CN116396620B - Heat conducting fin and preparation method thereof - Google Patents
Heat conducting fin and preparation method thereof Download PDFInfo
- Publication number
- CN116396620B CN116396620B CN202310590911.3A CN202310590911A CN116396620B CN 116396620 B CN116396620 B CN 116396620B CN 202310590911 A CN202310590911 A CN 202310590911A CN 116396620 B CN116396620 B CN 116396620B
- Authority
- CN
- China
- Prior art keywords
- molybdenum carbide
- heat
- parts
- mixing
- molybdenum
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000835 fiber Substances 0.000 claims abstract description 157
- -1 vinyl siloxane Chemical class 0.000 claims abstract description 91
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 85
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 46
- 239000000945 filler Substances 0.000 claims abstract description 31
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 30
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 26
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 23
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 23
- 239000004945 silicone rubber Substances 0.000 claims abstract description 20
- 239000003054 catalyst Substances 0.000 claims abstract description 19
- 239000003112 inhibitor Substances 0.000 claims abstract description 19
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 15
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 15
- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical compound O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229940083037 simethicone Drugs 0.000 claims abstract description 14
- 229910039444 MoC Inorganic materials 0.000 claims description 80
- 238000002156 mixing Methods 0.000 claims description 78
- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical compound [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 claims description 69
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 40
- 229910052750 molybdenum Inorganic materials 0.000 claims description 40
- 239000011733 molybdenum Substances 0.000 claims description 40
- 238000009987 spinning Methods 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 37
- 239000000203 mixture Substances 0.000 claims description 36
- 238000004073 vulcanization Methods 0.000 claims description 35
- 239000007864 aqueous solution Substances 0.000 claims description 32
- 239000002243 precursor Substances 0.000 claims description 28
- 238000001035 drying Methods 0.000 claims description 27
- 238000010438 heat treatment Methods 0.000 claims description 25
- BITPLIXHRASDQB-UHFFFAOYSA-N ethenyl-[ethenyl(dimethyl)silyl]oxy-dimethylsilane Chemical compound C=C[Si](C)(C)O[Si](C)(C)C=C BITPLIXHRASDQB-UHFFFAOYSA-N 0.000 claims description 24
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 17
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 16
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 16
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 16
- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical compound C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 claims description 14
- 239000007822 coupling agent Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 238000005303 weighing Methods 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- 238000005245 sintering Methods 0.000 claims description 11
- 238000000465 moulding Methods 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 8
- 244000028419 Styrax benzoin Species 0.000 claims description 7
- 235000000126 Styrax benzoin Nutrition 0.000 claims description 7
- 235000008411 Sumatra benzointree Nutrition 0.000 claims description 7
- 229960002130 benzoin Drugs 0.000 claims description 7
- 235000019382 gum benzoic Nutrition 0.000 claims description 7
- 229920002545 silicone oil Polymers 0.000 claims description 7
- KWPCLJSZQFXQCM-UHFFFAOYSA-M [Mo]S Chemical compound [Mo]S KWPCLJSZQFXQCM-UHFFFAOYSA-M 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical group C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 5
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- YEECOJZAMZEUBB-UHFFFAOYSA-N 2,2,3,3,6,6,7,7-octamethyloctane Chemical compound CC(C)(C)C(C)(C)CCC(C)(C)C(C)(C)C YEECOJZAMZEUBB-UHFFFAOYSA-N 0.000 claims description 4
- DSVRVHYFPPQFTI-UHFFFAOYSA-N bis(ethenyl)-methyl-trimethylsilyloxysilane;platinum Chemical compound [Pt].C[Si](C)(C)O[Si](C)(C=C)C=C DSVRVHYFPPQFTI-UHFFFAOYSA-N 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 230000003213 activating effect Effects 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 239000003999 initiator Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 239000000741 silica gel Substances 0.000 description 9
- 229910002027 silica gel Inorganic materials 0.000 description 9
- 239000000463 material Substances 0.000 description 6
- 230000000051 modifying effect Effects 0.000 description 4
- 239000002585 base Substances 0.000 description 3
- 239000011231 conductive filler Substances 0.000 description 3
- 238000013461 design Methods 0.000 description 2
- 150000001993 dienes Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N methyl pentane Natural products CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 125000003396 thiol group Chemical group [H]S* 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- FSIJKGMIQTVTNP-UHFFFAOYSA-N bis(ethenyl)-methyl-trimethylsilyloxysilane Chemical compound C[Si](C)(C)O[Si](C)(C=C)C=C FSIJKGMIQTVTNP-UHFFFAOYSA-N 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 125000000101 thioether group Chemical group 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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a heat conducting sheet and a preparation method thereof, wherein the heat conducting sheet comprises the following components in parts by weight: 35-55 parts of vinyl silicone rubber, 20-40 parts of polymethyl vinyl siloxane, 12-20 parts of hydroxyl-terminated polydimethylsiloxane, 5-8 parts of simethicone, 25-35 parts of heat conducting filler, 1.3-2.1 parts of catalyst, 3-6 parts of vulcanizing agent and 0.1-0.5 part of alcohol inhibitor; wherein the heat-conducting filler is polysiloxane thioether modified molybdenum carbide fiber. The invention improves the heat-conducting filler, the heat-conducting filler uses self-prepared polysiloxane thioether modified molybdenum carbide fiber, and the addition of the filler not only enhances the heat-conducting property of the heat-conducting sheet, but also improves the high temperature resistance and various mechanical property performances of the heat-conducting sheet.
Description
Technical Field
The invention relates to the field of heat conducting sheets, in particular to a heat conducting 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 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, simultaneously has the functions 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.
The heat conducting silica gel sheet is mainly used for filling gaps between the heating device and the radiating fin or the metal base, and the flexibility and the elasticity of the heat conducting silica gel sheet enable the heat conducting silica gel sheet to be used for covering uneven surfaces, and heat is conducted from the separating device or the whole PCB to the metal shell or the diffusion plate, so that the efficiency and the service life of the heating electronic component can be improved.
However, the current heat conduction silica gel sheet has low heat conduction performance, insufficient high temperature resistance and mechanical performance, and greatly limits the application of the heat conduction silica gel sheet.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a heat conducting sheet and a preparation method thereof.
The aim of the invention is realized by adopting the following technical scheme:
in a first aspect, the present invention provides a thermally conductive sheet comprising, in parts by weight:
35-55 parts of vinyl silicone rubber, 20-40 parts of polymethyl vinyl siloxane, 12-20 parts of hydroxyl-terminated polydimethylsiloxane, 5-8 parts of simethicone, 25-35 parts of heat conducting filler, 1.3-2.1 parts of catalyst, 3-6 parts of vulcanizing agent and 0.1-0.5 part of alcohol inhibitor.
