CN116462974B - Heat-conducting silica gel sheet and preparation method thereof - Google Patents
Heat-conducting silica gel sheet and preparation method thereof Download PDFInfo
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- CN116462974B CN116462974B CN202310482284.1A CN202310482284A CN116462974B CN 116462974 B CN116462974 B CN 116462974B CN 202310482284 A CN202310482284 A CN 202310482284A CN 116462974 B CN116462974 B CN 116462974B
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000000741 silica gel Substances 0.000 title claims abstract description 48
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 229920002545 silicone oil Polymers 0.000 claims abstract description 51
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 44
- 239000001257 hydrogen Substances 0.000 claims abstract description 42
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 42
- 239000003054 catalyst Substances 0.000 claims abstract description 27
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 10
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 10
- 239000000945 filler Substances 0.000 claims abstract description 9
- 239000003112 inhibitor Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 39
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 38
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 27
- 239000000835 fiber Substances 0.000 claims description 27
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical group [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 23
- 239000003607 modifier Substances 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 20
- 239000002131 composite material Substances 0.000 claims description 19
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 19
- 229910052697 platinum Inorganic materials 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 16
- 230000001070 adhesive effect Effects 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- 229920001296 polysiloxane Polymers 0.000 claims description 13
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical group C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 12
- DMWVYCCGCQPJEA-UHFFFAOYSA-N 2,5-bis(tert-butylperoxy)-2,5-dimethylhexane Chemical group CC(C)(C)OOC(C)(C)CCC(C)(C)OOC(C)(C)C DMWVYCCGCQPJEA-UHFFFAOYSA-N 0.000 claims description 12
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 12
- 239000000853 adhesive Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000001291 vacuum drying Methods 0.000 claims description 11
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 10
- 238000010041 electrostatic spinning Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- RFVVBBUVWAIIBT-UHFFFAOYSA-N beryllium nitrate Chemical compound [Be+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O RFVVBBUVWAIIBT-UHFFFAOYSA-N 0.000 claims description 8
- 238000003490 calendering Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000003292 glue Substances 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 239000000499 gel Substances 0.000 claims description 7
- POPVULPQMGGUMJ-UHFFFAOYSA-N octasilsesquioxane cage Chemical compound O1[SiH](O[SiH](O2)O[SiH](O3)O4)O[SiH]4O[SiH]4O[SiH]1O[SiH]2O[SiH]3O4 POPVULPQMGGUMJ-UHFFFAOYSA-N 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 6
- GAGGCOKRLXYWIV-UHFFFAOYSA-N europium(3+);trinitrate Chemical compound [Eu+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GAGGCOKRLXYWIV-UHFFFAOYSA-N 0.000 claims description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 5
- 230000005684 electric field Effects 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims description 2
- 238000013016 damping Methods 0.000 abstract description 6
- 230000000052 comparative effect Effects 0.000 description 28
- 238000012360 testing method Methods 0.000 description 17
- 239000000203 mixture Substances 0.000 description 9
- FRWYFWZENXDZMU-UHFFFAOYSA-N 2-iodoquinoline Chemical compound C1=CC=CC2=NC(I)=CC=C21 FRWYFWZENXDZMU-UHFFFAOYSA-N 0.000 description 6
- LTPBRCUWZOMYOC-UHFFFAOYSA-N beryllium oxide Inorganic materials O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 description 6
- 239000006258 conductive agent Substances 0.000 description 6
- 229910001940 europium oxide Inorganic materials 0.000 description 6
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 description 6
- 230000035939 shock Effects 0.000 description 6
- 230000003068 static effect Effects 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 238000012546 transfer Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000013100 final test Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- 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
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use 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; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
- C08J2383/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use 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; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/05—Polysiloxanes containing silicon bound to hydrogen
-
- 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
- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
-
- 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
-
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/08—Oxygen-containing compounds
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
Abstract
The invention provides a heat-conducting silica gel sheet which is prepared from the following raw materials in parts by weight: 6-10 parts of vinyl end-capped silicone oil, 2-4 parts of end-side hydrogen-containing silicone oil, 2-3 parts of filler, 0.5-1 part of catalyst, 0.4-0.8 part of vulcanizing agent, 0.2-0.3 part of inhibitor and 50-55 parts of heat conducting agent. The invention also provides a preparation method of the heat-conducting silica gel sheet. The heat-conducting silica gel sheet provided by the invention has better heat-conducting property, damping property and bonding property.
