CN116948405A - Heat-conducting silica gel material, heat-conducting silica gel sheet and preparation method of heat-conducting silica gel sheet - Google Patents
Heat-conducting silica gel material, heat-conducting silica gel sheet and preparation method of heat-conducting silica gel sheet Download PDFInfo
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- CN116948405A CN116948405A CN202310717033.7A CN202310717033A CN116948405A CN 116948405 A CN116948405 A CN 116948405A CN 202310717033 A CN202310717033 A CN 202310717033A CN 116948405 A CN116948405 A CN 116948405A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 239000000741 silica gel Substances 0.000 title claims abstract description 86
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 86
- 239000000463 material Substances 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims description 16
- 239000000843 powder Substances 0.000 claims abstract description 65
- 229920002545 silicone oil Polymers 0.000 claims abstract description 57
- 239000000945 filler Substances 0.000 claims abstract description 45
- 239000002245 particle Substances 0.000 claims abstract description 37
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 32
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 32
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 31
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000016 photochemical curing Methods 0.000 claims abstract description 21
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 17
- 239000004945 silicone rubber Substances 0.000 claims abstract description 17
- 239000003112 inhibitor Substances 0.000 claims abstract description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 13
- 239000001257 hydrogen Substances 0.000 claims abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 13
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 13
- 239000003292 glue Substances 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 42
- 239000000243 solution Substances 0.000 claims description 34
- 230000001070 adhesive effect Effects 0.000 claims description 32
- 239000000853 adhesive Substances 0.000 claims description 30
- 238000002156 mixing Methods 0.000 claims description 24
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 21
- 239000004202 carbamide Substances 0.000 claims description 21
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 19
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 229910021389 graphene Inorganic materials 0.000 claims description 14
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 239000003638 chemical reducing agent Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 230000008569 process Effects 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000001723 curing Methods 0.000 claims description 10
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 9
- 239000006229 carbon black Substances 0.000 claims description 9
- 239000000460 chlorine Substances 0.000 claims description 9
- 229910052801 chlorine Inorganic materials 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 239000011347 resin Substances 0.000 claims description 9
- 229920005989 resin Polymers 0.000 claims description 9
- 238000003825 pressing Methods 0.000 claims description 8
- 229920001296 polysiloxane Polymers 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical class [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000003786 synthesis reaction Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 238000013329 compounding Methods 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- HDZGCSFEDULWCS-UHFFFAOYSA-N monomethylhydrazine Chemical compound CNN HDZGCSFEDULWCS-UHFFFAOYSA-N 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- WSLDIBCXIOECNX-UHFFFAOYSA-N octylhydrazine Chemical compound CCCCCCCCNN WSLDIBCXIOECNX-UHFFFAOYSA-N 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- VMAWODUEPLAHOE-UHFFFAOYSA-N 2,4,6,8-tetrakis(ethenyl)-2,4,6,8-tetramethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound C=C[Si]1(C)O[Si](C)(C=C)O[Si](C)(C=C)O[Si](C)(C=C)O1 VMAWODUEPLAHOE-UHFFFAOYSA-N 0.000 claims description 2
- DBAMUTGXJAWDEA-UHFFFAOYSA-N Butynol Chemical compound CCC#CO DBAMUTGXJAWDEA-UHFFFAOYSA-N 0.000 claims description 2
- MUQNAPSBHXFMHT-UHFFFAOYSA-N tert-butylhydrazine Chemical compound CC(C)(C)NN MUQNAPSBHXFMHT-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000017525 heat dissipation Effects 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 239000006185 dispersion Substances 0.000 abstract description 2
- 238000010030 laminating Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 7
- 239000011800 void material Substances 0.000 description 6
- 239000011231 conductive filler Substances 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- KUDUQBURMYMBIJ-UHFFFAOYSA-N 2-prop-2-enoyloxyethyl prop-2-enoate Chemical compound C=CC(=O)OCCOC(=O)C=C KUDUQBURMYMBIJ-UHFFFAOYSA-N 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- -1 acrylic ester Chemical class 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000001588 bifunctional effect Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- XKLVLDXNZDIDKQ-UHFFFAOYSA-N butylhydrazine Chemical group CCCCNN XKLVLDXNZDIDKQ-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Cooling Or The Like Of Semiconductors Or Solid State Devices (AREA)
Abstract
The invention relates to the field of heat conduction materials, and discloses a heat conduction silica gel material which comprises the following components in parts by mass: 15-40 parts of methyl vinyl silicone rubber, 5-15 parts of dimethyl silicone oil, 5-10 parts of first vinyl silicone oil, 0.4-0.6 part of hydrogen-containing silicone oil, 50-500 parts of heat conducting filler, 0.05-0.5 part of platinum catalyst, 6-35 parts of photo-curing glue, 0.04-0.05 part of inhibitor and 0.1-5 parts of silane coupling agent; this heat conduction silica gel material through adding modified graphene powder, can be in the silicone oil base member of heat conduction silica gel good even dispersion for the material heat dissipation is more smooth and easy, has effectually improved heat conduction silica gel material's heat conductivity, tensile strength, through the reasonable ratio to the heat conduction filler selection different particle diameters, laminating degree is inseparabler promptly, and the heat conduction effect is better.