Preferably, the vinyl content of the vinyl silicone rubber is 0.21% -0.24%, the molecular weight is 45-80 ten thousand, and the volatile component is less than or equal to 2%.
Preferably, the vinyl content of the polymethylvinylsiloxane is 0.52% -0.58% and the viscosity (25 ℃) is 1500-2000 mPa.s.
Preferably, the hydroxyl-terminated polydimethylsiloxane has a hydroxyl content of 8% to 10% and a viscosity (25 ℃) of 2 to 2.5 mPa-s.
Preferably, the viscosity of the simethicone is 3000-5000 mPa.s.
Preferably, the catalyst is a platinum complex, i.e., a platinum complex of divinyl tetramethyl disiloxane.
Preferably, the vulcanizing agent is a bis-dipentaerythritol vulcanizing agent, namely 2, 5-dimethyl-2, 5-di-tert-butylperoxy hexane.
Preferably, the alcohol inhibitor is ethynyl cyclohexanol.
Preferably, the heat-conducting filler is polysiloxane thioether modified molybdenum carbide fiber, and the preparation method comprises the following steps:
(1) Preparing molybdenum carbide fibers:
mixing molybdenum acetylacetonate and ethanol water solution to obtain molybdenum sol spinning solution, spinning by a spinning machine to obtain precursor fiber, and drying and sintering to obtain molybdenum carbide fiber;
(2) Preparing sulfhydrylation molybdenum carbide fiber:
firstly, treating and activating molybdenum carbide fibers in hot alkali liquor to obtain active molybdenum carbide fibers, and then treating the active molybdenum carbide fibers by using a coupling agent KH-581 to prepare thiolated molybdenum carbide fibers;
(3) Preparation of polysiloxane thioether modified molybdenum carbide fibers:
and mixing tetramethyl divinyl disiloxane and the sulfhydrylation molybdenum carbide fiber in an organic solvent, adding a photoinitiator, and reacting under the irradiation of ultraviolet light to obtain the polysiloxane thioether modified molybdenum carbide fiber.
Preferably, the preparation process for preparing the molybdenum carbide fiber comprises the following steps:
s1, weighing and mixing an aqueous solution of molybdenum acetylacetonate and ethanol, adding tackifier polyethylene glycol-400, and fully stirring to form a molybdenum sol spinning solution;
s2, pouring the molybdenum sol spinning solution into a spinning machine, and forming precursor fibers through spinning;
s3, drying the precursor fiber to constant weight at 80-100 ℃, sintering in a high-temperature furnace taking inert gas as shielding gas, heating to 220-250 ℃, preserving heat for 2-5h, heating to 1250-1350 ℃, preserving heat for 1-4h, cooling along with the furnace, and collecting the product to obtain the molybdenum carbide fiber.
More preferably, in the step S1, the mass fraction of the aqueous solution of the ethanol is 45% -75%, and the mass ratio of the aqueous solution of the molybdenum acetylacetonate, the polyethylene glycol-400 and the ethanol is 1.6-3.2:0.2-0.4:5-10.
More preferably, in S2, the parameters of the obtained precursor fiber are: the diameter is 1.5-3.5 μm, and the length is 2-5cm.
Preferably, the preparation process for preparing the sulfhydryl molybdenum carbide fiber comprises the following steps:
s4, placing the molybdenum carbide fiber in an ethanol water solution, dropwise adding a sodium hydroxide solution until the pH value is 10.0-11.0, then heating to 45-65 ℃, preserving heat for 2-4 hours, filtering out the fiber, washing to be neutral by using deionized water, and drying to obtain the active molybdenum carbide fiber;
s5, ultrasonically dispersing the active molybdenum carbide fibers in deionized water, adding a coupling agent KH-581 after uniformly dispersing, stirring for 4-8 hours at room temperature, filtering out the fibers, washing three times by using deionized water, and drying to obtain the sulfhydryl molybdenum carbide fibers.
More preferably, in S4, the mass fraction of the aqueous solution of ethanol is 45% -75%, and the mass ratio of the molybdenum carbide fiber to the aqueous solution of ethanol is 1:10-20.
More preferably, in S5, the mass ratio of the active molybdenum carbide fiber, the coupling agent KH-581 and the deionized water is 1:0.1-0.3:6-12.
Preferably, the preparation process of the polysiloxane thioether modified molybdenum carbide fiber comprises the following steps:
s6, dissolving tetramethyl divinyl disiloxane in N-methylpyrrolidone, adding sulfhydrylation molybdenum carbide fiber, adding a photoinitiator benzoin dimethyl ether after uniform ultrasonic dispersion, stirring and reacting for 20-40min under the irradiation of ultraviolet light, centrifugally filtering out the fiber, washing with acetone for three times, and drying to obtain the polysiloxane thioether modified molybdenum carbide fiber.
More preferably, in the step S6, the mass ratio of the mercapto molybdenum carbide fiber, the tetramethyl divinyl disiloxane and the N-methyl pyrrolidone is 1:1.8-2.4:10-15.
More preferably, in the step S6, the addition mass of the photoinitiator benzoin dimethyl ether is 1.5% -5.5% of the mass of the tetramethyl divinyl disiloxane.
More preferably, in the step S6, the irradiance of the ultraviolet light is 40-50W/m 2 The wavelength is 290-340 nm.
In a second aspect, the present invention provides a method for preparing a thermally conductive sheet, comprising the steps of:
step 1, respectively weighing polymethyl vinyl siloxane, hydroxyl-terminated polydimethylsiloxane, dimethyl silicone oil and vinyl silicone rubber, mixing in an internal mixer, and forming a first mixture after uniform mixing;
step 2, adding the weighed heat conducting filler into the first mixture, and uniformly mixing to form a second mixture;
step 3, adding the weighed catalyst and alcohol inhibitor into the second mixture, and uniformly mixing to form a third mixture;
and step 4, adding a vulcanizing agent into the third mixture, uniformly mixing, and then placing the mixture on a vulcanizing machine for vulcanization molding treatment to obtain the heat-conducting sheet.
Preferably, in the step 1, the mixing speed is 80-120rpm, and the mixing time is 15-30min.
Preferably, in the step 2, the mixing speed is 60-100rpm, and the mixing time is 20-40min.
