distance of the through holes is 400 mu m;
the liquid silica gel is alpha, omega-dihydroxy polydimethylsiloxane, and is diluted to have the viscosity of 100 mPa.s by adopting tetrahydrofuran;
the curing temperature is 80 ℃;
through testing, the porosity of the sample is 84%, the heat conductivity coefficient is 76W/(m K), and the thermal resistance and compression rebound resilience of samples with different thicknesses are as follows:
example 4:
in this example, the graphene foam film accounts for 90wt.%, the liquid silica gel 10wt.%;
the thermal conductivity of the graphene foam film is 254W/(m K);
graphene foam film thickness 500 μm and density 0.5g/cm 3 ;
The average pore diameter of the inner pores of the graphene foam membrane is 50 mu m, the pore diameters of the upper and lower through holes are 300 mu m, and the center distance of the through holes is 800 mu m;
the liquid silica gel is polydiphenylsiloxane, and is diluted to have the viscosity of 500 mPa.s by adopting N, N-dimethylformamide;
the curing temperature is room temperature;
through testing, the porosity of the sample is 72%, the heat conductivity coefficient is 203W/(m K), and the thermal resistance and compression rebound resilience of samples with different thicknesses are as follows:
example 5:
in this example, the graphene foam film accounts for 80wt.%, the liquid silica gel 20wt.%;
graphene foam film thickness 400 μm and density 0.3g/cm 3 ;
The thermal conductivity of the graphene foam film is 174W/(m K);
the average pore diameter of the internal pores of the graphene foam membrane is 30 mu m, the pore diameter of the upper and lower through holes is 200 mu m, and the center distance of the through holes is 500 mu m;
the liquid silica gel is alpha, omega-dihydroxyl polymethyl (3, 3-trifluoropropyl) siloxane, and is diluted to have the viscosity of 300 mPa.s by adopting N-methylpyrrolidone;
curing temperature is 60 ℃;
through testing, the porosity of the sample is 79%, the heat conductivity coefficient is 140W/(m K), and the thermal resistance and compression rebound resilience of samples with different thicknesses are as follows:
example 6:
in this example, the graphene foam film accounts for 80wt.%, the liquid silica gel 20wt.%;
graphene foam film thickness 450 μm and density 0.4g/cm 3 ;
Graphene foam film thermal conductivity 220W/(m K);
the surface of the graphene foam film is treated by adopting air atmosphere plasma, and the plasma power is 5KW;
the average pore diameter of the inner pores of the graphene foam membrane is 25 mu m, the pore diameters of the upper and lower through holes are 250 mu m, and the center distance of the through holes is 550 mu m;
the liquid silica gel is cyano-siloxysilane, which is diluted to a viscosity of 550 mPa.s by pentane;
curing temperature is 100 ℃;
through testing, the porosity of the sample is 71%, the heat conductivity coefficient is 185W/(m K), and the thermal resistance and compression rebound resilience of samples with different thicknesses are as follows:
example 7:
in this example, the graphene foam film accounts for 65wt.%, the liquid silica gel 35wt.%;
the thermal conductivity of the graphene foam film is 90W/(m K);
graphene foam film thickness 250 μm and density 0.18g/cm 3 ;
Nickel plating treatment is carried out on the surface of the graphene foam film, and the thickness of a nickel layer is 1 mu m;
the average pore diameter of the inner pores of the graphene foam membrane is 13 mu m, the pore diameters of the upper and lower through holes are 90 mu m, and the center-to-center distance of the through holes is 350 mu m;
the liquid silica gel is alpha, omega-diethyl polydimethylsiloxane, and is diluted to have the viscosity of 90 mPa.s by adopting pentane;
curing temperature is 90 ℃;
through testing, the porosity of the sample is 82%, the heat conductivity coefficient is 63W/(m K), and the thermal resistance and compression rebound resilience of samples with different thicknesses are as follows:
example 8:
in this example, the graphene foam film was 92wt.%, liquid silica gel was 8wt.%;
the thermal conductivity of the graphene foam film is 332W/(m K);
graphene foam film thickness 700 μm and density 0.65g/cm 3 ;