Description
Technical Field
The invention relates to the field of heat conduction materials, in particular to a heat conduction silica gel material, a heat conduction silica gel sheet and a preparation method thereof.
Background
The heat-conducting silica gel sheet is a heat-conducting medium material which is synthesized by taking silica gel as a base material and adding various auxiliary materials such as metal oxide and the like through a special process, is also called a heat-conducting silica gel pad, a heat-conducting silica gel sheet, a soft heat-conducting pad, a heat-conducting silica gel pad and the like in the industry, is specially produced by using a design scheme of heat transfer of gaps, can fill the gaps, open a heat channel between a heating part and a heat dissipation part, effectively improves heat transfer efficiency, also plays roles of insulation, shock absorption, sealing and the like, can meet the design requirements of miniaturization and ultra-thinning of equipment, has manufacturability and usability, and has wide thickness application range, and is an excellent heat-conducting filling material; silica gel matrices have poor thermal conductivity and therefore require the addition of thermally conductive fillers to increase their thermal conductivity. In general, most of heat-conducting fillers such as copper, aluminum oxide, aluminum nitride and silicon carbide are applied in the market, the heat-conducting fillers adopt the same volume fraction or mass fraction to fill the heat-conducting silica gel matrix, and the heat conductivity is higher, but at the same time, the stretchability of the heat-conducting silica gel sheet is often greatly reduced along with the increase of the addition amount of the fillers, so that the performance stability of the heat-conducting silica gel sheet is affected.
Disclosure of Invention
(one) solving the technical problems
Aiming at the defects of the prior art, the invention provides a heat-conducting silica gel material, a heat-conducting silica gel sheet and a preparation method thereof, and solves the problems.
(II) technical scheme
In order to achieve the above purpose, the present invention provides the following technical solutions: the heat-conducting silica gel material comprises the following components in parts by mass: 15-40 parts of methyl vinyl silicone rubber, 5-15 parts of dimethyl silicone oil, 5-10 parts of first vinyl silicone oil, 0.4-0.6 part of hydrogen-containing silicone oil, 50-500 parts of heat conducting filler, 0.05-0.5 part of platinum catalyst, 6-35 parts of photo-curing glue, 0.04-0.05 part of inhibitor and 0.1-5 parts of silane coupling agent;
the photo-curing adhesive comprises the following components in parts by weight: the mass ratio of the resin to the glycol diacrylate to the photoinitiator is 3:1.5:1;
the heat conducting filler consists of modified graphene powder and aluminum oxide powder;
the heat conducting filler comprises 35-45% of 60-120 mu m particle size powder, 30-40% of 10-60 mu m particle size powder, 20-30% of 1-5 mu m particle size powder and 1-5% of 0.1-1 mu m particle size powder.
Preferably, the preparation method of the modified graphene comprises the following steps:
a, heating the graphene oxide solution to 50-60 ℃;
b, slowly adding a reducing agent into the graphene oxide solution, and reacting for 23-25 hours under the water bath condition of 65-75 ℃, wherein the volume ratio of the graphene oxide solution to the reducing agent is 1:10-15, and the dripping speed of the reducing agent is 0.1-0.12mL/s;
and c, carrying out centrifugal separation on the obtained solution after the reaction is finished, washing the solution to be neutral, and finally carrying out vacuum drying to obtain modified graphene powder.