Preferably, in the step 3, the mixing speed is 60-100rpm, and the mixing time is 10-20min.
Preferably, in the step 4, the mixing speed after adding the vulcanizing agent is 80-120rpm, and the mixing time is 2-5min; the vulcanization molding process comprises twice vulcanization, wherein the first vulcanization temperature is 150-180 ℃, the vulcanization time is 15-20min, the second vulcanization temperature is 220-250 ℃, and the vulcanization time is 1-2h.
The beneficial effects of the invention are as follows:
1. the heat conducting sheet of the invention takes vinyl silicone rubber as a base material, and is compounded with a plurality of polysiloxanes or silicone oil, thereby improving the performance. The polymethyl vinyl siloxane and the hydroxyl-terminated polydimethylsiloxane are respectively used as cross-linking agents, so that the molecular chain structure of the silicon rubber can be enhanced to a certain extent, and meanwhile, the dimethyl silicone oil is added for improving the fluidity and lubricity among internal materials. In addition, the invention improves the heat-conducting filler, and the heat-conducting filler uses self-prepared polysiloxane thioether modified molybdenum carbide fiber, and the addition of the filler not only enhances the heat-conducting property of the heat-conducting sheet, but also improves the high temperature resistance and various mechanical property performances of the heat-conducting sheet.
2. The specific preparation process of the heat-conducting filler comprises the steps of firstly mixing precursor molybdenum acetylacetonate with ethanol solution to form sol spinning solution, then spinning to form precursor fiber yarn, and sintering and carbonizing the fiber to generate molybdenum carbide fiber; and then molybdenum acetylacetonate is used as a matrix, firstly, a sulfhydryl coupling agent is used for modifying the molybdenum acetylacetonate, and then the molybdenum acetylacetonate is combined with tetramethyl divinyl disiloxane of diene, so that the polysiloxane thioether modified molybdenum carbide fiber is finally obtained.
3. In the process of modifying the molybdenum carbide fiber by mercapto, hot alkali liquor is firstly used for treating the surface of the molybdenum carbide fiber, and after the surface of the fiber is activated, a coupling agent KH-581 is used for modifying the surface of the fiber, so that the surface of the fiber has a better modifying effect.
4. In the invention, tetramethyl divinyl disiloxane containing a diene structure is combined with mercapto modified molybdenum carbide fibers under ultraviolet light to generate click chemical reaction of mercapto-double bonds, and meanwhile, a little excessive tetramethyl divinyl disiloxane is added, and the tetramethyl divinyl disiloxane can generate polymerization reaction under the condition, so that the finally obtained product is polymer coated molybdenum carbide fibers containing thioether groups, and based on the structural characteristics, the prepared polysiloxane thioether modified molybdenum carbide fibers not only have good dispersibility in the silicon rubber heat-conducting sheet, but also can generate some performance enhancement effects on the performance of the silicon rubber heat-conducting sheet.
Detailed Description
The technical features, objects and advantages of the present invention will be more clearly understood from the following detailed description of the technical aspects of the present invention, but should not be construed as limiting the scope of the invention.
The invention is further described with reference to the following examples.
Example 1
A heat conductive sheet comprises the following components in parts by weight:
45 parts of vinyl silicone rubber, 30 parts of polymethyl vinyl siloxane, 16 parts of hydroxyl-terminated polydimethylsiloxane, 6 parts of simethicone, 30 parts of heat-conducting filler, 1.7 parts of catalyst, 4 parts of vulcanizing agent and 0.3 part of alcohol inhibitor.
Wherein, the vinyl content of the vinyl silicone rubber is 0.22%, the molecular weight is 65 ten thousand, and the volatile component is less than or equal to 2%; the vinyl content of the polymethylvinylsiloxane was 0.54% and the viscosity (25 ℃) was 1600 mPas; the hydroxyl-terminated polydimethylsiloxane had a hydroxyl content of 8% and a viscosity (25 ℃) of 2 ten thousand mPas; the viscosity of the simethicone was 4000 mPas.
Wherein the catalyst is a platinum complex, namely a divinyl tetramethyl disiloxane platinum complex; the vulcanizing agent is a bis-dipentaerythritol vulcanizing agent, namely 2, 5-dimethyl-2, 5-di-tert-butyl-hexane peroxide; the alcohol inhibitor is ethynyl cyclohexanol.
Wherein, the heat-conducting filler is polysiloxane thioether modified molybdenum carbide fiber, and the preparation method comprises the following steps:
s1, weighing and mixing an aqueous solution of molybdenum acetylacetonate and ethanol, adding tackifier polyethylene glycol-400, and fully stirring to form a molybdenum sol spinning solution; the mass fraction of the aqueous solution of ethanol is 55%, and the mass ratio of the aqueous solution of molybdenum acetylacetonate, polyethylene glycol-400 and ethanol is 2.4:0.3:8.
S2, pouring the molybdenum sol spinning solution into a spinning machine, and forming precursor fibers through spinning, wherein the parameters of the precursor fibers are as follows: 2.5 μm in diameter and 3+ -0.3 cm in length;
s3, drying the precursor fiber to constant weight at 90 ℃, sintering in a high-temperature furnace taking inert gas as shielding gas, heating to 230 ℃, preserving heat for 3 hours, heating to 1300 ℃, preserving heat for 2 hours, cooling along with the furnace, and collecting the product to obtain the molybdenum carbide fiber.
S4, placing the molybdenum carbide fiber into an ethanol water solution with the mass fraction of 55%, dropwise adding a sodium hydroxide solution to the pH value of 10.0-11.0, then heating to 55 ℃, preserving heat for 3 hours, filtering out the fiber, washing to be neutral by using deionized water, and drying to obtain the active molybdenum carbide fiber; the mass ratio of the molybdenum carbide fiber to the ethanol aqueous solution is 1:15.
S5, ultrasonically dispersing the active molybdenum carbide fibers in deionized water, adding a coupling agent KH-581 after uniformly dispersing, stirring for 6 hours at room temperature, filtering out the fibers, washing three times by using the deionized water, and drying to obtain the sulfhydryl molybdenum carbide fibers; the mass ratio of the active molybdenum carbide fiber to the coupling agent KH-581 to the deionized water is 1:0.2:9.