The average pore diameter of the inner pores of the graphene foam membrane is 70 mu m, the pore diameters of the upper and lower through holes are 450 mu m, and the center distance of the through holes is 900 mu m;
the liquid silica gel is polydimethyl cyclosiloxane-polydimethyl siloxane, and the liquid silica gel is diluted to have the viscosity of 750 mPa.s by adopting n-hexane-n-heptane;
curing temperature is 40 ℃;
through testing, the porosity of the sample is 65%, the heat conductivity coefficient is 305W/(m K), and the thermal resistance and compression rebound resilience of samples with different thicknesses are as follows:
example 9:
in this example, the graphene foam film accounts for 83wt.%, the liquid silica gel 17wt.%;
the thermal conductivity of the graphene foam film is 230W/(m K);
graphene foam film thickness 580 μm and density 0.45g/cm 3 ;
The average pore diameter of the inner pores of the graphene foam membrane is 70 mu m, the pore diameters of the upper and lower through holes are 450 mu m, and the center distance of the through holes is 900 mu m;
the liquid silica gel is polydimethyl cyclosiloxane-polydimethyl siloxane, and the liquid silica gel is diluted to have the viscosity of 750 mPa.s by adopting n-hexane-n-heptane;
solidifying under normal temperature;
through testing, the porosity of the sample is 71%, the heat conductivity coefficient is 188W/(m K), and the thermal resistance and compression rebound resilience of samples with different thicknesses are as follows:
example 10:
in this example, the graphene foam film accounts for 83wt.%, the liquid silica gel 17wt.%;
graphene foam film thickness 580 μm and density 0.45g/cm 3 ;
The thermal conductivity of the graphene foam film is 230W/(m K);
the average pore diameter of the inner pores of the graphene foam membrane is 70 mu m, the pore diameters of the upper and lower through holes are 450 mu m, and the center distance of the through holes is 900 mu m;
the liquid silica gel is polydimethylsiloxane-alpha, omega-dihydroxypolydimethylsiloxane, and is diluted to have the viscosity of 750 mPa.s by adopting tetrahydrofuran;
fully solidifying the liquid silica gel under normal temperature;
through testing, the porosity of the sample is 70%, the heat conductivity coefficient is 176W/(m K), and the thermal resistance and compression rebound resilience of samples with different thicknesses are as follows:
comparative example 1:
in this example, the graphene foam film accounts for 50wt.%, the liquid silica gel 50wt.%;
the graphene foam film has a thermal conductivity of 150W/(m K);
graphene foam film thickness 500 μm and density 0.3g/cm 3 ;
The average pore diameter of the inner pores of the graphene foam membrane is 70 mu m, the pore diameters of the upper and lower through holes are 450 mu m, and the center distance of the through holes is 900 mu m;
the liquid silica gel is polydimethyl cyclosiloxane, and is diluted to have the viscosity of 750 mPa.s by adopting tetrahydrofuran;
curing temperature is 100 ℃;
through testing, the porosity of the sample is 57%, the heat conductivity coefficient is 9W/(m K), and the thermal resistance and compression rebound resilience of samples with different thicknesses are as follows:
the heat conduction performance of the prepared sample is obviously reduced due to more liquid silica gel, and the application thermal resistance is obviously improved;
comparative example 2:
in this example, the graphene foam film accounts for 97wt.%, the liquid silica gel 3wt.%;
graphene foam film thickness 500 μm and density 0.3g/cm 3 ;
The thermal conductivity of the graphene foam film is 150W/(m K);
the average pore diameter of the inner pores of the graphene foam membrane is 70 mu m, the pore diameters of the upper and lower through holes are 450 mu m, and the center distance of the through holes is 900 mu m;
the liquid silica gel is polydimethylsiloxane-alpha, omega-dihydroxypolydimethylsiloxane, and is diluted to have the viscosity of 750 mPa.s by adopting tetrahydrofuran;
curing temperature is 120 ℃;
because of the small content of liquid silica gel used in this comparative example, the resulting sample cracked and could not be molded.