Preferably, the reducing agent is compounded by one or more of R-group hydrazine, tertiary butyl hydrazine, methyl hydrazine and octyl hydrazine, wherein R is alkyl of 1-8 and isomers thereof.
The preparation method of the R-based hydrazine comprises the following steps:
adding concentrated sulfuric acid and urea into a synthesis device, and reacting for 1-3 hours at 15-25 ℃ in an ice bath condition, wherein the molar ratio is 2:1;
slowly dropwise adding R alcohol into a synthesis device, wherein the molar ratio of the R alcohol to urea is 1:1, carrying out heat preservation reaction for 3-5 hours at 20-25 ℃, then standing for 15-17 hours at room temperature, adding ammonia water to neutralize PH to 3-4, filtering and drying to obtain white crystal R-based urea;
c, dissolving R-based urea in ethanol, and then dropwise adding an ethanol solution containing chlorine into the device, wherein the chlorine and the R-based urea react for 0.2-1 hour at the temperature of 14-16 ℃ after the dropwise adding is finished, and the molar ratio of the chlorine to the R-based urea is 1.05:1.0;
and D, dissolving NaOH in water to prepare an aqueous solution, slowly dripping the aqueous solution into a device, keeping the temperature of 4-6 ℃ for reaction for 0.5-1.5 hours, wherein the mol ratio of the NaOH to the R-yl urea is 4.5-5.0:1.0, filtering the reaction solution, and heating the filtrate to obtain a fraction of 80-104 ℃ to obtain the special R-yl hydrazine.
Preferably, the methyl vinyl silicone rubber is formed by compounding second vinyl silicone oil, white carbon black and hexamethyldisilazane, and the mass ratio of the second vinyl silicone oil to the white carbon black to the hexamethyldisilazane is 11:4:1.
preferably, the viscosity of the second vinyl silicone oil is 3500-10000cps, the mass fraction of vinyl is 0.1-0.2%, the viscosity of the first vinyl silicone oil is 400-1000cps, and the mass fraction of vinyl is 0.28-0.52%.
Preferably, the inhibitor is one or two of tetramethyl tetravinyl cyclotetrasiloxane and butynol.
Preferably, the heat-conducting silica gel sheet is prepared from the heat-conducting silica gel material, and the preparation method comprises the following steps:
s1: heating the ethanol solution, adding a silane coupling agent into the heated ethanol solution for uniform mixing, adding aluminum oxide powder in the heat conducting filler into the mixed solution, stirring for 20min, and separating and drying the aluminum oxide powder to obtain oleophylic modified aluminum oxide powder;
s2: uniformly mixing methyl vinyl silicone rubber, dimethyl silicone oil, first vinyl silicone oil, hydrogen-containing silicone oil, photo-curing adhesive and inhibitor, then adding heat conducting filler in batches, adding platinum catalyst, uniformly stirring and mixing to obtain a heat conducting adhesive material, ensuring a vacuum state in the mixing process, and then pressing and curing the heat conducting adhesive material at 120 ℃ to obtain the heat conducting silica gel sheet.
(III) beneficial effects
Compared with the prior art, the invention provides a heat-conducting silica gel material and a heat-conducting silica gel sheet, which have the following beneficial effects:
1. according to the heat conduction silica gel material, the modified graphene powder is added, so that the heat conduction silica gel material can be well and evenly dispersed in a silicone oil matrix of the heat conduction silica gel, the heat dissipation of the material is smoother, the heat conductivity and the tensile strength of the heat conduction silica gel material are effectively improved, the curing time and the material viscosity of the heat conduction silica gel are optimized, and the heat conduction silica gel can be better used as a thermal interface composite material.
2. According to the heat-conducting silica gel material, through selecting the reasonable proportion of different particle sizes for the heat-conducting filler, gaps in a silica gel system can be filled more effectively, and gaps among large particles are filled through small particles, so that the gaps among the heat-conducting filler particles are further reduced, and meanwhile, the contact degree among the heat-conducting filler particles is higher, and the heat-conducting performance can be effectively improved. On the other hand, after the void ratio between the heat conducting fillers is reduced, the compressibility of the prepared silica gel heat conducting gasket is reduced, the elastic space between the heat radiating device and the heating device is reduced during assembly, and then the void degree between the heat radiating device and the heating device caused by elastic compression is reduced, namely the attaching degree is more compact, and the heat conducting effect is better.