S6, dissolving tetramethyl divinyl disiloxane in N-methylpyrrolidone, adding sulfhydrylation molybdenum carbide fiber, adding a photoinitiator benzoin dimethyl ether after ultrasonic dispersion is uniform, adding 3.5% of the weight of tetramethyl divinyl disiloxane, stirring and reacting for 30min under the irradiation of ultraviolet light, wherein the irradiance of the ultraviolet light is 45W/m 2 Wavelength of 3After the fibers are centrifugally filtered out at 25nm, washing the fibers for three times by using acetone, and drying the fibers to obtain polysiloxane thioether modified molybdenum carbide fibers; the mass ratio of the mercapto molybdenum carbide fiber, the tetramethyl divinyl disiloxane and the N-methyl pyrrolidone is 1:2.1:12.
The preparation method of the heat conducting fin comprises the following steps:
step 1, respectively weighing polymethyl vinyl siloxane, hydroxyl-terminated polydimethylsiloxane, dimethyl silicone oil and vinyl silicone rubber, mixing in an internal mixer, and forming a first mixture after uniform mixing; the speed of mixing was 100rpm and the mixing time was 20min.
Step 2, adding the weighed heat conducting filler into the first mixture, and uniformly mixing to form a second mixture; the speed of mixing was 80rpm and the mixing time was 30min.
Step 3, adding the weighed catalyst and alcohol inhibitor into the second mixture, and uniformly mixing to form a third mixture; the mixing speed was 80rpm and the mixing time was 15min.
And 4, adding a vulcanizing agent into the third mixture for mixing, wherein the mixing speed is 100rpm, the mixing time is 3min, and the mixture is placed on a vulcanizing machine for vulcanization molding treatment, wherein the vulcanization molding process comprises two times of vulcanization, the first vulcanization temperature is 160 ℃, the vulcanization time is 15min, the second vulcanization temperature is 230 ℃, and the vulcanization time is 1.5h, so that the heat-conducting fin is finally obtained.
Example 2
A heat conductive sheet comprises the following components in parts by weight:
35 parts of vinyl silicone rubber, 20 parts of polymethyl vinyl siloxane, 12 parts of hydroxyl-terminated polydimethylsiloxane, 5 parts of simethicone, 25 parts of heat-conducting filler, 1.3 parts of catalyst, 3 parts of vulcanizing agent and 0.1 part of alcohol inhibitor.
Wherein, the vinyl content of the vinyl silicone rubber is 0.21%, the molecular weight is 45 ten thousand, and the volatile component is less than or equal to 2%; the vinyl content of the polymethylvinylsiloxane was 0.52% and the viscosity (25 ℃) was 1500 mPas; the hydroxyl-terminated polydimethylsiloxane had a hydroxyl content of 8% and a viscosity (25 ℃) of 2 ten thousand mPas; the viscosity of the simethicone was 3000 mPas.
Wherein the catalyst is a platinum complex, namely a divinyl tetramethyl disiloxane platinum complex; the vulcanizing agent is a bis-dipentaerythritol vulcanizing agent, namely 2, 5-dimethyl-2, 5-di-tert-butyl-hexane peroxide; the alcohol inhibitor is ethynyl cyclohexanol.
Wherein, the heat-conducting filler is polysiloxane thioether modified molybdenum carbide fiber, and the preparation method comprises the following steps:
s1, weighing and mixing an aqueous solution of molybdenum acetylacetonate and ethanol, adding tackifier polyethylene glycol-400, and fully stirring to form a molybdenum sol spinning solution; the mass fraction of the aqueous solution of ethanol is 45%, and the mass ratio of the aqueous solution of molybdenum acetylacetonate, polyethylene glycol-400 and ethanol is 1.6:0.2:5.
S2, pouring the molybdenum sol spinning solution into a spinning machine, and forming precursor fibers through spinning, wherein the parameters of the precursor fibers are as follows: a diameter of 1.5 μm and a length of 2.+ -. 0.2cm;
s3, drying the precursor fiber to constant weight at 80 ℃, sintering in a high-temperature furnace taking inert gas as shielding gas, heating to 220 ℃, preserving heat for 2 hours, heating to 1250 ℃, preserving heat for 1 hour, cooling along with the furnace, and collecting the product to obtain the molybdenum carbide fiber.
S4, placing the molybdenum carbide fiber into an ethanol water solution with the mass fraction of 45%, dropwise adding a sodium hydroxide solution to the pH value of 10.0-11.0, then heating to 45 ℃, preserving heat for 2 hours, filtering out the fiber, washing to be neutral by using deionized water, and drying to obtain the active molybdenum carbide fiber; the mass ratio of the molybdenum carbide fiber to the ethanol aqueous solution is 1:10.
S5, ultrasonically dispersing the active molybdenum carbide fibers in deionized water, adding a coupling agent KH-581 after uniformly dispersing, stirring for 4 hours at room temperature, filtering out the fibers, washing three times by using the deionized water, and drying to obtain the sulfhydryl molybdenum carbide fibers; the mass ratio of the active molybdenum carbide fiber to the coupling agent KH-581 to the deionized water is 1:0.1:6.
S6, dissolving tetramethyl divinyl disiloxane in N-methylpyrrolidone, adding sulfhydrylation molybdenum carbide fiber, after ultrasonic dispersion is uniform, adding a photoinitiator to restThe dimethyl ether is added with the mass of 1.5 percent of the mass of the tetramethyl divinyl disiloxane, and the mixture is stirred and reacted for 20 minutes under the irradiation of ultraviolet light, wherein the irradiance of the ultraviolet light is 40W/m 2 After centrifugally filtering out the fiber, washing the fiber with acetone for three times, and drying the fiber to obtain the polysiloxane thioether modified molybdenum carbide fiber; the mass ratio of the mercapto molybdenum carbide fiber, the tetramethyl divinyl disiloxane and the N-methyl pyrrolidone is 1:1.8:10.
The preparation method of the heat conducting fin comprises the following steps:
step 1, respectively weighing polymethyl vinyl siloxane, hydroxyl-terminated polydimethylsiloxane, dimethyl silicone oil and vinyl silicone rubber, mixing in an internal mixer, and forming a first mixture after uniform mixing; the speed of mixing was 80rpm and the mixing time was 15min.
Step 2, adding the weighed heat conducting filler into the first mixture, and uniformly mixing to form a second mixture; the speed of mixing was 60rpm and the mixing time was 20min.
Step 3, adding the weighed catalyst and alcohol inhibitor into the second mixture, and uniformly mixing to form a third mixture; the mixing speed was 60rpm and the mixing time was 10min.
And 4, adding a vulcanizing agent into the third mixture for mixing, wherein the mixing speed is 80rpm, the mixing time is 2min, and the mixture is placed on a vulcanizing machine for vulcanization molding treatment, wherein the vulcanization molding process comprises two times of vulcanization, the first vulcanization temperature is 150 ℃, the vulcanization time is 15min, the second vulcanization temperature is 220 ℃, and the vulcanization time is 1h, so that the heat-conducting fin is finally obtained.