Comparative example 3:
in this example, the graphene foam film accounts for 80wt.%, the liquid silica gel 20wt.%;
the thermal conductivity of the graphene foam film is 150W/(m K);
graphene foam film thickness 1500 μm and density 0.3g/cm 3 ;
The average pore diameter of the inner pores of the graphene foam membrane is 70 mu m, the pore diameters of the upper and lower through holes are 450 mu m, and the center distance of the through holes is 900 mu m;
the liquid silica gel is polydimethyl cyclosiloxane, and is diluted to have the viscosity of 750 mPa.s by adopting tetrahydrofuran; the curing temperature is 80 ℃;
because the graphene foam film with the thickness of 1500 mu m is adopted, the liquid silica gel cannot be effectively impregnated into the foam film, so that the prepared heat conduction gasket is layered and cracked and cannot be molded.
Comparative example 4:
in this example, the graphene foam film accounts for 80wt.%, the liquid silica gel 20wt.%;
graphene foam film thickness 25 μm and density 0.3g/cm 3 ;
The average pore diameter of the inner pores of the graphene foam membrane is 70 mu m, the pore diameters of the upper and lower through holes are 450 mu m, and the center distance of the through holes is 900 mu m;
the liquid silica gel is polydimethyl cyclosiloxane, and is diluted to have the viscosity of 750 mPa.s by adopting tetrahydrofuran; curing temperature is 60 ℃;
because the graphene foam film with the thickness of 25 μm is adopted, the foam film has poor mechanical property, and is seriously damaged in the punching and soaking processes, so that a gasket sample cannot be obtained.
Comparative example 5:
in this example, the graphene foam film accounts for 80wt.%, the liquid silica gel 20wt.%;
the thermal conductivity of the graphene foam film is 41W/(m K);
graphene foam film thickness 400 μm and density 0.08g/cm 3 ;
The average pore diameter of the inner pores of the graphene foam membrane is 70 mu m, the pore diameters of the upper and lower through holes are 450 mu m, and the center distance of the through holes is 900 mu m;
the liquid silica gel is polydimethyl cyclosiloxane, and is diluted to have the viscosity of 750 mPa.s by adopting tetrahydrofuran; curing temperature is 60 ℃;
due to the adoption of the density of 0.1g/cm 3 The graphene foam film has poor mechanical properties, is seriously damaged in the punching and soaking processes, and cannot obtain a gasket sample.
Comparative example 6:
in this example, the graphene foam film accounts for 80wt.%, the liquid silica gel 20wt.%;
the thermal conductivity of the graphene foam film is 660W/(m K);
graphene foam film thickness 400 μm and density 1.3g/cm 3 ;
The average pore diameter of the inner pores of the graphene foam membrane is 70 mu m, the pore diameters of the upper and lower through holes are 450 mu m, and the center distance of the through holes is 900 mu m;
the liquid silica gel is polydimethyl cyclosiloxane, and is diluted to have the viscosity of 750 mPa.s by adopting tetrahydrofuran; the curing temperature is 80 ℃;
due to the adoption of the density of 1.3g/cm 3 The graphene foam film cannot be effectively impregnated into the foam film, so that the prepared heat conduction gasket is layered and cracked and cannot be molded.
Comparative example 7:
in this comparative example, the graphene foam film accounts for 80wt.%, the liquid silica gel 20wt.%;
the thermal conductivity of the graphene foam film is 150W/(m K);
graphene foam film thickness 400 μm and density 0.3gcm 3 ;
The average pore diameter of the internal pores of the graphene foam membrane is 30 mu m, the pore diameters of the upper and lower through holes are 450 mu m, and the center distance of the through holes is 900 mu m;
the liquid silica gel is polydimethyl cyclosiloxane, and is diluted to have the viscosity of 750 mPa.s by adopting tetrahydrofuran; curing temperature is 60 ℃;
the average pore diameter of the upper and lower through holes of the graphene foam membrane is only 30 mu m, so that the impregnation effect of the liquid silica gel in the graphene foam membrane is poor, and the heat conduction gasket is cracked and cannot be molded.