Description
Technical Field
The invention relates to a heat-conducting silica gel sheet and a preparation method thereof.
Background
The heat-conducting silica gel sheet is a heat-conducting medium material synthesized by a special process by taking silica gel as a base material and adding various auxiliary materials such as metal oxide, and 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. The heat-conducting silica gel gasket has the characteristics of certain flexibility, self-adhesion, better heat conductivity, compressibility, weather resistance, insulation or high impact voltage resistance and the like, and can guide heat transfer between a heating part and a heat dissipation part, so that the heat-conducting silica gel gasket is widely used in the heat conduction field of electronic and electric appliances. The current heat-conducting silica gel sheet has some problems: if the heat conducting silicone sheet itself has limited heat conducting performance, a heat conducting filler is generally required to be added to improve the heat conducting performance, but after the heat conducting performance is improved, other performances of the heat conducting silicone sheet, such as damping performance, bonding performance and the like, can be weakened.
The invention with the application number of CN202210632510.5 discloses a heat-conducting silica gel sheet and a preparation method thereof, wherein the preparation method comprises the following steps: s1, respectively preparing a first mixture, a second mixture and a third mixture; s2, flatly paving the first mixture in a container, heating for solidification, and then cooling; s3, spreading the second mixture on the solidified first mixture, heating and solidifying, and then cooling; s4, repeating the steps S2 and S3 to obtain a primary product of the heat-conducting silica gel sheet; s5, spreading the third mixture on the primary product of the heat-conducting silica gel sheet, and vulcanizing to obtain the heat-conducting silica gel sheet. The heat-conducting silica gel sheet has the problems that the actual heat-conducting property is not ideal, and the shock absorption property and the bonding property are poor.
Disclosure of Invention
The invention aims to solve the technical problem of providing a heat-conducting silica gel sheet which has better heat-conducting property, damping property and bonding property.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a heat-conducting silica gel sheet is prepared from the following raw materials in parts by weight: 6-10 parts of vinyl end-capped silicone oil, 2-4 parts of end-side hydrogen-containing silicone oil, 2-3 parts of filler, 0.5-1 part of catalyst, 0.4-0.8 part of vulcanizing agent, 0.2-0.3 part of inhibitor and 50-55 parts of heat conducting agent.
Further, the vinyl content of the vinyl-terminated silicone oil is 1-1.5wt%, and the hydrogen content of the terminal hydrogen-containing silicone oil is 0.2-0.6wt%.
Further, the filler is calcium carbonate.
Further, the catalyst of the invention is a platinum catalyst.
Further, the vulcanizing agent is 2, 5-dimethyl-2, 5-di (tert-butyl peroxy) hexane.
Further, the inhibitor of the present invention is ethynyl cyclohexanol.
Further, the preparation steps of the heat conducting agent provided by the invention are as follows:
A1. adding europium nitrate into water, mixing uniformly to obtain a first solution, adding beryllium nitrate into water, mixing uniformly to obtain a second solution, adding polyvinylpyrrolidone into absolute ethyl alcohol, mixing uniformly to obtain a third solution, mixing the first solution, the second solution and the third solution, carrying out water bath at 65 ℃ for 45 minutes to obtain sol, transferring the sol into an electrostatic spinning machine, carrying out electrostatic spinning to obtain gel fibers, heating the gel fibers in a muffle furnace to 600 ℃, and then preserving heat for 3 hours to obtain composite fibers for later use;
A2. adding hydrogen-containing silicone oil at the end side, a platinum catalyst and octavinyl octasilsesquioxane into N, N-dimethylformamide under the protection of nitrogen, heating to 100 ℃, stirring and reacting for 10 hours, and evaporating the N, N-dimethylformamide under reduced pressure to obtain a modifier for later use;
A3. and (3) adding the modifier obtained in the step A2 into tetrahydrofuran, uniformly mixing to obtain a modifier solution, immersing the composite fiber obtained in the step A1 into the modifier solution, standing for 12 hours, transferring into a vacuum drying oven, drying at 180 ℃ for 2 hours, and taking out to obtain the heat conducting agent.