Example 3
A heat conductive sheet comprises the following components in parts by weight:
55 parts of vinyl silicone rubber, 40 parts of polymethyl vinyl siloxane, 20 parts of hydroxyl-terminated polydimethylsiloxane, 8 parts of simethicone, 35 parts of heat conducting filler, 2.1 parts of catalyst, 6 parts of vulcanizing agent and 0.5 part of alcohol inhibitor.
Wherein, the vinyl content of the vinyl silicone rubber is 0.24%, the molecular weight is 80 ten thousand, and the volatile component is less than or equal to 2%; the vinyl content of the polymethylvinylsiloxane was 0.58% and the viscosity (25 ℃) was 2000 mPas; the hydroxyl-terminated polydimethylsiloxane had a hydroxyl content of 10% and a viscosity (25 ℃) of 2.5 mPa.s; the viscosity of the simethicone was 5000 mPas.
Wherein the catalyst is a platinum complex, namely a divinyl tetramethyl disiloxane platinum complex; the vulcanizing agent is a bis-dipentaerythritol vulcanizing agent, namely 2, 5-dimethyl-2, 5-di-tert-butyl-hexane peroxide; the alcohol inhibitor is ethynyl cyclohexanol.
Wherein, the heat-conducting filler is polysiloxane thioether modified molybdenum carbide fiber, and the preparation method comprises the following steps:
s1, weighing and mixing an aqueous solution of molybdenum acetylacetonate and ethanol, adding tackifier polyethylene glycol-400, and fully stirring to form a molybdenum sol spinning solution; the mass fraction of the aqueous solution of ethanol is 75%, and the mass ratio of the aqueous solution of molybdenum acetylacetonate, polyethylene glycol-400 and ethanol is 3.2:0.4:10.
S2, pouring the molybdenum sol spinning solution into a spinning machine, and forming precursor fibers through spinning, wherein the parameters of the precursor fibers are as follows: 3.5 μm in diameter and 5+ -0.5 cm in length;
s3, drying the precursor fiber to constant weight at 100 ℃, sintering in a high-temperature furnace taking inert gas as shielding gas, heating to 250 ℃, preserving heat for 5 hours, heating to 1350 ℃, preserving heat for 4 hours, cooling along with the furnace, and collecting the product to obtain the molybdenum carbide fiber.
S4, placing the molybdenum carbide fiber into an ethanol water solution with the mass fraction of 75%, dropwise adding a sodium hydroxide solution to the pH value of 10.0-11.0, then heating to 65 ℃, preserving heat for 4 hours, filtering out the fiber, washing to be neutral by using deionized water, and drying to obtain the active molybdenum carbide fiber; the mass ratio of the molybdenum carbide fiber to the ethanol aqueous solution is 1:20.
S5, ultrasonically dispersing the active molybdenum carbide fibers in deionized water, adding a coupling agent KH-581 after uniformly dispersing, stirring for 8 hours at room temperature, filtering out the fibers, washing three times by using the deionized water, and drying to obtain the sulfhydryl molybdenum carbide fibers; the mass ratio of the active molybdenum carbide fiber to the coupling agent KH-581 to the deionized water is 1:0.3:12.
S6, dissolving tetramethyl divinyl disiloxane in N-methylpyrrolidone, adding sulfhydrylation molybdenum carbide fiber, adding a photoinitiator benzoin dimethyl ether after ultrasonic dispersion is uniform, adding 5.5% of the weight of tetramethyl divinyl disiloxane, stirring and reacting for 40min under the irradiation of ultraviolet light, wherein the irradiance of the ultraviolet light is 50W/m 2 After centrifugally filtering out the fiber, washing the fiber with acetone for three times, and drying the fiber to obtain the polysiloxane thioether modified molybdenum carbide fiber; the mass ratio of the mercapto molybdenum carbide fiber, the tetramethyl divinyl disiloxane and the N-methyl pyrrolidone is 1:2.4:15.
The preparation method of the heat conducting fin comprises the following steps:
step 1, respectively weighing polymethyl vinyl siloxane, hydroxyl-terminated polydimethylsiloxane, dimethyl silicone oil and vinyl silicone rubber, mixing in an internal mixer, and forming a first mixture after uniform mixing; the speed of mixing was 120rpm and the mixing time was 30min.
Step 2, adding the weighed heat conducting filler into the first mixture, and uniformly mixing to form a second mixture; the speed of mixing was 100rpm and the mixing time was 40min.
Step 3, adding the weighed catalyst and alcohol inhibitor into the second mixture, and uniformly mixing to form a third mixture; the mixing speed was 100rpm and the mixing time was 20min.
And 4, adding a vulcanizing agent into the third mixture for mixing, wherein the mixing speed is 120rpm, the mixing time is 5min, and the mixture is placed on a vulcanizing machine for vulcanization molding treatment, wherein the vulcanization molding process comprises two times of vulcanization, the first vulcanization temperature is 180 ℃, the vulcanization time is 20min, the second vulcanization temperature is 250 ℃, and the vulcanization time is 2h, so that the heat-conducting fin is finally obtained.
Comparative example 1
This comparative example is based on example 1, and differs from example 1 only in the thermally conductive filler.
A heat conductive sheet comprises the following components in parts by weight:
45 parts of vinyl silicone rubber, 30 parts of polymethyl vinyl siloxane, 16 parts of hydroxyl-terminated polydimethylsiloxane, 6 parts of simethicone, 30 parts of heat-conducting filler, 1.7 parts of catalyst, 4 parts of vulcanizing agent and 0.3 part of alcohol inhibitor.
The heat conducting filler is molybdenum carbide fiber, and the preparation method comprises the following steps:
s1, weighing and mixing an aqueous solution of molybdenum acetylacetonate and ethanol, adding tackifier polyethylene glycol-400, and fully stirring to form a molybdenum sol spinning solution; the mass fraction of the aqueous solution of ethanol is 55%, and the mass ratio of the aqueous solution of molybdenum acetylacetonate, polyethylene glycol-400 and ethanol is 2.4:0.3:8.