Comparative example 8:
in this example, the graphene foam film accounts for 80wt.%, the liquid silica gel 20wt.%;
the thermal conductivity of the graphene foam film is 150W/(m K);
graphene foam film thickness 400 μm and density 0.3g/cm 3 ;
The average pore diameter of the inner pores of the graphene foam membrane is 800 mu m, the pore diameters of the upper and lower through holes are 450 mu m, and the center distance of the through holes is 900 mu m; curing temperature is 60 ℃;
the liquid silica gel is polydimethyl cyclosiloxane, and is diluted to have the viscosity of 750 mPa.s by adopting tetrahydrofuran;
the average pore diameter of the upper and lower through holes of the graphene foam membrane is 600 mu m, and the pore diameter is too large, so that the mechanical property of the graphene foam is reduced, and the obtained heat-conducting gasket cannot be molded.
Comparative example 9:
in this comparative example, the graphene foam film accounts for 80wt.%, the liquid silica gel 20wt.%;
the thermal conductivity of the graphene foam film is 150W/(m K);
graphene foam film thickness 400 μm and density 0.3g/cm 3 ;
The average pore diameter of the internal pores of the graphene foam membrane is 300 mu m, the pore diameters of the upper and lower through holes are 450 mu m, and the center distance of the through holes is 200 mu m;
the liquid silica gel is polydimethyl cyclosiloxane, and is diluted to have the viscosity of 750 mPa.s by adopting tetrahydrofuran; curing temperature is 60 ℃;
because the center distance between the upper through holes and the lower through holes of the graphene foam film is 200 mu m, the through holes are too dense, the graphene foam film is easy to break and break, and the graphene foam film is not suitable for impregnating and preparing the heat conducting gaskets.
Comparative example 10:
in this example, the graphene foam film accounts for 80wt.%, the liquid silica gel 20wt.%;
the thermal conductivity of the graphene foam film is 150W/(m K);
graphene foam film thickness 400 μm and density 0.3g/cm 3 ;
The average pore diameter of the internal pores of the graphene foam membrane is 300 mu m, the pore diameters of the upper and lower through holes are 450 mu m, and the center distance of the through holes is 1500 mu m;
the liquid silica gel is polydimethyl cyclosiloxane, and is diluted to have the viscosity of 750 mPa.s by adopting tetrahydrofuran; curing temperature is 60 ℃;
because the center distance between the upper through hole and the lower through hole of the graphene foam film is 1500 mu m, the dipping effect of the liquid silica gel in the graphene foam film is poor, and the heat conduction gasket is cracked and cannot be molded.
Comparative example 11:
in this example, the graphene foam film accounts for 80wt.%, the liquid silica gel 20wt.%;
the thermal conductivity of the graphene foam film is 35W/(m K);
graphene foam film thickness 400 μm and density 0.2g/cm 3 ;
The average pore diameter of the internal pores of the graphene foam membrane is 300 mu m, the pore diameters of the upper and lower through holes are 450 mu m, and the center distance of the through holes is 1500 mu m; curing temperature is 60 ℃;
the liquid silica gel is polydimethyl cyclosiloxane, and is diluted to have the viscosity of 750 mPa.s by adopting tetrahydrofuran;
through testing, the porosity of the heat conduction gasket is 86%, and the heat conduction coefficient is 12W/(m K); the applied thermal resistances for the samples of different thickness were as follows:
the comparative example adopts the graphene foam film with the concentration of 35W/(m K), so that the thermal conductivity coefficient of the prepared thermal conductive gasket is obviously reduced, and the application thermal resistance is obviously increased.