3. The heat-conducting silica gel material is added through the photo-curing glue, so that the viscosity of the heat-conducting silica gel material can be changed, and the heat-conducting silica gel material can be used for obtaining heat-conducting silica gel sheets with different surface properties, so that the heat-conducting silica gel sheets provided by the invention can meet various special requirements.
Drawings
Fig. 1 is a schematic flow chart of a preparation method of the heat-conducting silica gel sheet.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1, a heat conductive silica gel material comprises the following components in parts by mass: 15-40 parts of methyl vinyl silicone rubber, 5-15 parts of dimethyl silicone oil, 5-10 parts of first vinyl silicone oil, 0.4-0.6 part of hydrogen-containing silicone oil, 50-500 parts of heat conducting filler, 0.05-0.5 part of platinum catalyst, 6-35 parts of photo-curing glue, 0.04-0.05 part of inhibitor and 0.1-5 parts of silane coupling agent;
the photo-curing adhesive comprises the following components in parts by weight: the mass ratio of the resin to the ethylene glycol diacrylate to the photoinitiator is 3:1.5:1, the ethylene glycol diacrylate is bifunctional acrylic ester, has higher reactivity and low toxicity, can react with the resin under the initiation of the photoinitiator, realizes the modification of the resin, changes the adhesive property of the resin, ensures that the adhesive property of the heat-conducting silicon material can be changed by adding the photo-curing adhesive, and can be used for obtaining the heat-conducting silicon sheet with different surface properties, so that the heat-conducting silicon sheet provided by the invention can meet various special requirements;
the heat-conducting filler consists of modified graphene powder and aluminum oxide powder, and the modified graphene powder can be well and uniformly dispersed in a silicone oil matrix of the heat-conducting silica gel, so that heat dissipation of the material is smoother, the heat conductivity and tensile strength of the heat-conducting silica gel material are effectively improved, the curing time and the material viscosity of the heat-conducting silica gel are optimized, and the heat-conducting silica gel can be better used as a thermal interface composite material;
the heat conducting filler comprises 35-45% of 60-120 mu m particle size powder, 30-40% of 10-60 mu m particle size powder, 20-30% of 1-5 mu m particle size powder and 1-5% of 0.1-1 mu m particle size powder; the heat conducting filler is reasonably proportioned with different particle sizes, so that gaps in a silica gel system can be filled more effectively, gaps among large particles are filled through small particles, gaps among the heat conducting filler particles are further reduced, the contact degree among the heat conducting filler particles is higher, and the heat conducting property can be effectively improved. On the other hand, after the void ratio between the heat conducting fillers is reduced, the compressibility of the prepared silica gel heat conducting gasket is reduced, the elastic space between the heat radiating device and the heating device is reduced during assembly, and then the void degree between the heat radiating device and the heating device caused by elastic compression is reduced, namely the attaching degree is more compact, and the heat conducting effect is better.
The preparation method of the modified graphene comprises the following steps:
a, heating the graphene oxide solution to 50-60 ℃;
b, slowly adding a reducing agent into the graphene oxide solution, and reacting for 23-25 hours under the water bath condition of 65-75 ℃, wherein the volume ratio of the graphene oxide solution to the reducing agent is 1:10-15, and the dripping speed of the reducing agent is 0.1-0.12mL/s;
and c, carrying out centrifugal separation on the obtained solution after the reaction is finished, washing the solution to be neutral, and finally carrying out vacuum drying to obtain modified graphene powder.
The reducing agent is compounded by one or more of R-group hydrazine, tert-butyl hydrazine, methyl hydrazine and octyl hydrazine, wherein R is alkyl of 1-8 and isomer thereof.