S2, pouring the molybdenum sol spinning solution into a spinning machine, and forming precursor fibers through spinning, wherein the parameters of the precursor fibers are as follows: 2.5 μm in diameter and 3+ -0.3 cm in length;
s3, drying the precursor fiber to constant weight at 90 ℃, sintering in a high-temperature furnace taking inert gas as shielding gas, heating to 230 ℃, preserving heat for 3 hours, heating to 1300 ℃, preserving heat for 2 hours, cooling along with the furnace, and collecting the product to obtain the molybdenum carbide fiber.
Comparative example 2
This comparative example is based on example 1, and differs from example 1 only in the thermally conductive filler.
A heat conductive sheet comprises the following components in parts by weight:
45 parts of vinyl silicone rubber, 30 parts of polymethyl vinyl siloxane, 16 parts of hydroxyl-terminated polydimethylsiloxane, 6 parts of simethicone, 30 parts of heat-conducting filler, 1.7 parts of catalyst, 4 parts of vulcanizing agent and 0.3 part of alcohol inhibitor.
The heat conducting filler is active molybdenum carbide fiber, and the preparation method comprises the following steps:
s1, weighing and mixing an aqueous solution of molybdenum acetylacetonate and ethanol, adding tackifier polyethylene glycol-400, and fully stirring to form a molybdenum sol spinning solution; the mass fraction of the aqueous solution of ethanol is 55%, and the mass ratio of the aqueous solution of molybdenum acetylacetonate, polyethylene glycol-400 and ethanol is 2.4:0.3:8.
S2, pouring the molybdenum sol spinning solution into a spinning machine, and forming precursor fibers through spinning, wherein the parameters of the precursor fibers are as follows: 2.5 μm in diameter and 3+ -0.3 cm in length;
s3, drying the precursor fiber to constant weight at 90 ℃, sintering in a high-temperature furnace taking inert gas as shielding gas, heating to 230 ℃, preserving heat for 3 hours, heating to 1300 ℃, preserving heat for 2 hours, cooling along with the furnace, and collecting the product to obtain the molybdenum carbide fiber.
S4, placing the molybdenum carbide fiber into an ethanol water solution with the mass fraction of 55%, dropwise adding a sodium hydroxide solution to the pH value of 10.0-11.0, then heating to 55 ℃, preserving heat for 3 hours, filtering out the fiber, washing to be neutral by using deionized water, and drying to obtain the active molybdenum carbide fiber; the mass ratio of the molybdenum carbide fiber to the ethanol aqueous solution is 1:15.
Comparative example 3
This comparative example is based on example 1, and differs from example 1 only in the thermally conductive filler.
A heat conductive sheet comprises the following components in parts by weight:
45 parts of vinyl silicone rubber, 30 parts of polymethyl vinyl siloxane, 16 parts of hydroxyl-terminated polydimethylsiloxane, 6 parts of simethicone, 30 parts of heat-conducting filler, 1.7 parts of catalyst, 4 parts of vulcanizing agent and 0.3 part of alcohol inhibitor.
The heat conducting filler is molybdenum carbide fiber, and the preparation method comprises the following steps:
s1, weighing and mixing an aqueous solution of molybdenum acetylacetonate and ethanol, adding tackifier polyethylene glycol-400, and fully stirring to form a molybdenum sol spinning solution; the mass fraction of the aqueous solution of ethanol is 55%, and the mass ratio of the aqueous solution of molybdenum acetylacetonate, polyethylene glycol-400 and ethanol is 2.4:0.3:8.
S2, pouring the molybdenum sol spinning solution into a spinning machine, and forming precursor fibers through spinning, wherein the parameters of the precursor fibers are as follows: 2.5 μm in diameter and 3+ -0.3 cm in length;
s3, drying the precursor fiber to constant weight at 90 ℃, sintering in a high-temperature furnace taking inert gas as shielding gas, heating to 230 ℃, preserving heat for 3 hours, heating to 1300 ℃, preserving heat for 2 hours, cooling along with the furnace, and collecting the product to obtain the molybdenum carbide fiber.
S4, dissolving tetramethyl divinyl disiloxane in N-methylpyrrolidone, adding molybdenum carbide fibers, uniformly dispersing by ultrasonic waves, adding a photoinitiator benzoin dimethyl ether, wherein the mass of the added material is 3.5% of that of the tetramethyl divinyl disiloxane, stirring and reacting for 30min under the irradiation of ultraviolet light, wherein the irradiance of the ultraviolet light is 45W/m 2 Centrifugally filtering out fibers with the wavelength of 325nm, washing with acetone for three times, and drying to obtain polysiloxane modified molybdenum carbide fibers; the mass ratio of the molybdenum carbide fiber, the tetramethyl divinyl disiloxane and the N-methylpyrrolidone is 1:2.1:12.
Experimental example
The heat conductive sheets prepared in example 1 and comparative examples 1 to 3 were prepared into products having a thickness of 0.3.+ -. 0.01cm, and the corresponding mechanical strength, heat resistance and heat conductivity were examined, and the examination results are shown in Table 1:
table 1 results of performance tests of thermally conductive sheets prepared by different methods
| Example 1 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Shore A hardness | 48 | 41 | 45 | 46 |
| Tensile Strength (MPa) | 9.3 | 6.8 | 7.4 | 8.7 |
| Tear strength (KN/m) | 45.2 | 33.9 | 38.2 | 40.3 |
| High temperature resistance (DEG C) | 287 | 256 | 269 | 274 |
| Thermal conductivity (W/(m.K)) | 5.73 | 4.21 | 4.57 | 5.30 |
The corresponding standards in Table 1 include, among others, shore A hardness (GB/T531.1-2008), tensile strength (GB 1040.1-2006), tear strength (GB/T529-2008, right angle test specimen), thermal conductivity (ASTM D5470).
As can be seen from table 1, the heat conducting sheet prepared in example 1 of the present invention has high heat conductivity and high temperature resistance, the heat conductivity reaches 5.73W/(m·k), and the high temperature resistance is higher than 287 ℃; and the hardness, tensile strength and tearing strength are all higher than those of the common heat conducting sheet, for example, the tensile strength can reach 9.3MPa, which is far higher than 6.8MPa of comparative example 1, and the tearing strength can reach 45.2KN/m, which is far higher than 33.9KN/m of comparative example 1.
Therefore, in summary, the heat conductive sheet prepared in embodiment 1 of the present invention has high heat conductive performance, high temperature resistance, and excellent continuing performance (such as tensile strength and tear strength), and can better expand the application range of the heat conductive sheet.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention.