Comparative example 12:
in this example, graphene foam film was 75wt.%, liquid silica gel 25wt.%;
graphene foam film thickness 300 μm and density 0.2g/cm 3 ;
The thermal conductivity of the graphene foam film is 102W/(m K);
the average pore diameter of the internal pores of the graphene foam membrane is 15 mu m, the pore diameters of the upper and lower through holes are 100 mu m, and the center distance of the through holes is 400 mu m;
the liquid silica gel is alpha, omega-dihydroxy polydimethylsiloxane, and is diluted to have the viscosity of 100 mPa.s by adopting tetrahydrofuran; curing temperature is 200 ℃;
the sample is destroyed and cracked due to the curing at 200 ℃.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present application, and the present application is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present application has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (18)
1. A graphene foam membrane reinforced thermally conductive gasket, comprising: the heat-conducting gasket comprises a multi-layer graphene foam film and an adhesive filled in the graphene foam film and between the graphene foam film, wherein the graphene foam film accounts for 60-95 wt% of the total weight of the heat-conducting gasket; stacking and bonding the impregnated graphene foam films layer by layer to form a block, and fully curing the adhesive; cutting the block into a plurality of sheets along the height direction of the layer stack; the graphene foam film comprises a plurality of first pores and a plurality of second pores, wherein the first pores penetrate through the graphene foam film in the thickness direction; the first pores and the second pores are filled with adhesive; the aperture of the second pores is 50-500 mu m, and the center-to-center distance between adjacent pores between the second pores is 300-1000 mu m; the surface roughening treatment enables the surface of the graphene foam film to have a roughness of 4-10 mu m;
the thermal conductivity of the graphene foam film is greater than or equal to 50W/(m.K); the density of the graphene foam film is 0.2-0.5g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The thickness of the graphene foam film is 50-1000 mu m; the graphene foam film is formed by coating, drying and heat treatment of graphene oxide slurry, and first pores are formed among graphene sheets in the graphene foam film;
the second holes which are communicated up and down are communicated with the first holes, and the first holes and the second holes inside are distributed with adhesives;
the aperture of the first pore is 10-100 mu m;
the first pores account for 60% -95% of the volume of the graphene foam film body;
the curing adopts heating curing or normal temperature curing under 150 ℃.
2. The graphene foam membrane-reinforced thermal gasket according to claim 1, wherein the graphene foam membrane has a thermal conductivity of 100W/(m-K) or more and a thickness of 300-500 μm.
3. The graphene foam membrane reinforced thermal pad of claim 1, wherein the graphene foam membrane comprises 75wt% to 90wt% of the total weight of the thermal pad.
4. The graphene foam membrane reinforced thermally conductive gasket of claim 1, wherein the porosity of the thermally conductive gasket is 50% -90%.
5. The graphene foam membrane-reinforced thermally conductive gasket of claim 1,
the aperture of the first pore is 15-50 mu m;
the first pores account for 75% -90% of the volume of the graphene foam film body;
the aperture of the second pore is 100-300 mu m;
the center-to-center spacing between the second pores is 400-800 μm.
6. The graphene foam membrane-reinforced thermal pad of claim 1, wherein the graphene foam membrane is aligned in the thermal pad in a thickness direction of the thermal pad;
the thickness of the heat conducting gasket is 0.1-5mm.
7. The graphene foam membrane reinforced thermally conductive gasket according to claim 1 wherein the adhesive is a compressible, compression resilient adhesive.
8. The graphene foam membrane-reinforced thermally conductive gasket of claim 7,
the adhesive adopts at least one of epoxy resin, phenolic resin, furfural resin, polyurethane, acrylic resin and organic silica gel.
9. The graphene foam membrane reinforced thermally conductive gasket according to claim 8 wherein the adhesive is selected from the group consisting of polydimethylsiloxane, α, ω -dihydroxypolydimethylsiloxane, polydiphenylsiloxane, α, ω -dihydroxypolymethyl3, 3, 3-trifluoropropyl siloxane, cyanosiloxysilane, α, ω -diethylpolydimethylsiloxane.