Further, in the preparation step A1 of the heat conducting agent, the concentration of the solution A is 8wt%, the concentration of the solution B is 2wt%, the mass ratio of polyvinylpyrrolidone to absolute ethyl alcohol in the solution C is 1:15, and the ratio of the solution A to the solution B to the solution C is 10g:9g:6mL; during electrostatic spinning, the inner diameter of the spinneret is 0.9mm, the distance between the spinneret and the receiving plate is 20cm, the sample injection amount is 0.5 mL/hour, and the external electric field is 20kV; the temperature rising speed of the muffle furnace is 2 ℃/min; in the preparation step A2 of the heat conducting agent, the hydrogen content of the end-side hydrogen-containing silicone oil is 1wt%, and the ratio of the end-side hydrogen-containing silicone oil, the platinum catalyst, the octavinyl octasilsesquioxane and the N, N-dimethylformamide is 10g:0.1g:4g:20mL; in the preparation step A3 of the heat conducting agent, the proportion of the modifier obtained in the step A2, tetrahydrofuran and the composite fiber obtained in the step A1 is 9g:80mL:12g.
Another technical problem to be solved by the present invention is to provide a method for preparing the above-mentioned heat conductive silicon sheet,
in order to solve the technical problems, the technical scheme is as follows:
a preparation method of a heat-conducting silica gel sheet comprises the following steps:
B1. weighing the raw materials according to parts by weight, sequentially adding vinyl-terminated silicone oil, terminal hydrogen-containing silicone oil, a catalyst and an inhibitor into a reaction kettle, and stirring for 1-2 hours at 100-120 ℃ to obtain a base material;
B2. adding filler, vulcanizing agent and heat conducting agent into the base material obtained in the step B1, and stirring for 30-60 minutes at normal temperature to obtain heat conducting glue;
B3. and B2, calendaring and molding the heat-conducting adhesive obtained in the step B2 by using a calendar, making a sheet, then transferring the sheet into a vacuum drying oven, drying at 100 ℃ for 2 hours, and taking out the sheet to obtain the heat-conducting silica gel sheet.
Further, the stirring speed in the step B1 is 30rpm, and the stirring speed in the step B2 is 60rpm.
Compared with the prior art, the invention has the following beneficial effects:
1) According to the invention, europium nitrate, beryllium nitrate and the like are used as raw materials to prepare the composite fiber through a solvent gel method and electrostatic spinning, the composite fiber is formed by compounding europium oxide and beryllium oxide, the beryllium oxide has high heat conductivity coefficient, and the europium oxide has good damping performance, so that the composite fiber can effectively improve the heat conductivity and damping performance of a silica gel sheet, and compared with a powder form, the composite fiber has a better effect of improving the heat conductivity of the silica gel sheet.
2) The surface properties of the composite fiber prepared by the invention and the vinyl-terminated silicone oil and the terminal hydrogen-containing silicone oil are different to a certain extent, and the effect is poor if the composite fiber is directly mixed, so that the composite fiber is pretreated by using the modifier, and the modifier is prepared by reacting the terminal hydrogen-containing silicone oil and octavinyl octasilsesquioxane under the catalysis of a platinum catalyst, so that the dispersibility of the composite fiber in the vinyl-terminated silicone oil and the terminal hydrogen-containing silicone oil can be effectively improved, and the heat conduction performance and the shock absorption performance of a silica gel sheet are further improved; in addition, the modifier can play a better role in tackifying, and can effectively improve the adhesive property of the silica gel sheet.
3) The heat-conducting silica gel sheet prepared by the invention is specially produced by using the design scheme of heat transfer of gaps, can fill the gaps, opens up the heat-conducting channel between the heating part and the heat-radiating part, effectively improves the heat transfer efficiency, plays roles of insulation, shock absorption, sealing and the like, can meet the design requirements of equipment miniaturization and ultra-thin, and has wide application range.
Description of the embodiments
The present invention will be described in detail with reference to specific examples, wherein the exemplary embodiments of the present invention and the descriptions thereof are provided for the purpose of illustrating the present invention, but are not to be construed as limiting the present invention.
Examples
The heat-conducting silica gel sheet is prepared from the following raw materials in parts by weight: 8 parts of vinyl-terminated silicone oil with the vinyl content of 1.2wt%, 3 parts of terminal hydrogen-containing silicone oil with the hydrogen content of 0.5wt%, 2.5 parts of calcium carbonate, 0.8 part of platinum catalyst, 0.6 part of 2, 5-dimethyl-2, 5-di (tert-butyl peroxy) hexane, 0.3 part of ethynyl cyclohexanol and 54 parts of heat conducting agent.
The preparation steps of the heat conducting agent are as follows:
A1. adding europium nitrate into water, mixing uniformly to obtain a solution A with the concentration of 8wt%, adding beryllium nitrate into water, mixing uniformly to obtain a solution B with the concentration of 2wt%, adding polyvinylpyrrolidone into absolute ethyl alcohol, mixing uniformly to obtain a solution C, mixing the solution A, the solution B and the solution C with the mass ratio of polyvinylpyrrolidone to absolute ethyl alcohol of 1:15, mixing 10g:9g:6mL of solution A, solution B and solution C in a water bath at 65 ℃ for 45 minutes to obtain sol, transferring the sol into an electrostatic spinning machine, carrying out electrostatic spinning to obtain gel fibers, wherein during electrostatic spinning, the inner diameter of a spinneret is 0.9mm, the distance between the spinneret and a receiving plate is 20cm, the sample feeding amount is 0.5 mL/hour, an external electric field is 20kV, and placing the gel fibers in a muffle furnace, heating to 600 ℃ at the heating rate of 2 ℃/min, and then preserving the temperature for 3 hours to obtain composite fibers for later use;
A2. adding end side hydrogen silicone oil with hydrogen content of 1wt%, platinum catalyst and octavinyl octasilsesquioxane into N, N-dimethylformamide under the protection of nitrogen, heating to 100 ℃, stirring and reacting for 10 hours, and evaporating N, N-dimethylformamide under reduced pressure to obtain a modifier for later use, wherein the ratio of the end side hydrogen silicone oil to the platinum catalyst to the octavinyl octasilsesquioxane to the N, N-dimethylformamide is 10g:0.1g:4g:20mL;
A3. adding the modifier obtained in the step A2 into tetrahydrofuran, uniformly mixing to obtain a modifier solution, immersing the composite fiber obtained in the step A1 into the modifier solution, standing for 12 hours, transferring into a vacuum drying oven, drying at 180 ℃ for 2 hours, and taking out to obtain a heat conducting agent, wherein the ratio of the modifier obtained in the step A2 to the composite fiber obtained in the step A1 is 9g:80mL:12g.
The preparation method of example 1 comprises the following steps:
B1. weighing the raw materials according to the weight parts, sequentially adding vinyl-terminated silicone oil, terminal hydrogen-containing silicone oil, platinum catalyst and ethynyl cyclohexanol into a reaction kettle, and stirring at the speed of 30rpm at 110 ℃ for 1.5 hours to obtain a base material;
B2. adding calcium carbonate, 2, 5-dimethyl-2, 5-di (tert-butyl peroxy) hexane and a heat conducting agent into the base material obtained in the step B1, and stirring at the normal temperature for 45 minutes at the speed of 60rpm to obtain heat conducting glue;
B3. and B2, calendaring and molding the heat-conducting adhesive obtained in the step B2 by using a calendar, making a sheet, then transferring the sheet into a vacuum drying oven, drying at 100 ℃ for 2 hours, and taking out the sheet to obtain the heat-conducting silica gel sheet.
Examples
The heat-conducting silica gel sheet is prepared from the following raw materials in parts by weight: 10 parts of vinyl-terminated silicone oil with the vinyl content of 1wt%, 2 parts of terminal hydrogen-containing silicone oil with the hydrogen content of 0.3wt%, 2 parts of calcium carbonate, 0.5 part of platinum catalyst, 0.8 part of 2, 5-dimethyl-2, 5-di (tert-butyl peroxy) hexane, 0.2 part of ethynyl cyclohexanol and 50 parts of heat conducting agent. The procedure for preparing the heat-conducting agent was the same as in example 1.
The preparation method of example 2 comprises the following steps:
B1. weighing the raw materials according to the weight parts, sequentially adding vinyl-terminated silicone oil, terminal hydrogen-containing silicone oil, platinum catalyst and ethynyl cyclohexanol into a reaction kettle, and stirring at the speed of 30rpm at 120 ℃ for 1 hour to obtain a base material;
B2. adding calcium carbonate, 2, 5-dimethyl-2, 5-di (tert-butyl peroxy) hexane and a heat conducting agent into the base material obtained in the step B1, and stirring at the normal temperature for 30 minutes at the speed of 60rpm to obtain heat conducting glue;
B3. and B2, calendaring and molding the heat-conducting adhesive obtained in the step B2 by using a calendar, making a sheet, then transferring the sheet into a vacuum drying oven, drying at 100 ℃ for 2 hours, and taking out the sheet to obtain the heat-conducting silica gel sheet.
Examples
The heat-conducting silica gel sheet is prepared from the following raw materials in parts by weight: 6 parts of vinyl-terminated silicone oil with vinyl content of 1.5wt%, 4 parts of terminal hydrogen-containing silicone oil with hydrogen content of 0.4wt%, 3 parts of calcium carbonate, 1 part of platinum catalyst, 0.4 part of 2, 5-dimethyl-2, 5-di (tert-butyl peroxy) hexane, 0.3 part of ethynyl cyclohexanol and 55 parts of heat conducting agent. The procedure for preparing the heat-conducting agent was the same as in example 1.
The preparation method of example 3 comprises the following steps:
B1. weighing the raw materials according to the weight parts, sequentially adding vinyl-terminated silicone oil, terminal hydrogen-containing silicone oil, platinum catalyst and ethynyl cyclohexanol into a reaction kettle, and stirring at 30rpm at 100 ℃ for 2 hours to obtain a base material;
B2. adding calcium carbonate, 2, 5-dimethyl-2, 5-di (tert-butyl peroxy) hexane and a heat conducting agent into the base material obtained in the step B1, and stirring at the normal temperature for 30 minutes at the speed of 60rpm to obtain heat conducting glue;
B3. and B2, calendaring and molding the heat-conducting adhesive obtained in the step B2 by using a calendar, making a sheet, then transferring the sheet into a vacuum drying oven, drying at 100 ℃ for 2 hours, and taking out the sheet to obtain the heat-conducting silica gel sheet.
Examples
The heat-conducting silica gel sheet is prepared from the following raw materials in parts by weight: 7 parts of vinyl-terminated silicone oil with the vinyl content of 1.1wt%, 3.5 parts of terminal hydrogen-containing silicone oil with the hydrogen content of 0.6wt%, 2.1 parts of calcium carbonate, 0.7 part of platinum catalyst, 0.5 part of 2, 5-dimethyl-2, 5-di (tert-butyl peroxy) hexane, 0.3 part of ethynyl cyclohexanol and 51 parts of heat conducting agent. The procedure for preparing the heat-conducting agent was the same as in example 1.
The preparation method of example 4 comprises the following steps:
B1. weighing the raw materials according to the weight parts, sequentially adding vinyl-terminated silicone oil, terminal hydrogen-containing silicone oil, platinum catalyst and ethynyl cyclohexanol into a reaction kettle, and stirring at the speed of 30rpm at 105 ℃ for 1.5 hours to obtain a base material;
B2. adding calcium carbonate, 2, 5-dimethyl-2, 5-di (tert-butyl peroxy) hexane and a heat conducting agent into the base material obtained in the step B1, and stirring at the normal temperature for 40 minutes at the speed of 60rpm to obtain heat conducting glue;
B3. and B2, calendaring and molding the heat-conducting adhesive obtained in the step B2 by using a calendar, making a sheet, then transferring the sheet into a vacuum drying oven, drying at 100 ℃ for 2 hours, and taking out the sheet to obtain the heat-conducting silica gel sheet.
Examples
The heat-conducting silica gel sheet is prepared from the following raw materials in parts by weight: 9 parts of vinyl-terminated silicone oil with the vinyl content of 1.4wt%, 3 parts of terminal hydrogen-containing silicone oil with the hydrogen content of 0.2wt%, 2.8 parts of calcium carbonate, 0.6 part of platinum catalyst, 0.7 part of 2, 5-dimethyl-2, 5-di (tert-butyl peroxy) hexane, 0.2 part of ethynyl cyclohexanol and 52 parts of heat conducting agent. The procedure for preparing the heat-conducting agent was the same as in example 1.
The preparation method of example 5 comprises the following steps:
B1. weighing the raw materials according to the weight parts, sequentially adding vinyl-terminated silicone oil, terminal hydrogen-containing silicone oil, platinum catalyst and ethynyl cyclohexanol into a reaction kettle, and stirring at 30rpm at 115 ℃ for 1 hour to obtain a base material;
B2. adding calcium carbonate, 2, 5-dimethyl-2, 5-di (tert-butyl peroxy) hexane and a heat conducting agent into the base material obtained in the step B1, and stirring at the normal temperature for 50 minutes at the speed of 60rpm to obtain heat conducting glue;
B3. and B2, calendaring and molding the heat-conducting adhesive obtained in the step B2 by using a calendar, making a sheet, then transferring the sheet into a vacuum drying oven, drying at 100 ℃ for 2 hours, and taking out the sheet to obtain the heat-conducting silica gel sheet.
Comparative example 1
The difference from example 1 is that: the heat conductive agent is replaced by a mixture of europium oxide powder and beryllium oxide powder, and the proportion of europium oxide to beryllium oxide in the mixture is the same as that of europium oxide to beryllium oxide in the heat conductive agent in the embodiment 1, so that the preparation step of the heat conductive agent is omitted.
Comparative example 2
The difference from example 1 is that: europium nitrate is not used in the preparation step A1 of the heat conducting agent, namely, the composite fiber is replaced by beryllium oxide fiber.
Comparative example 3
The difference from example 1 is that: the preparation step of the heat conducting agent does not comprise the steps A2 and A3, namely the heat conducting agent is replaced by the composite fiber which is not modified.
Comparative example 4
The difference from example 1 is that: the preparation step of the heat-conducting agent does not include the step A2, and the modifier in the step A3 is replaced by terminal hydrogen-containing silicone oil with the hydrogen content of 1 weight percent.
Control example: example 1 of the invention with application number CN 202210632510.5.
Performance test experiment:
the sizes of the heat-conducting silica gel sheets for testing are 20mm multiplied by 5mm, each group of the heat-conducting silica gel sheets are adopted for parallel testing, and the average value of three groups of data obtained by testing is taken as final testing data.
Experimental example one: thermal conductivity testing
Test instrument: DRL heat conduction instrument.
Test reference standard/method: ASTM D5470-2017.
Test object, target: thermal conductivity coefficients of the thermal conductive silicon sheets prepared in examples 1 to 5, comparative example 1, comparative example 3, and comparative example.
Higher thermal conductivity indicates better thermal conductivity, and the test results are shown in table 1:
| coefficient of thermal conductivity (W/m.K) | |
| Example 1 | 1.69 |
| Implementation of the embodimentsExample 2 | 1.63 |
| Example 3 | 1.74 |
| Example 4 | 1.72 |
| Example 5 | 1.65 |
| Comparative example 1 | 1.58 |
| Comparative example 3 | 1.50 |
| Comparative example | 1.33 |
TABLE 1
As can be seen from Table 1, the heat conductivity coefficients of the heat conductive silicon sheets prepared in examples 1 to 5 of the present invention are all higher than those of the comparative examples, which indicates that the present invention has good heat conductivity. The partial raw materials and preparation steps used in comparative examples 1 and 3 are different from those in example 1, and compared with example 1, the thermal conductivity coefficient of comparative example 1 is reduced, which shows that the thermal conductive agent in fiber form has better effect of improving the thermal conductive property of the thermal conductive silica gel sheet compared with the powder form; the decrease of the heat conductivity coefficient of the comparative example 3 is more obvious, which indicates that the modifier used in the invention can further improve the heat conductivity of the heat conductive silica gel sheet.
Experimental example two: shock absorbing property test
Test instrument: dynamic and static stiffness instrument.
Test object, target: dynamic and static stiffness ratios of the heat conductive silicon sheets prepared in examples 1 to 5, comparative example 2 and comparative example.
The closer the dynamic-static stiffness ratio is to 1, the better the shock absorbing performance is, and the test results are shown in table 2:
| ratio of dynamic to static stiffness | |
| Example 1 | 1.16 |
| Example 2 | 1.21 |
| Example 3 | 1.13 |
| Example 4 | 1.14 |
| Example 5 | 1.19 |
| Comparative example 2 | 1.28 |
| Comparative example | 1.35 |
TABLE 2
As can be seen from Table 2, compared with the comparative examples, the dynamic and static stiffness ratios of the heat-conducting silica gel sheets prepared in examples 1 to 5 of the present invention are all closer to 1, which indicates that the present invention has good damping performance. The part of raw materials and preparation steps used in comparative example 2 are different from those in example 1, and the dynamic and static stiffness ratio of comparative example 2 is increased compared with that of example 1, which shows that europium oxide in the heat conductive agent used in the invention can improve the shock absorption performance of the heat conductive silica gel sheet.
Experimental example three: adhesive property test
Test instrument: dynamic and static stiffness instrument.
Test reference standard/method: GB/T13936-2014.
Test object, target: adhesive shear strength of the heat conductive silicone sheets prepared in examples 1 to 5, comparative example 4 and comparative example to aluminum sheets.
The higher the adhesive shear strength, the better the adhesive properties, and the test results are shown in table 3:
| bonding shear Strength (MPa) | |
| Example 1 | 4.12 |
| Example 2 | 4.08 |
| Example 3 | 4.15 |
| Example 4 | 4.13 |
| Example 5 | 4.10 |
| Comparative example 4 | 4.01 |
| Comparative example | 3.57 |
TABLE 3 Table 3
As can be seen from Table 3, the bonding shear strength of the thermally conductive silicone sheets prepared in examples 1 to 5 of the present invention is higher than that of the comparative example, which indicates that the present invention has good bonding performance. The difference between the raw materials and the production steps used in comparative example 4 and those used in example 1 is that the adhesive shear strength of comparative example 4 is lower than that of example 1, and it is shown that the modifier in the heat conductive agent used in the present invention has a better effect of improving the adhesive property of the heat conductive silicone sheet than the non-reacted end-side hydrogen-containing silicone oil.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure.
Claims (9)
1. A thermally conductive silicone sheet, characterized in that: the material is prepared from the following raw materials in parts by weight: 6-10 parts of vinyl end-capped silicone oil, 2-4 parts of end-side hydrogen-containing silicone oil, 2-3 parts of filler, 0.5-1 part of catalyst, 0.4-0.8 part of vulcanizing agent, 0.2-0.3 part of inhibitor and 50-55 parts of heat conducting agent;
the preparation method of the heat-conducting silica gel sheet comprises the following steps:
B1. weighing the raw materials according to parts by weight, sequentially adding vinyl-terminated silicone oil, terminal hydrogen-containing silicone oil, a catalyst and an inhibitor into a reaction kettle, and stirring for 1-2 hours at 100-120 ℃ to obtain a base material;
B2. adding filler, vulcanizing agent and heat conducting agent into the base material obtained in the step B1, and stirring for 30-60 minutes at normal temperature to obtain heat conducting glue;
B3. b2, calendaring and molding the heat-conducting adhesive obtained in the step B2 by using a calendar, making a sheet, then transferring the sheet into a vacuum drying oven, drying at 100 ℃ for 2 hours, and taking out the sheet to obtain a heat-conducting silica gel sheet;
the preparation steps of the heat conducting agent are as follows:
A1. adding europium nitrate into water, mixing uniformly to obtain a first solution, adding beryllium nitrate into water, mixing uniformly to obtain a second solution, adding polyvinylpyrrolidone into absolute ethyl alcohol, mixing uniformly to obtain a third solution, mixing the first solution, the second solution and the third solution, carrying out water bath at 65 ℃ for 45 minutes to obtain sol, transferring the sol into an electrostatic spinning machine, carrying out electrostatic spinning to obtain gel fibers, heating the gel fibers in a muffle furnace to 600 ℃, preserving heat for 3 hours, and taking out to obtain composite fibers for later use;
A2. adding hydrogen-containing silicone oil at the end side, a platinum catalyst and octavinyl octasilsesquioxane into N, N-dimethylformamide under the protection of nitrogen, heating to 100 ℃, stirring and reacting for 10 hours, and evaporating the N, N-dimethylformamide under reduced pressure to obtain a modifier for later use;
A3. and (3) adding the modifier obtained in the step A2 into tetrahydrofuran, uniformly mixing to obtain a modifier solution, immersing the composite fiber obtained in the step A1 into the modifier solution, standing for 12 hours, transferring into a vacuum drying oven, drying at 180 ℃ for 2 hours, and taking out to obtain the heat conducting agent.
2. A thermally conductive silicone sheet as set forth in claim 1 wherein: the vinyl content of the vinyl-terminated silicone oil is 1-1.5wt%, and the hydrogen content of the terminal hydrogen-containing silicone oil is 0.2-0.6wt%.
3. A thermally conductive silicone sheet as set forth in claim 1 wherein: the filler is calcium carbonate.
4. A thermally conductive silicone sheet as set forth in claim 1 wherein: the catalyst is a platinum catalyst.
5. A thermally conductive silicone sheet as set forth in claim 1 wherein: the vulcanizing agent is 2, 5-dimethyl-2, 5-di (tert-butyl peroxy) hexane.
6. A thermally conductive silicone sheet as set forth in claim 1 wherein: the inhibitor is ethynyl cyclohexanol.
7. A thermally conductive silicone sheet as set forth in claim 1 wherein: in the preparation step A1 of the heat conducting agent, the concentration of the solution A is 8wt%, the concentration of the solution B is 2wt%, the mass ratio of polyvinylpyrrolidone to absolute ethyl alcohol in the solution C is 1:15, and the ratio of the solution A to the solution B to the solution C is 10g:9g:6mL; during electrostatic spinning, the inner diameter of the spinneret is 0.9mm, the distance between the spinneret and the receiving plate is 20cm, the sample injection amount is 0.5 mL/hour, and the external electric field is 20kV; the temperature rising speed of the muffle furnace is 2 ℃/min; in the preparation step A2 of the heat conducting agent, the hydrogen content of the end-side hydrogen-containing silicone oil is 1wt%, and the ratio of the end-side hydrogen-containing silicone oil, the platinum catalyst, the octavinyl octasilsesquioxane and the N, N-dimethylformamide is 10g:0.1g:4g:20mL; in the preparation step A3 of the heat conducting agent, the proportion of the modifier obtained in the step A2, tetrahydrofuran and the composite fiber obtained in the step A1 is 9g:80mL:12g.
8. The method for preparing a thermally conductive silicone sheet according to any one of claims 1 to 7, characterized in that: the method comprises the following steps:
B1. weighing the raw materials according to parts by weight, sequentially adding vinyl-terminated silicone oil, terminal hydrogen-containing silicone oil, a catalyst and an inhibitor into a reaction kettle, and stirring for 1-2 hours at 100-120 ℃ to obtain a base material;
B2. adding filler, vulcanizing agent and heat conducting agent into the base material obtained in the step B1, and stirring for 30-60 minutes at normal temperature to obtain heat conducting glue;
B3. and B2, calendaring and molding the heat-conducting adhesive obtained in the step B2 by using a calendar, making a sheet, then transferring the sheet into a vacuum drying oven, drying at 100 ℃ for 2 hours, and taking out the sheet to obtain the heat-conducting silica gel sheet.
9. The method for preparing the heat-conducting silica gel sheet according to claim 8, wherein the method comprises the following steps: the stirring speed in the step B1 is 30rpm, and the stirring speed in the step B2 is 60rpm.
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| RU2009134004A (en) * | 2009-09-10 | 2011-03-20 | Институт автоматики и процессов управления Дальневосточного отделения Российской академии наук (статус государственного учреждения) ( | METHOD FOR OBTAINING SILICON ORGANIC DENDRONS |
| CN104193860A (en) * | 2014-08-15 | 2014-12-10 | 上海理工大学 | Method for synthesizing polyhedron oligomerization silsesquioxane macromolecule composite luminescent material containing rare earth |
| CN111892821A (en) * | 2020-08-19 | 2020-11-06 | 常州威可特新材料有限公司 | Heat-conducting silica gel sheet and preparation method thereof |
| CN112680181A (en) * | 2020-12-28 | 2021-04-20 | 晟大科技(南通)有限公司 | High-electric-conductivity high-heat-conductivity pouring sealant and preparation method thereof |
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| RU2009134004A (en) * | 2009-09-10 | 2011-03-20 | Институт автоматики и процессов управления Дальневосточного отделения Российской академии наук (статус государственного учреждения) ( | METHOD FOR OBTAINING SILICON ORGANIC DENDRONS |
| CN104193860A (en) * | 2014-08-15 | 2014-12-10 | 上海理工大学 | Method for synthesizing polyhedron oligomerization silsesquioxane macromolecule composite luminescent material containing rare earth |
| CN111892821A (en) * | 2020-08-19 | 2020-11-06 | 常州威可特新材料有限公司 | Heat-conducting silica gel sheet and preparation method thereof |
| CN112680181A (en) * | 2020-12-28 | 2021-04-20 | 晟大科技(南通)有限公司 | High-electric-conductivity high-heat-conductivity pouring sealant and preparation method thereof |
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