Claims (8)
1. A thermally conductive sheet characterized by comprising the following components in parts by weight:
35-55 parts of vinyl silicone rubber, 20-40 parts of polymethyl vinyl siloxane, 12-20 parts of hydroxyl-terminated polydimethylsiloxane, 5-8 parts of simethicone, 25-35 parts of heat conducting filler, 1.3-2.1 parts of catalyst, 3-6 parts of vulcanizing agent and 0.1-0.5 part of alcohol inhibitor;
wherein the heat-conducting filler is polysiloxane thioether modified molybdenum carbide fiber;
the preparation method of the heat conduction filler comprises the following steps:
(1) Preparing molybdenum carbide fibers:
mixing molybdenum acetylacetonate and ethanol water solution to obtain molybdenum sol spinning solution, spinning by a spinning machine to obtain precursor fiber, and drying and sintering to obtain molybdenum carbide fiber;
(2) Preparing sulfhydrylation molybdenum carbide fiber:
firstly, treating and activating molybdenum carbide fibers in hot alkali liquor to obtain active molybdenum carbide fibers, and then treating the active molybdenum carbide fibers by using a coupling agent KH-581 to prepare thiolated molybdenum carbide fibers;
(3) Preparation of polysiloxane thioether modified molybdenum carbide fibers:
mixing tetramethyl divinyl disiloxane and sulfhydrylation molybdenum carbide fiber in an organic solvent, adding a photoinitiator, and reacting under the irradiation of ultraviolet light to obtain polysiloxane thioether modified molybdenum carbide fiber;
the catalyst is a platinum complex, namely a divinyl tetramethyl disiloxane platinum complex; the vulcanizing agent is a bis-dipentaerythritol vulcanizing agent, namely 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide; the alcohol inhibitor is ethynyl cyclohexanol.
2. The heat conducting fin according to claim 1, wherein the vinyl silicone rubber has a vinyl content of 0.21% -0.24%, a molecular weight of 45-80 ten thousand, and a volatile component of 2% or less; the vinyl content of the polymethyl vinyl siloxane is 0.52-0.58%, and the viscosity (25 ℃) is 1500-2000 mPa.s; the hydroxyl content of the hydroxyl-terminated polydimethylsiloxane is 8% -10%, and the viscosity (25 ℃) is 2-2.5 mPa.s; the viscosity of the simethicone is 3000-5000 mPa.s.
3. A thermally conductive sheet according to claim 1, wherein the process for producing the molybdenum carbide fiber comprises:
s1, weighing and mixing an aqueous solution of molybdenum acetylacetonate and ethanol, adding tackifier polyethylene glycol-400, and fully stirring to form a molybdenum sol spinning solution; wherein, the mass fraction of the aqueous solution of the ethanol is 45-75 percent, and the mass ratio of the aqueous solution of the molybdenum acetylacetonate, the polyethylene glycol-400 and the ethanol is 1.6-3.2:0.2-0.4:5-10;
s2, pouring the molybdenum sol spinning solution into a spinning machine, and forming precursor fibers through spinning; wherein, the parameters of the obtained precursor fiber are as follows: the diameter is 1.5-3.5 μm, and the length is 2-5cm;
s3, drying the precursor fiber to constant weight at 80-100 ℃, sintering in a high-temperature furnace taking inert gas as shielding gas, heating to 220-250 ℃, preserving heat for 2-5h, heating to 1250-1350 ℃, preserving heat for 1-4h, cooling along with the furnace, and collecting the product to obtain the molybdenum carbide fiber.
4. A thermally conductive sheet according to claim 1, wherein the preparation process of the mercapto molybdenum carbide fiber comprises:
s4, placing the molybdenum carbide fiber in an ethanol water solution, dropwise adding a sodium hydroxide solution until the pH value is 10.0-11.0, then heating to 45-65 ℃, preserving heat for 2-4 hours, filtering out the fiber, washing to be neutral by using deionized water, and drying to obtain the active molybdenum carbide fiber; wherein, the mass fraction of the ethanol aqueous solution is 45% -75%, and the mass ratio of the molybdenum carbide fiber to the ethanol aqueous solution is 1:10-20;
s5, ultrasonically dispersing the active molybdenum carbide fibers in deionized water, adding a coupling agent KH-581 after uniformly dispersing, stirring for 4-8 hours at room temperature, filtering out the fibers, washing three times by using deionized water, and drying to obtain the sulfhydryl molybdenum carbide fibers; wherein the mass ratio of the active molybdenum carbide fiber to the coupling agent KH-581 to the deionized water is 1:0.1-0.3:6-12.
5. A thermally conductive sheet according to claim 1, wherein the process for producing the polysiloxane thioether modified molybdenum carbide fiber comprises:
s6, dissolving tetramethyl divinyl disiloxane in N-methylpyrrolidone, adding sulfhydrylation molybdenum carbide fiber, adding a photoinitiator benzoin dimethyl ether after uniform ultrasonic dispersion, stirring and reacting for 20-40min under the irradiation of ultraviolet light, centrifugally filtering out fiber, washing with acetone for three times, and drying to obtain polysiloxane thioether modified molybdenum carbide fiber;
wherein the mass ratio of the mercapto molybdenum carbide fiber to the tetramethyl divinyl disiloxane to the N-methyl pyrrolidone is 1:1.8-2.4:10-15; the addition mass of the initiator benzoin dimethyl ether is 1.5% -5.5% of the mass of the tetramethyl divinyl disiloxane; irradiance of ultraviolet light is 40-50W/m 2 The wavelength is 290-340 nm.
6. A method for producing the heat conductive sheet according to claim 1, comprising the steps of:
step 1, respectively weighing polymethyl vinyl siloxane, hydroxyl-terminated polydimethylsiloxane, dimethyl silicone oil and vinyl silicone rubber, mixing in an internal mixer, and forming a first mixture after uniform mixing;
step 2, adding the weighed heat conducting filler into the first mixture, and uniformly mixing to form a second mixture;
step 3, adding the weighed catalyst and alcohol inhibitor into the second mixture, and uniformly mixing to form a third mixture;
and step 4, adding a vulcanizing agent into the third mixture, uniformly mixing, and then placing the mixture on a vulcanizing machine for vulcanization molding treatment to obtain the heat-conducting sheet.
7. The method of producing a heat conductive sheet according to claim 6, wherein in the step 1, the mixing speed is 80 to 120rpm and the mixing time is 15 to 30 minutes; in the step 2, the mixing speed is 60-100rpm, and the mixing time is 20-40min; in the step 3, the mixing speed is 60-100rpm, and the mixing time is 10-20min.