10. The method for preparing the graphene foam membrane reinforced heat-conducting gasket according to any one of claims 1 to 5, comprising:
taking a graphene foam film, wherein a plurality of first pores are formed in the graphene foam film;
punching the graphene foam film to form a plurality of second holes penetrating up and down in the thickness direction of the graphene foam film;
immersing the graphene foam film in an adhesive or an adhesive solution;
stacking and bonding the impregnated graphene foam films layer by layer to form a block, and fully curing the adhesive;
cutting the block into a plurality of slices along the height direction of the layer stack.
11. The method for preparing the graphene foam membrane reinforced heat-conducting gasket according to claim 10, wherein the graphene foam membrane is subjected to surface treatment.
12. The method for preparing a graphene foam membrane reinforced thermal pad according to claim 11, wherein the surface treatment is at least one of surface metallization treatment and plasma treatment.
13. The method of preparing a graphene foam membrane reinforced thermal pad according to claim 12 wherein the surface metallization treatment is copper plating, nickel plating, iron plating or silver plating;
the surface metallization treatment is carried out, and the thickness of a plating layer is 0.1-2 mu m; the plasma treatment is carried out in an air atmosphere, a nitrogen atmosphere or an oxygen atmosphere, and the plasma power is 1-10KW.
14. The method for preparing the graphene foam film reinforced heat-conducting gasket according to claim 13, wherein the surface metallization treatment is performed, and the thickness of a plating layer is 0.5-1 μm; the plasma treatment and the plasma power are 3-8KW.
15. The method for preparing the graphene foam membrane reinforced heat-conducting gasket according to claim 10, wherein,
the solvent of the adhesive solution adopts at least one of dimethylbenzene, ethanol, acetone, hexane, pentane, heptane, tetrahydrofuran, N-dimethylformamide and N-methylpyrrolidone;
the viscosity of the adhesive solution is 30-1000 mPa.s.
16. The method for preparing a graphene foam membrane reinforced thermal conductive gasket according to claim 15, wherein the viscosity of the adhesive solution is 100-500 mPa-s.
17. The method for preparing the graphene foam film reinforced heat-conducting gasket according to claim 10, wherein wire cutting, laser cutting, ultrasonic cutting, blade cutting or freezing cutting are adopted; cutting into sheet with thickness of 0.1-5mm.
18. The method for preparing a graphene foam membrane reinforced thermal conductive gasket according to claim 17, cutting into sheets with a thickness of 0.25-0.5mm.
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CN113510979B (en) * | 2021-07-15 | 2022-08-30 | 常州富烯科技股份有限公司 | Graphene composite heat conduction gasket and preparation method thereof |
CN115802694A (en) * | 2021-09-10 | 2023-03-14 | 荣耀终端有限公司 | Electronic equipment |
CN113817327A (en) * | 2021-10-26 | 2021-12-21 | 深圳烯材科技有限公司 | Preparation method of graphene-based composite material heat conduction pad |
CN114148044B (en) * | 2021-11-24 | 2024-04-19 | 常州富烯科技股份有限公司 | Graphene composite heat-conducting gasket and preparation method thereof |
CN114590803A (en) * | 2022-03-04 | 2022-06-07 | 浙江道明超导科技有限公司 | Manufacturing process of graphene heat dissipation film coiled material |
CN114801421A (en) * | 2022-04-27 | 2022-07-29 | 广东墨睿科技有限公司 | Preparation method of graphene heat-conducting gasket |
CN115141487B (en) * | 2022-07-12 | 2023-11-21 | 常州富烯科技股份有限公司 | Graphene heat conduction foam, graphene heat conduction gasket and preparation method |
CN115073793B (en) * | 2022-08-05 | 2023-07-18 | 常州富烯科技股份有限公司 | Graphene heat conducting film, preparation method thereof and heat conducting gasket |
CN115340767A (en) * | 2022-08-26 | 2022-11-15 | 安徽宇航派蒙健康科技股份有限公司 | High-thermal-conductivity insulating silica gel and preparation method thereof |
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