In the process of reducing graphene oxide by the compounded special reducing agent, the graphene microchip structure contains functional groups, the special oxygen-containing functional groups can be better connected with organic matter long chains such as silica gel and the like, so that the graphene microchip and the silica gel are effectively combined, the phenomena of poor dispersion and serious agglomeration of common graphene in the heat-conducting silica gel are improved, modified graphene powder can be well and evenly dispersed in a silicone oil matrix of the heat-conducting silica gel, heat dissipation of the material is smoother, heat conductivity and tensile strength of the heat-conducting silica gel material are effectively improved, and curing time and material viscosity of the heat-conducting silica gel are optimized, so that the heat-conducting silica gel can be better used as a thermal interface composite material.
The preparation method of the R-based hydrazine comprises the following steps:
adding concentrated sulfuric acid and urea into a synthesis device, and reacting for 1-3 hours at 15-25 ℃ in an ice bath condition, wherein the molar ratio is 2:1;
slowly dropwise adding R alcohol into a synthesis device, wherein the molar ratio of the R alcohol to urea is 1:1, carrying out heat preservation reaction for 3-5 hours at 20-25 ℃, then standing for 15-17 hours at room temperature, adding ammonia water to neutralize PH to 3-4, filtering and drying to obtain white crystal R-based urea;
c, dissolving R-based urea in ethanol, and then dropwise adding an ethanol solution containing chlorine into the device, wherein the chlorine and the R-based urea react for 0.2-1 hour at the temperature of 14-16 ℃ after the dropwise adding is finished, and the molar ratio of the chlorine to the R-based urea is 1.05:1.0;
and D, dissolving NaOH in water to prepare an aqueous solution, slowly dripping the aqueous solution into a device, keeping the reaction at the temperature of 4-6 ℃ for 0.5-1.5 hours, wherein the molar ratio of NaOH to R-based urea is 4.5-5.0:1.0, filtering the reaction solution, and heating the filtrate to obtain a fraction at the temperature of 80-104 ℃ to obtain the special R-based hydrazine.
The methyl vinyl silicone rubber is formed by compounding second vinyl silicone oil, white carbon black and hexamethyldisilazane, and the mass ratio of the second vinyl silicone oil to the white carbon black to the hexamethyldisilazane is 11:4:1, white carbon black can play the reinforcement effect, and hexamethyldisilazane can carry out surface treatment to white carbon black for white carbon black can mix with second vinyl silicone oil better, makes methyl vinyl silicone rubber's texture even, improves thermal conductivity and.
The viscosity of the second vinyl silicone oil is 3500-10000cps, the mass fraction of vinyl is 0.1-0.2%, the viscosity of the first vinyl silicone oil is 400-1000cps, and the mass fraction of vinyl is 0.28-0.52%.
The inhibitor is one or two of tetramethyl tetravinyl cyclosiloxane and butyl alkynol.
The heat-conducting silica gel sheet is prepared from the heat-conducting silica gel material, and the preparation method comprises the following steps:
s1: heating the ethanol solution, adding a silane coupling agent into the heated ethanol solution for uniform mixing, adding aluminum oxide powder in the heat conducting filler into the mixed solution, stirring for 20min, and separating and drying the aluminum oxide powder to obtain oleophylic modified aluminum oxide powder;
s2: uniformly mixing methyl vinyl silicone rubber, dimethyl silicone oil, first vinyl silicone oil, hydrogen-containing silicone oil, photo-curing adhesive and inhibitor, then adding heat conducting filler in batches, adding platinum catalyst, uniformly stirring and mixing to obtain a heat conducting adhesive material, ensuring a vacuum state in the mixing process, carrying out vacuumizing treatment in the stirring process and the pressing process of the preparation raw materials, effectively avoiding gas entering the heat conducting adhesive material in the stirring process and the pressing process, reducing air holes in the heat conducting adhesive material, and then pressing and curing the heat conducting adhesive material at 120 ℃ to obtain the heat conducting adhesive sheet.
Example 1
The heat-conducting silica gel material comprises the following components in parts by mass: 15 parts of methyl vinyl silicone rubber, 5 parts of dimethyl silicone oil, 5 parts of first vinyl silicone oil, 0.4 part of hydrogen-containing silicone oil, 50 parts of heat-conducting filler, 0.05 part of platinum catalyst, 6 parts of photo-curing adhesive, 0.04 part of inhibitor and 0.1 part of silane coupling agent;
the photo-curing adhesive comprises the following components in parts by weight: the mass ratio of the resin to the glycol diacrylate to the photoinitiator is 3:1.5:1;
the heat conducting filler consists of modified graphene powder and aluminum oxide powder;
the heat conductive filler comprises 40% of 90 μm particle size powder, 30% of 40 μm particle size powder, 25% of 3 μm particle size powder and 5% of 0.5 μm particle size powder.
The heat-conducting silica gel sheet is prepared from the heat-conducting silica gel material, and the preparation method comprises the following steps:
s1: heating the ethanol solution, adding a silane coupling agent into the heated ethanol solution for uniform mixing, adding aluminum oxide powder in the heat conducting filler into the mixed solution, stirring for 20min, and separating and drying the aluminum oxide powder to obtain oleophylic modified aluminum oxide powder;
s2: uniformly mixing methyl vinyl silicone rubber, dimethyl silicone oil, first vinyl silicone oil, hydrogen-containing silicone oil, photo-curing adhesive and inhibitor, then adding heat conducting filler in batches, adding platinum catalyst, uniformly stirring and mixing to obtain a heat conducting adhesive material, ensuring a vacuum state in the mixing process, and then pressing and curing the heat conducting adhesive material at 120 ℃ to obtain the heat conducting silica gel sheet.
Example two
The heat-conducting silica gel material comprises the following components in parts by mass: 28 parts of methyl vinyl silicone rubber, 10 parts of dimethyl silicone oil, 8 parts of first vinyl silicone oil, 0.5 part of hydrogen-containing silicone oil, 300 parts of heat conducting filler, 0.3 part of platinum catalyst, 20 parts of photo-curing glue, 0.045 part of inhibitor and 2.5 parts of silane coupling agent;
the photo-curing adhesive comprises the following components in parts by weight: the mass ratio of the resin to the glycol diacrylate to the photoinitiator is 3:1.5:1;
the heat conducting filler consists of modified graphene powder and aluminum oxide powder;
the heat conductive filler comprises 40% of 90 μm particle size powder, 30% of 40 μm particle size powder, 25% of 3 μm particle size powder and 5% of 0.5 μm particle size powder.
The heat-conducting silica gel sheet is prepared from the heat-conducting silica gel material, and the preparation method comprises the following steps:
s1: heating the ethanol solution, adding a silane coupling agent into the heated ethanol solution for uniform mixing, adding aluminum oxide powder in the heat conducting filler into the mixed solution, stirring for 20min, and separating and drying the aluminum oxide powder to obtain oleophylic modified aluminum oxide powder;
s2: uniformly mixing methyl vinyl silicone rubber, dimethyl silicone oil, first vinyl silicone oil, hydrogen-containing silicone oil, photo-curing adhesive and inhibitor, then adding heat conducting filler in batches, adding platinum catalyst, uniformly stirring and mixing to obtain a heat conducting adhesive material, ensuring a vacuum state in the mixing process, and then pressing and curing the heat conducting adhesive material at 120 ℃ to obtain the heat conducting silica gel sheet.
Example III
The heat-conducting silica gel material comprises the following components in parts by mass: 40 parts of methyl vinyl silicone rubber, 15 parts of dimethyl silicone oil, 10 parts of first vinyl silicone oil, 0.6 part of hydrogen-containing silicone oil, 500 parts of heat-conducting filler, 0.5 part of platinum catalyst, 35 parts of photo-curing adhesive, 0.05 part of inhibitor and 5 parts of silane coupling agent;
the photo-curing adhesive comprises the following components in parts by weight: the mass ratio of the resin to the glycol diacrylate to the photoinitiator is 3:1.5:1;
the heat conducting filler consists of modified graphene powder and aluminum oxide powder;
the heat conductive filler comprises 40% of 90 μm particle size powder, 30% of 40 μm particle size powder, 25% of 3 μm particle size powder and 5% of 0.5 μm particle size powder.
The heat-conducting silica gel sheet is prepared from the heat-conducting silica gel material, and the preparation method comprises the following steps:
s1: heating the ethanol solution, adding a silane coupling agent into the heated ethanol solution for uniform mixing, adding aluminum oxide powder in the heat conducting filler into the mixed solution, stirring for 20min, and separating and drying the aluminum oxide powder to obtain oleophylic modified aluminum oxide powder;
s2: uniformly mixing methyl vinyl silicone rubber, dimethyl silicone oil, first vinyl silicone oil, hydrogen-containing silicone oil, photo-curing adhesive and inhibitor, then adding heat conducting filler in batches, adding platinum catalyst, uniformly stirring and mixing to obtain a heat conducting adhesive material, ensuring a vacuum state in the mixing process, and then pressing and curing the heat conducting adhesive material at 120 ℃ to obtain the heat conducting silica gel sheet.
Comparative example one
The heat conducting filler in the embodiment is composed of common graphene and aluminum oxide powder, and the rest is the same.
Comparative example two
The powder materials of the heat conductive filler in the second embodiment are all 2.5 μm powder materials, and the rest are the same.
Experimental test
Thermal conductivity: the thermal conductivity coefficients of the thermal silicon sheets prepared according to examples one to three and comparative example one and two were tested according to astm d5470 standard; mechanical properties: test tensile strength of thermally conductive silicone sheets prepared according to examples one to three and comparative example one to two were measured according to astm d412 standard; shore hardness: the heat conductive silicone sheets prepared according to examples one to three and comparative example one and two were tested for shore hardness according to astm d2440 standard; the test results are shown in the following table:
| group of | Coefficient of thermal conductivity (W/m.k) | Tensile Strength (MPa) | Shore hardness (Shore 00) |
| Example 1 | 3.12 | 0.43 | 63.2 |
| Example two | 3.56 | 0.49 | 62.5 |
| Example III | 3.28 | 0.41 | 62.9 |
| Comparative example one | 2.86 | 0.28 | 66.3 |
| Comparative example two | 2.73 | 0.35 | 68.2 |
According to the data, the heat-conducting silica gel sheet prepared by the heat-conducting silica gel material can be well and evenly dispersed in a silicone oil matrix of the heat-conducting silica gel by adding the modified graphene powder, so that the heat dissipation of the material is smoother, the heat conductivity and the tensile strength of the heat-conducting silica gel material are effectively improved, the curing time and the material viscosity of the heat-conducting silica gel are optimized, and the heat-conducting silica gel can be better used as a thermal interface composite material;
through selecting the reasonable ratio of different particle diameters to the heat conduction filler, can fill the space in the silica gel system more effectively, pack the clearance between the big granule through the tiny particle simultaneously for the clearance between the heat conduction filler granule further reduces simultaneously the contact degree between the heat conduction filler granule is higher, can effectively promote heat conductivility. On the other hand, after the void ratio between the heat conducting fillers is reduced, the compressibility of the prepared silica gel heat conducting gasket is reduced, the elastic space between the heat radiating device and the heating device is reduced during assembly, and then the void degree between the heat radiating device and the heating device caused by elastic compression is reduced, namely the attaching degree is more compact, and the heat conducting effect is better.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. The heat-conducting silica gel material is characterized by comprising the following components in parts by mass: 15-40 parts of methyl vinyl silicone rubber, 5-15 parts of dimethyl silicone oil, 5-10 parts of first vinyl silicone oil, 0.4-0.6 part of hydrogen-containing silicone oil, 50-500 parts of heat conducting filler, 0.05-0.5 part of platinum catalyst, 6-35 parts of photo-curing glue, 0.04-0.05 part of inhibitor and 0.1-5 parts of silane coupling agent;
the photo-curing adhesive comprises the following components in parts by weight: the mass ratio of the resin to the glycol diacrylate to the photoinitiator is 3:1.5:1;
the heat conducting filler consists of modified graphene powder and aluminum oxide powder;
the heat conducting filler comprises 35-45% of 60-120 mu m particle size powder, 30-40% of 10-60 mu m particle size powder, 20-30% of 1-5 mu m particle size powder and 1-5% of 0.1-1 mu m particle size powder.
2. The heat conducting silica gel material according to claim 1, wherein the preparation method of the modified graphene comprises the following steps:
a, heating the graphene oxide solution to 50-60 ℃;
b, slowly adding a reducing agent into the graphene oxide solution, and reacting for 23-25 hours under the water bath condition of 65-75 ℃, wherein the volume ratio of the graphene oxide solution to the reducing agent is 1:10-15, and the dripping speed of the reducing agent is 0.1-0.12mL/s;
and c, carrying out centrifugal separation on the obtained solution after the reaction is finished, washing the solution to be neutral, and finally carrying out vacuum drying to obtain modified graphene powder.
3. The heat-conducting silica gel material according to claim 2, wherein the reducing agent is compounded by one or more of R-based hydrazine, tert-butyl hydrazine, methyl hydrazine and octyl hydrazine, wherein R is an alkyl group of 1-8 or an isomer thereof.
4. A thermally conductive silicone material as set forth in claim 3 wherein said R-based hydrazine is prepared by the process of:
adding concentrated sulfuric acid and urea into a synthesis device, and reacting for 1-3 hours at 15-25 ℃ in an ice bath condition, wherein the molar ratio is 2:1;
slowly dropwise adding R alcohol into a synthesis device, wherein the molar ratio of the R alcohol to urea is 1:1, carrying out heat preservation reaction for 3-5 hours at 20-25 ℃, then standing for 15-17 hours at room temperature, adding ammonia water to neutralize PH to 3-4, filtering and drying to obtain white crystal R-based urea;
c, dissolving R-based urea in ethanol, and then dropwise adding an ethanol solution containing chlorine into the device, wherein the chlorine and the R-based urea react for 0.2-1 hour at the temperature of 14-16 ℃ after the dropwise adding is finished, and the molar ratio of the chlorine to the R-based urea is 1.05:1.0;
and D, dissolving NaOH in water to prepare an aqueous solution, slowly dripping the aqueous solution into a device, keeping the temperature of 4-6 ℃ for reaction for 0.5-1.5 hours, wherein the mol ratio of the NaOH to the R-yl urea is 4.5-5.0:1.0, filtering the reaction solution, and heating the filtrate to obtain a fraction of 80-104 ℃ to obtain the special R-yl hydrazine.
5. The heat-conducting silica gel material according to claim 1, wherein the methyl vinyl silicone rubber is formed by compounding second vinyl silicone oil, white carbon black and hexamethyldisilazane, and the mass ratio of the second vinyl silicone oil, the white carbon black and the hexamethyldisilazane is 11:4:1.
6. the heat conductive silicone material as set forth in claim 5, wherein the second vinyl silicone oil has a viscosity of 3500-10000cps and a vinyl mass fraction of 0.1-0.2%, and the first vinyl silicone oil has a viscosity of 400-1000cps and a vinyl mass fraction of 0.28-0.52%.
7. The heat conductive silica gel material of claim 1 wherein the inhibitor is one or both of tetramethyl tetravinyl cyclotetrasiloxane and butynol.
8. A thermally conductive silicone sheet made of the thermally conductive silicone material of claim 1.
9. A method of making a thermally conductive silicone sheet as set forth in claim 8, comprising the steps of:
s1: heating the ethanol solution, adding a silane coupling agent into the heated ethanol solution for uniform mixing, adding aluminum oxide powder in the heat conducting filler into the mixed solution, stirring for 20min, and separating and drying the aluminum oxide powder to obtain oleophylic modified aluminum oxide powder;
s2: uniformly mixing methyl vinyl silicone rubber, dimethyl silicone oil, first vinyl silicone oil, hydrogen-containing silicone oil, photo-curing adhesive and inhibitor, then adding heat conducting filler in batches, adding platinum catalyst, uniformly stirring and mixing to obtain a heat conducting adhesive material, ensuring a vacuum state in the mixing process, and then pressing and curing the heat conducting adhesive material at 120 ℃ to obtain the heat conducting silica gel sheet.
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| CN117801341A (en) * | 2023-12-29 | 2024-04-02 | 江苏诺德新材料股份有限公司 | Graphene heat-conducting insulating silicon wafer and preparation method thereof |
| CN117844256A (en) * | 2024-01-11 | 2024-04-09 | 东莞建盟新材料有限公司 | Heat-conducting silica gel composition and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117801341A (en) * | 2023-12-29 | 2024-04-02 | 江苏诺德新材料股份有限公司 | Graphene heat-conducting insulating silicon wafer and preparation method thereof |
| CN117844256A (en) * | 2024-01-11 | 2024-04-09 | 东莞建盟新材料有限公司 | Heat-conducting silica gel composition and preparation method thereof |
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