8. The method of producing a heat conductive sheet according to claim 6, wherein in the step 4, the mixing speed after adding the vulcanizing agent is 80 to 120rpm, and the mixing time is 2 to 5 minutes; the vulcanization molding process comprises twice vulcanization, wherein the first vulcanization temperature is 150-180 ℃, the vulcanization time is 15-20min, the second vulcanization temperature is 220-250 ℃, and the vulcanization time is 1-2h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310590911.3A CN116396620B (en) | 2023-05-24 | 2023-05-24 | Heat conducting fin and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310590911.3A CN116396620B (en) | 2023-05-24 | 2023-05-24 | Heat conducting fin and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116396620A CN116396620A (en) | 2023-07-07 |
| CN116396620B true CN116396620B (en) | 2023-12-19 |
Family
ID=87020083
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310590911.3A Active CN116396620B (en) | 2023-05-24 | 2023-05-24 | Heat conducting fin and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116396620B (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4039503A (en) * | 1975-02-19 | 1977-08-02 | Shin-Etsu Chemical Co., Ltd. | Silicone rubber compositions |
| CN104357937A (en) * | 2014-11-10 | 2015-02-18 | 上海交通大学 | Method for preparing porous molybdenum carbide nanofiber by adopting electrostatic spinning |
| CN105646945A (en) * | 2016-03-30 | 2016-06-08 | 南昌航空大学 | Method for preparing nanometer silicon dioxide grafted carbon fiber reinforcements by aid of mercapto-alkene click reaction |
| CN106633078A (en) * | 2016-12-28 | 2017-05-10 | 江苏美思德化学股份有限公司 | Mercapto nano-silica and polyether dual modified organosilicon surfactant and preparation method |
| CN110591374A (en) * | 2019-09-05 | 2019-12-20 | 上海阿莱德实业股份有限公司 | Silicone rubber heat conduction material and preparation method thereof |
| CN111057379A (en) * | 2019-12-26 | 2020-04-24 | 华南理工大学 | High-thermal-conductivity insulating silicone rubber composite material containing carbon fibers and preparation method thereof |
| CN113652010A (en) * | 2020-05-12 | 2021-11-16 | 北京化工大学 | Rubber composite material filled with end group functionalized liquid rubber and mercapto silane coupling agent synergistically modified white carbon black and preparation method thereof |
| WO2023057347A1 (en) * | 2021-10-06 | 2023-04-13 | Wacker Chemie Ag | Thermally conductive silicone composition and method for producing the same |
-
2023
- 2023-05-24 CN CN202310590911.3A patent/CN116396620B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4039503A (en) * | 1975-02-19 | 1977-08-02 | Shin-Etsu Chemical Co., Ltd. | Silicone rubber compositions |
| CN104357937A (en) * | 2014-11-10 | 2015-02-18 | 上海交通大学 | Method for preparing porous molybdenum carbide nanofiber by adopting electrostatic spinning |
| CN105646945A (en) * | 2016-03-30 | 2016-06-08 | 南昌航空大学 | Method for preparing nanometer silicon dioxide grafted carbon fiber reinforcements by aid of mercapto-alkene click reaction |
| CN106633078A (en) * | 2016-12-28 | 2017-05-10 | 江苏美思德化学股份有限公司 | Mercapto nano-silica and polyether dual modified organosilicon surfactant and preparation method |
| CN110591374A (en) * | 2019-09-05 | 2019-12-20 | 上海阿莱德实业股份有限公司 | Silicone rubber heat conduction material and preparation method thereof |
| CN111057379A (en) * | 2019-12-26 | 2020-04-24 | 华南理工大学 | High-thermal-conductivity insulating silicone rubber composite material containing carbon fibers and preparation method thereof |
| CN113652010A (en) * | 2020-05-12 | 2021-11-16 | 北京化工大学 | Rubber composite material filled with end group functionalized liquid rubber and mercapto silane coupling agent synergistically modified white carbon black and preparation method thereof |
| WO2023057347A1 (en) * | 2021-10-06 | 2023-04-13 | Wacker Chemie Ag | Thermally conductive silicone composition and method for producing the same |
Non-Patent Citations (1)
| Title |
|---|
| 同济大学普通化学及无机化学教研室.《普通化学》.高等教育出版社,2004,(第1版),第217页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116396620A (en) | 2023-07-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106467668B (en) | Organic silicon resin aluminum-based copper-clad plate and preparation method thereof | |
| CN108395702A (en) | A kind of production method of heat-conducting silica gel sheet | |
| CN113563721A (en) | High-tear-strength heat-conducting silica gel material and preparation method thereof | |
| CN115124842B (en) | Wide-temperature-range storage-resistant silicone rubber and preparation method thereof | |
| CN115011125B (en) | High-heat-conductivity antioxidant wave-absorbing silicon rubber composite material and preparation method thereof | |
| CN116396620B (en) | Heat conducting fin and preparation method thereof | |
| CN108299830B (en) | Silicone rubber-based flexible graphene heating film, preparation method thereof, heating device and application | |
| CN110982281B (en) | Blended fluorosilicone rubber composition and preparation method thereof | |
| CN105838077A (en) | Surface treatment method of graphene used for producing heat conducting silicon sheets | |
| CN116330777A (en) | Heating film with high-strength insulating material | |
| CN113480856B (en) | Thermal conductive gel containing pendant chain and preparation method and application thereof | |
| CN113717534A (en) | Heat conduction material and preparation process | |
| CN116589973B (en) | High-temperature-resistant COB packaging adhesive and preparation method thereof | |
| Yu et al. | Self-healing electromagnetic interference shielding composite based on Diels–Alder chemistry | |
| CN112724685A (en) | Organic silicon heat-conducting sheet and preparation method thereof | |
| CN111875852B (en) | Composite heat conduction material, silicone rubber and preparation method and application thereof | |
| CN113604190B (en) | Ultraviolet light curing type heat conduction pouring sealant and preparation method and application thereof | |
| CN112280304A (en) | Efficient heat-conducting silica gel sheet and processing technology | |
| CN111533953A (en) | Preparation method of high-thermal-conductivity powder for heat-conducting rubber | |
| CN115260703B (en) | Plastic packaging material with high temperature resistance and small thermal expansion coefficient and preparation method thereof | |
| CN109627779A (en) | A kind of integrated circuit silicone rubber compound and preparation process | |
| CN114921101B (en) | Preparation method of heat conduction gasket | |
| TWI813019B (en) | Resin material and metal substrate | |
| CN115449223B (en) | Preparation method of high-heat-conductivity interface material | |
| TWI803025B (en) | Resin material and metal substrate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |