CN105968822A - Heat conductive silicone rubber, preparation method of heat conductive silicone rubber, and laser projection equipment - Google Patents
Heat conductive silicone rubber, preparation method of heat conductive silicone rubber, and laser projection equipment Download PDFInfo
- Publication number
- CN105968822A CN105968822A CN201610474471.5A CN201610474471A CN105968822A CN 105968822 A CN105968822 A CN 105968822A CN 201610474471 A CN201610474471 A CN 201610474471A CN 105968822 A CN105968822 A CN 105968822A
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- Prior art keywords
- heat
- silicone rubber
- silicon rubber
- preparation
- conducting silicon
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- 239000004945 silicone rubber Substances 0.000 title claims abstract description 85
- 238000002360 preparation method Methods 0.000 title claims abstract description 49
- 238000002156 mixing Methods 0.000 claims abstract description 37
- 229910052751 metal Inorganic materials 0.000 claims abstract description 36
- 239000002184 metal Substances 0.000 claims abstract description 36
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 15
- 238000004132 cross linking Methods 0.000 claims abstract description 11
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910000077 silane Inorganic materials 0.000 claims abstract description 9
- 238000011049 filling Methods 0.000 claims description 48
- 239000011159 matrix material Substances 0.000 claims description 43
- -1 mercaptan compound Chemical class 0.000 claims description 28
- 239000000428 dust Substances 0.000 claims description 26
- 239000000376 reactant Substances 0.000 claims description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 239000003960 organic solvent Substances 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 15
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- 238000005286 illumination Methods 0.000 claims description 12
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- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 1
- 229940118308 colloid sulfur Drugs 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000039 congener Substances 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 125000002704 decyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000012933 diacyl peroxide Substances 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 1
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 229940074391 gallic acid Drugs 0.000 description 1
- 235000004515 gallic acid Nutrition 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 235000003642 hunger Nutrition 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000003949 imides Chemical class 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 1
- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 229960004194 lidocaine Drugs 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- YLHXLHGIAMFFBU-UHFFFAOYSA-N methyl phenylglyoxalate Chemical compound COC(=O)C(=O)C1=CC=CC=C1 YLHXLHGIAMFFBU-UHFFFAOYSA-N 0.000 description 1
- DEQZTKGFXNUBJL-UHFFFAOYSA-N n-(1,3-benzothiazol-2-ylsulfanyl)cyclohexanamine Chemical compound C1CCCCC1NSC1=NC2=CC=CC=C2S1 DEQZTKGFXNUBJL-UHFFFAOYSA-N 0.000 description 1
- DUWWHGPELOTTOE-UHFFFAOYSA-N n-(5-chloro-2,4-dimethoxyphenyl)-3-oxobutanamide Chemical compound COC1=CC(OC)=C(NC(=O)CC(C)=O)C=C1Cl DUWWHGPELOTTOE-UHFFFAOYSA-N 0.000 description 1
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 125000001400 nonyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 150000001451 organic peroxides Chemical class 0.000 description 1
- 150000002923 oximes Chemical class 0.000 description 1
- AUONHKJOIZSQGR-UHFFFAOYSA-N oxophosphane Chemical compound P=O AUONHKJOIZSQGR-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- RGSFGYAAUTVSQA-UHFFFAOYSA-N pentamethylene Natural products C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 1
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920002589 poly(vinylethylene) polymer Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000000191 radiation effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- FWMUJAIKEJWSSY-UHFFFAOYSA-N sulfur dichloride Chemical compound ClSCl FWMUJAIKEJWSSY-UHFFFAOYSA-N 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 150000003568 thioethers Chemical group 0.000 description 1
- 150000003573 thiols Chemical class 0.000 description 1
- 150000003672 ureas Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- 239000011787 zinc oxide Substances 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/14—Peroxides
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03B—APPARATUS OR ARRANGEMENTS FOR TAKING PHOTOGRAPHS OR FOR PROJECTING OR VIEWING THEM; APPARATUS OR ARRANGEMENTS EMPLOYING ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ACCESSORIES THEREFOR
- G03B21/00—Projectors or projection-type viewers; Accessories therefor
- G03B21/14—Details
- G03B21/16—Cooling; Preventing overheating
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- 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
-
- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a heat conductive silicone rubber, a preparation method of the heat conductive silicone rubber, and laser projection equipment comprising the heat conductive silicone rubber. The preparation method of the heat conductive silicone rubber comprises the following steps: 1, dispersing a heat conductive filler into a silicone rubber substrate, 2, dispersing a vulcanizing agent into the silicone rubber substrate, and 3, conducting cross linking reaction on the vulcanizing agent and the silicone rubber substrate to obtain the heat conductive silicone rubber, wherein the a heat conductive filler is formed by compounding silane polymers and metal powder through a solution mixing method. According to the preparation method of the heat conductive silicone rubber, the used heat conductive filler is obtained by compounding the metal powder and the silane polymers in advance, and the silane polymers compounded with the metal powder have excellent solubility with the silicone rubber substrate, so that the uniform dispersity of the heat conductive filler in the silicone rubber substrate can be improved.
Description
Technical field
The present invention relates to heat-conducting silicon rubber and preparation method thereof, the laser projection device comprising this heat-conducting silicon rubber.
Background technology
The main chain of silicone rubber is made up of silicon, oxygen atom, and side chain is carbon-containing group.Combination ratio due to siliconoxygen bond
It is relatively tight, so heat-resisting, the cold tolerance of silicone rubber well, and have the against weather of excellence, resistance to ozone
Property and good insulating properties, therefore silicone rubber can be widely applied to the fields such as medical treatment, life, industry
In.Specifically, the most commonly used silicone rubber in Electronic Assemblies field.But in recent years, Electronic Assemblies is just
Develop to densification direction, cause the power density of electronic component constantly to raise, in using, be easily caused temperature
Too high, therefore for the occasion of application silicone rubber, high-termal conductivity becomes affects electronic devices and components reliability
Key factor with service life.And, in order to reduce the thermal contact resistance between interface, it is desirable to boundary material
Existing higher heat conductivity, also requires that it possesses good processing characteristics and mechanical property, in order to can be more preferably
Filling interface between minim gap.The heat conductivility of silicone rubber itself is very poor, and thermal conductivity generally only has
0.13-0.25W/M about K, it is impossible to the improving constantly of power density enough meeting Electronic Assemblies is brought
The heat conductivity demand improved constantly.Therefore the scheme having been proposed that is, by being added to high thermal conductivity
Filler, improve the heat conductivility of silicon rubber composite material, therefore can bring along with the raising of heat conductivility
The optimization of heat dispersion.
At present, the method that the filler of high heat conduction adds to silicone rubber matrix is mainly included solution blending, powder
The methods such as end mixing, melting mixing.As above the heat-conducting silicon rubber that method obtains is cheap, be easily processed into
Type, thus it is widely used in the silastic product field contacted with electronic devices and components.As an example, west
Peace University of Science and Technology Wang Ni discloses in its paper " preparation of heat-conducting silicon rubber and performance characterization ", selects stone
Ink, carborundum, boron nitride, aluminium nitride prepare heat-conducting silicon rubber as heat filling, and wherein boron nitride is used
When amount is 30 parts, the silicone rubber best results of preparation, heat conductivity be 0.647W/M K (testing standard:
GB/T11205-2009), hot strength is 2.761MPa (testing standard: GB/T528-92).
It will be appreciated, however, that in order to form efficient thermal conductive network chain structure, need to add a large amount of heat conduction and fill out
Material, this can cause the mechanical properties decrease of silicone rubber, be unfavorable for machine-shaping.And, leading in a large number of interpolation
Hot filler not can be uniformly dispersed in silicone rubber matrix, causes the interruption of heat conduction network chain, have impact on heat radiation effect
Really.Such as in patent documentation CN102827480A, disclose one and prepare high-heat-conductingsilicon silicon rubber compound material
Method, its core be by heat filling and deionized water, ethanol, toluene, dimethylbenzene, oxolane or/
It is configured to the dispersion liquid that solid content is 1wt%～20wt% with acetone, and in dispersing apparatus, in normal pressure and room
Under the conditions of temperature, dispersion processes 1 hour to 48 hours, and gained dispersion liquid can be used directly, or filters gained dispersion
Liquid, gained solid formation is after drying as heat filling.
Inventor finds, fills out although the method in above-mentioned patent documentation CN102827480A can improve heat conduction
Material and the contact performance of silicone rubber matrix, but yet suffer from disperseing uneven phenomenon.
Summary of the invention
Therefore, the technical problem to be solved is, it is provided that the preparation method of a kind of heat-conducting silicon rubber,
Utilize the preparation method of this heat-conducting silicon rubber, it is possible to prepare heat filling therein and obtain homodisperse leading
Hot silicone rubber.
In order to solve above-mentioned technical problem, the present invention provides following technical scheme:
The preparation method of a kind of heat-conducting silicon rubber, comprises the steps of
Step 1, heat filling is dispersed in silicone rubber matrix；
Step 2, vulcanizing agent is dispersed in described silicone rubber matrix；
Step 3, described vulcanizing agent and silicone rubber matrix is made to crosslink reaction and obtain heat-conducting silicon rubber；
Wherein, described heat filling is to be prepared as follows the heat filling obtained；
Step (a): make the silane chloride containing at least one double bond, the mercaptan compound of excess and light draw
Send out agent to react under conditions of illumination in the first organic solvent, obtain the first reactant, then remove first
Organic solvent and unreacted mercaptan compound obtain the second reactant, and the second reactant is dissolved in second has
In machine solvent, obtain the solution of the second reactant；
Step (b): make metal dust be dispersed in the solution of described second reactant, then remove described second
The second organic solvent in the solution of reactant；Obtain the compound of described metal dust and described second reactant
Body, described complex is heat filling.
Preferably, the weight average molecular weight of described silicone rubber matrix is 150,000～1,000,000；In described silicone rubber matrix
Vinyl molar content be 0.05%～2%；Described silicone rubber matrix is type siloxane silicone rubber matrix.
Preferably, the number of described silicone rubber matrix and heat filling is respectively 100 parts and 10～40 parts；Institute
The number stating vulcanizing agent is 0.3～5 part.
Preferably, in described step 1, after heat filling is dispersed in silicone rubber matrix, carry out
Comprise the two-stage mixing that first paragraph is mixing and second segment is mixing；The mixing condition of described first paragraph is that temperature is
60～70 DEG C, the time is 5～30 minutes；The mixing condition of described second segment be temperature be 75～85 DEG C, the time is
5～30 minutes.
Preferably, in described step 2, described vulcanizing agent is 2,5-dimethyl-2,5-bis(t-butylperoxy)
Hexane；In step 3, the condition of described cross-linking reaction be temperature be 150～170 DEG C, pressure is
10～100MPa, the retention time is 10～80 minutes.
Preferably, in described step (a), the described silane chloride containing at least one double bond for have as
The dichlorosilane of lower structure:
Wherein, R1Or R2It it is the group with at least one-C=C-double bond；
In described step (a), described mercaptan compound is 3,6-dioxa-1,8-octanedithiol；
In described step (a), described light trigger is double acylphosphine oxides with following structural formula:
In described step (a), the condition of described illumination is to be irradiated under the light that wavelength is 365 nanometers；
In described step (a), described first organic solvent is oxolane；
In described step (a), described second organic solvent is ethanol；
In described step (b), described metal dust is to utilize acid to carry out surface-treated metal dust.
Preferably, in described step (b), described acid is hydrochloric acid or sulphuric acid；Described metal dust selected from copper powder,
Iron powder, bronze, argentum powder, zinc powder or a combination thereof.
Preferably, in described step (b), the particle diameter of described metal dust is 200 nanometers～20 microns.
Preferably, in described step (b), remove the second organic solvent in the solution of described second reactant
Mode be to be dried under inert gas shielding；Described dry temperature is 30～35 DEG C.
It addition, the present invention also provides for a kind of heat-conducting silicon rubber, it is for be prepared by any of the above-described heat-conducting silicon rubber
Method prepares.
It addition, the present invention also provides for a kind of laser projection device, including above-mentioned heat-conducting silicon rubber as heat transfer
Parts.
The preparation method of the heat-conducting silicon rubber according to the present invention, it is possible to prepare heat filling therein and obtain all
Even scattered heat-conducting silicon rubber.Why can prepare heat filling and be dispersed in silicone rubber matrix
Heat-conducting silicon rubber, is because in the present invention, and the heat filling of use is in advance by metal dust and silanes
The heat filling that polymer is compound and obtains, thus by being compounded with silanes polymer and the silicon of metal dust
The good intermiscibility of rubber matrix, improves uniformly dispersed in silicone rubber matrix of heat filling.It addition,
Silicone rubber prepared by the preparation method of the heat-conducting silicon rubber of the present invention, processing characteristics is good, and reason is,
Metal dust being evenly distributed in silicone rubber, will not affect processing characteristics because there are the phenomenons such as reunion.
Accompanying drawing explanation
Fig. 1 is first application of the silicone rubber prepared by the preparation method of the heat-conducting silicon rubber utilizing the present invention
The schematic diagram of mode.
Fig. 2 is second application of the silicone rubber prepared by the preparation method of the heat-conducting silicon rubber utilizing the present invention
The schematic diagram of mode.
Fig. 3 is the 3rd application of the silicone rubber prepared by the preparation method of the heat-conducting silicon rubber utilizing the present invention
The schematic diagram of mode.
Fig. 4 is the 4th application of the silicone rubber prepared by the preparation method of the heat-conducting silicon rubber utilizing the present invention
The schematic diagram of mode.
Fig. 5 is the 5th application of the silicone rubber prepared by the preparation method of the heat-conducting silicon rubber utilizing the present invention
The schematic diagram of mode.
Description of reference numerals:
1 printed circuit board (PCB)
2 metal racks
3 heat-conducting silicon rubbers
4 radiators
5 fluorescent material wheel motors
6 structural members
7 total internal reflection prisms
8 laser instrument
9 liquid cold heads
Detailed description of the invention
In order to those skilled in the art can be more fully understood from technical scheme, below in conjunction with tool
Body embodiment illustrates.
The preparation method of a kind of heat-conducting silicon rubber, comprises the steps of
Step 1, heat filling is dispersed in silicone rubber matrix；
Step 2, vulcanizing agent is dispersed in described silicone rubber matrix；
Step 3, described vulcanizing agent and silicone rubber matrix is made to crosslink reaction and obtain heat-conducting silicon rubber；
Wherein, described heat filling is to be prepared as follows the heat filling obtained；
Step (a): make the silane chloride containing at least one double bond, the mercaptan of excess and light trigger exist
First organic solvent reacts under conditions of illumination, obtains the first reactant, then remove first organic molten
Agent and unreacted mercaptan compound obtain the second reactant, and the second reactant is dissolved in the second organic solvent
In, obtain the solution of the second reactant；
Step (b): make metal dust be dispersed in the solution of described second reactant, then remove described second
The second organic solvent in the solution of reactant；Obtain the compound of described metal dust and described second reactant
Body, described complex is heat filling.
In the preparation method of the heat-conducting silicon rubber of the present invention, by using heat filling as above, can
To improve heat filling dispersing uniformity in silicone rubber matrix.Therefore, in above-mentioned heat filling,
Compound due to metal dust and silanes polymer, recycling silanes polymer is good with silicone rubber matrix
Good intermiscibility, it is possible to increase uniformly dispersed in silicone rubber matrix of heat filling.Due to above-mentioned rubber
Class matrix is also silanes polymer, it is preferable that above-mentioned silanes polymer is phase with above-mentioned silicone rubber matrix
Congener polymer.
Weight average molecular weight about described silicone rubber matrix is not particularly limited, such as can with more than 150,000,
It is specifically as follows 200,000,300,000,400,000,500,000,600,000, about 700,000, more preferably 150,000～100
Ten thousand.The assay method of weight average molecular weight can use the methods such as intrinsic viscosity method.
It addition, can contain vinyl in described silicone rubber matrix, the molar content of vinyl is not
There is particularly restriction.As long as can strengthen being cross-linked to form polymer network.Specifically, the rubbing of vinyl
You are preferably 0.05%～2% by percentage composition.If the molar content of vinyl is less than 0.05%, then can not
Enough fully play crosslinked action；And if the molar content of vinyl is more than 2%, then ultimately form
The crosslink density of silicone rubber is the most excessive, thus decreases elasticity.
About the kind of described silicone rubber matrix, it is not particularly limited.General silicone rubber can be used.
It is specially type siloxane silicone rubber matrix.As silicone rubber, specifically can enumerate: methyl vinyl silicone rubber,
Dimethyl silicone rubber, methyl phenyl vinyl silicone rubber etc..
About described silicone rubber matrix and the proportioning of heat filling, it is not particularly limited.Heat filling
Can as long as content can play increased thermal conductivity.Such as can preferred described silicone rubber matrix and heat conduction fill out
The proportioning of material is respectively 100 parts and 10～40 parts, the most described silicone rubber matrix and the proportioning of heat filling
Being respectively 100 parts and 15～35 parts, the proportioning of further preferred described silicone rubber matrix and heat filling is respectively
It it is 100 parts and 20～30 parts.Specifically, the proportioning of described silicone rubber matrix and heat filling is respectively 100
Part and 25 parts.
About the kind of vulcanizing agent, the most specific restriction, premise is that the work playing cross-linked silicone rubber
With.Usual composition can be used according to the kind of rubber constituent, such as, can enumerate: metal-oxide (oxygen
Change magnesium, zinc oxide etc.), organic peroxide (diacyl peroxide, peroxyester, dialkyl peroxide
Deng), sulfur class vulcanizing agent etc..Further, sulfur class vulcanizing agent is common.As sulfur class vulcanizing agent, can enumerate
The most such as powder sulfur, sedimentation sulfur, colloid sulfur, insoluble sulfur, polymolecularity sulfur, Disulfur dichloride (sulfur monochloride,
Sulfur dichloride) etc..These cross-linking agent may be used singly or in combination of two or more.It addition, burning
Thing can be applied in combination with other vulcanizing agents (sulfur class vulcanizing agent etc.), and metal-oxide and/or sulfur class vulcanizing agent can
To be used alone or to be applied in combination with vulcanization accelerator.The usage amount of vulcanizing agent can be according to vulcanizing agent and rubber
The kind of glue composition from relative to rubber constituent 100 weight portion be in the range of 0.3 weight portion～20 weight portions select
Select, the most preferably 0.3 weight portion～5 weight portions.
When sulfuration, in addition to vulcanizing agent, it is also possible to use other crosslinking coagent or vulcanization accelerator.
Known crosslinking coagent, the most multifunctional (different) cyanurate (such as, triallyl isocyanuric acid can be enumerated
Ester (TAIC), triallylcyanurate (TAC) etc.), polydiene (such as, 1,2-polybutadiene etc.), insatiable hunger
Slaine (such as, (methyl) zinc acrylate resin, (methyl) Magnesium Acrylate Prepared etc.), oximes (such as, quinone two with carboxylic acid
Oxime etc.), guanidine (such as, diphenylguanidine etc.), multifunctional (methyl) acrylate (such as, ethylene glycol bisthioglycolate (methyl)
Acrylate, butanediol two (methyl) acrylate, trimethylolpropane tris (methyl) acrylate etc.), span
Come acid imide (aliphatic BMI, such as, N, N '-ethylene BMI, 1,6 '
-BMI-(2,2,4-trimethyl) hexamethylene etc.；Aromatic hydrocarbons BMI or aromatic series bismaleimide
Amine, such as, N-N '-meta-phenylene bismaleimide, 4-methyl isophthalic acid, 3-phenylene BMI,
Double [4-(4-maleimidephenoxy) phenyl] propane of 4,4 '-diphenyl methane BMI, 2,2-, 4,4 '
Double (the 3-maleimide benzene of-diphenyl ether BMI, 4,4 '-sulfobenzide. BMI, 1,3-
Epoxide) benzene) etc..These crosslinking coagents may be used singly or in combination of two or more.In these crosslinking coagents,
Preferably bismaleimide amine (N, N ' aromatic hydrocarbons BMI or the fragrance such as-meta-phenylene bismaleimide
Race's BMI).By adding bismaleimide amine, it is possible to increase the degree of cross linking, prevent bonding abrasion
Deng.The ratio of crosslinking coagent is counted by solid constituent conversion can be as a example by the silicone rubber relative to 100 weight portions
As selected in the range of 0.01 weight portion～10 weight portions, can be such as 0.1 weight portion～5 weight portions (such as
0.3 weight portion～4 weight portions), preferably 0.5 weight portion～3 weight portions (such as 0.5 weight portion～2 weight portions).
As vulcanization accelerator, such as thuriam acceserator (such as, tetra methylthiuram list sulfur can be enumerated
Compound (TMTM), tetramethyl thiuram disulfide (TMTD), Thiuram disulphide (TETD),
Tetrabutyl thiuram disulfides (TBTD), double pentamethylene thiuram tetrasulfide (DPTT), N, N '-two
Methyl-N, N '-diphenyl thiuram disulfides etc.), thiazole accelerator (such as, 2-mercaptobenzothiazole,
The zinc salt of 2-mercaptobenzothiazole, 2-mercaptothiazoline, bisbenzothiazole disulphide, 2-(4 '-morpholinyl two
Sulfur generation) benzothiazole etc.), sulfenamide type accelerators (such as, N cyclohexyl 2 benzothiazole sulfenamide
(CBS), N, N '-dicyclohexyl-2-[4-morpholinodithio sulfenamide etc.), bismaleimide amine accelerator (such as,
N, N '-meta-phenylene bismaleimide, N, N '-1,2-ethylenebismaleimide etc.), guanidine (diphenyl
Guanidine, di-o-tolyl guanidine etc.), ureas or Thiourea accelerator (such as, ethylene thiourea etc.), dithio ammonia
Base formiate, xanthic acid salt etc..These vulcanization accelerators can be used alone or two or more combination makes
With.In these vulcanization accelerators, TMTD, DPTT, CBS etc. are widely used.The ratio of vulcanization accelerator
Can be such as 0.1 weight portion～15 weight relative to 100 parts by weight of silicone rubber matrixes in terms of solid constituent conversion
Part, preferably 0.3 weight portion～10 weight portions, more preferably 0.5 weight portion～5 weight portions.
It addition, for the mixing mode of the present invention, be not particularly limited, as long as can play each silicon
The raw material of rubber is mixing uniformly.Such as can mix by using the mixing roll such as banbury, mill
Refining.And mixing hop count (or referred to as number of times) is not particularly limited.Can be such as one section mixing or
Person two sections is mixing.Preferably, in described step 1, use two-stage mixing.That is, heat filling is being divided
After being dissipated in silicone rubber matrix, can carry out comprising the two-stage mixing that first paragraph is mixing and second segment is mixing.
For mixing condition, also it is that there is no particular limitation.Go out in terms of taking into account melting efficiency and mixing uniformity
Send out, the mixing condition of described first paragraph be temperature be 60～70 DEG C, the time is 5～30 minutes.Can preferred institute
State the mixing condition of second segment be temperature be 75～85 DEG C, the time is 5～30 minutes.
About the vulcanizing agent used in described step 2, such as, can use vulcanizing agent as enumerated above.
2,5-dimethyl-2,5-bis(t-butylperoxy) hexane is preferably used as vulcanizing agent.
About the condition of described cross-linking reaction in step 3, it is not particularly limited, as long as can carry
Make to cause cross-linking reaction for enough energy.Such as preferable temperature is 150～170 DEG C, and pressure is
10～100MPa, the retention time is 10～80 minutes.
It addition, in described step (a), the described silane chloride containing at least one double bond preferably has
The dichlorosilane of following structure:
Wherein, R1Or R2For having the group of at least one-C=C-double bond.R1Or R2Can be identical or not
With.Specifically, R1Or R2Can be the alkyl or alkenyl with-C=C-a double bond, such as, can be band
Have the ethyl an of-C=C-double bond, propyl group, isopropyl, butyl, isobutyl group, sec-butyl, the tert-butyl group, penta
Base, isopentyl, neopentyl, tertiary pentyl, hexyl, isohesyl, heptyl, octyl group, nonyl, decyl etc..
In described step (a), described mercaptan compound can be n-dodecyl mercaptan, ethanethio, fourth
The straight chain type thiols such as base mercaptan, but it is not limited to this.In the present invention, 3,6-dioxa-1,8-octane two sulfur
Alcohol can be as preferred example.
It addition, in described step (a), as light trigger, such as can enumerate: benzil, benzoin
Ether, benzoin butyl ether, benzoin propyl ether, benzophenone, 3,3 '-dimethyl-4-methoxy benzophenone, benzene
Carbamoyl benzoate, the carboxylate of benzoylbenzoic acid, 4-benzoyl-4 '-methyldiphenyl thioether, benzil
Dimethyl ketal, 2-butoxyethyl group-4-methylamino acid ester, clopenthixal ketone, methyl thiaxanthone, ethyl
Thiaxanthone, isopropyl thioxanthone, dimethyl thioxanthone, diethyl thioxanthone, diisopropylthioxanthone, two
Methyaminomethyl benzoate, 1-(4-dodecylphenyl)-2-hydroxy-2-methyl propane-1-ketone, 1-hydroxy cyclohexylphenyl
Base phenyl ketone, 2-hydroxy-2-methyl-1-phenyl-propane-1-ketone, 1-(4-isopropyl phenyl)-2-hydroxy-2-methyl
Propane-1-ketone, methyl benzoylformate, 2-methyl isophthalic acid-(4-methyl mercapto phenyl)-2-morpholino propane-1-ketone, 2-
Double (trichloromethyl)-6-(the 4-methoxybenzene of benzyl-2-dimethylamino-1-(4-morphlinophenyl)-1-butanone, 2,4-
Base)-1,3,5-s-triazine, 2,4,6-tri-(trichloromethyl)-1,3,5-s-triazine, double (trisbromomethyl)-6-(the 4 '-first of 2,4-
Phenyl)-1,3,5-s-triazine, 2,4,6-tri-(trisbromomethyl)-1,3,5-s-triazine, double (three chloromethanes of 2,4-
Base)-6-(1,3-benzodioxolane-5-base)-1,3,5-s-triazine, benzophenone, benzoylbenzoic acid, 1-(4-
Phenylsulfanylphenyl) butane-1,2-diketone-2-oxime-O-benzoate, 1-(4-methyl mercapto phenyl) butane-1,2-diketone-2-
Oxime-O-acetas, 1-(4-methyl mercapto phenyl) butane-1-ketoxime-O-acetas, 4,4 '-bis-(lignocaine) hexichol
Ketone, IADB, (dimethylamino)-ethyl benzoate, 2,2 '-bis-(O-chlorobenzenes
Base)-4,4 ', 5,5 '-tetraphenyl-1,2 ' and-bisglyoxaline, diazo naphthoquinone class initiator etc..It is also preferable to use
Phosphine oxide system light trigger.The double acylphosphine oxides with following structural formula such as can be preferably used:
It addition, in described step (a), the condition of described illumination is not particularly limited.For specifically
Light trigger, for double acylphosphine oxides as escribed above, is preferably to enter under the light that wavelength is 365 nanometers
Row irradiates.It addition, in described step (a), described first organic solvent is preferably oxolane.It addition,
In described step (a), described second organic solvent is preferably ethanol.
About above-mentioned steps (b), described metal dust is preferably and utilizes acid to carry out surface-treated metal dust.
Described acid is not limited, such as, can be mineral acid or organic acid.As long as metal powder can be removed
The spot on surface, end.As mineral acid, can enumerate: hydrochloric acid, sulphuric acid, nitric acid, phosphoric acid, boric acid
Deng.As organic acid, can enumerate: formic acid, acetic acid, propanoic acid, butanoic acid, gallic acid, succinic acid etc..
Wherein, preferably hydrochloric acid or sulphuric acid.Concentration about hydrochloric acid or sulphuric acid is not particularly limited, but with
One premise, i.e. when metal dust can have reactivity with acid, such as when metal dust is iron powder, ferrum
Powder just can generate hydrogen with acid reaction, then now the requirement to acid is that concentration can not be too high.Such as conduct
Hydrochloric acid can use dilute hydrochloric acid or dilute sulfuric acid, the such as concentration dilute hydrochloric acid less than 1% or dilute sulfuric acid.Described
In step (b), described metal dust is preferably selected from copper powder, iron powder, bronze, argentum powder, zinc powder or a combination thereof.
Particle diameter for the described metal dust in described step (b) is not particularly limited, preferably 200 nanometers
～20 microns.If the particle diameter of metal dust is less than 200 nanometers, then it is very easy to reunite, thus affects behaviour
The property made, nor be easily dispersed in above-mentioned acid.If the particle diameter of metal dust is more than 20 microns, then hold
Easily there is sedimentation phenomenon, and cause dispersion inequality.Furthermore it is preferred that in described step (b), remove institute
The mode stating the second organic solvent in the solution of the second reactant is to be dried under inert gas shielding.
Preferably, described dry temperature is 30～35 DEG C.
Hereinafter, by specific embodiment, technical scheme is described in detail.
Method of testing:
The method of testing use american standard of testing material of thermal conductivity: ASTM D5470
The method of testing use american standard of testing material of hot strength: ASTM D638
Chemical sources is as shown in table 1 below:
Table 1
It should be noted that in embodiment of the present invention (including embodiment), without specified otherwise,
" part " refers to " weight portion ".
Embodiment 1
Step 1, by 80 parts of raw-silastic continuouslies (that is, silicone rubber matrix), 20 parts of silicone oil, 10 parts of heat fillings
(preparation method of heat filling is as described later) carries out first paragraph mixing 30 minutes at 60 DEG C；After be warming up to
75 DEG C carry out second segment mixing 30 minutes；
Step 2, raw material after mixing add 0.3 part of 2,5-dimethyl-2,5-bis(t-butylperoxy) oneself
Alkane；
Step 3, at 150 DEG C, under pressure 10MPa hot-forming 80 minutes, i.e. obtain heat-conducting silicon rubber.
The preparation of heat filling
The preparation method of the heat filling in the present embodiment is as follows:
78 parts of dichlorosilanes, 1 part of 3,6-dioxa-1,8-octanedithiol, 1 part of BAPO are depended on by step (a)
Secondary join in tetrahydrofuran solution, be stirred at room temperature, after question response thing is completely dissolved, be kept stirring for shape
State is reacted 1 hour under the illumination that illumination wavelength is 365 nanometers.Vacuum removes tetrahydrochysene furan after completion of the reaction
Mutter, product is precipitated three times in normal hexane, utilize bag filter to dialyse in aqueous three days and remove not
Reaction mercaptan compound, be dissolved in ethanol solution after being dried under vacuum to constant weight, and with bubbling argon deaerate 30
Minute, obtain modified dichlorosilane solution.
The Fe powder that 1 part of particle diameter is 20 microns is dissolved in the hydrochloric acid solution that concentration is 2% by step (b), stirring
Filter after 15 minutes, flush three times with isopropanol, dried at 35 DEG C in argon atmosphere, add
In the modified dichlorosilane solution that step (a) is prepared, it is dried at 35 DEG C after being stirred at room temperature 1 hour,
Obtain heat filling.
Embodiment 2
Step 1, by 100 parts of raw-silastic continuouslies (that is, silicone rubber matrix), 40 parts of heat filling (heat fillings
Preparation method as described later) at 70 DEG C, carry out first paragraph mixing 5 minutes；After be warming up to 85 DEG C and carry out
Two-stage mixing 5 minutes；
Step 2, raw material after mixing add 5 parts of 2,5-dimethyl-2,5-bis(t-butylperoxy) hexanes；
Step 3, at 170 DEG C, under pressure 100MPa hot-forming 80 minutes, i.e. obtain heat-conducting silicon rubber.
The preparation of heat filling
The preparation method of the heat filling in the present embodiment is as follows:
Step (a) is by 100 parts of dichlorosilanes, 10 parts of 3,6-dioxa-1,8-octanedithiol, 10 parts of BAPO
It is added sequentially in tetrahydrofuran solution, is stirred at room temperature, after question response thing is completely dissolved, be kept stirring for
State is reacted 24 hours under the illumination that illumination wavelength is 365 nanometers.Vacuum removes tetrahydrochysene furan after completion of the reaction
Mutter, product is precipitated three times in normal hexane, utilize bag filter to dialyse in aqueous three days and remove not
Reaction mercaptan compound, be dissolved in ethanol solution after being dried under vacuum to constant weight, and with bubbling argon deaerate 30
Minute, obtain modified dichlorosilane solution.
The Au powder that 3 parts of particle diameters are 200 nanometers is dissolved in the hydrochloric acid solution that concentration is 2% by step (b), stirring
Filter after 15 minutes, flush three times with isopropanol, dried at 30 DEG C in argon atmosphere, add
In the modified dichlorosilane solution that step (a) is prepared, dry at 30 DEG C after being stirred at room temperature 16 hours
Dry, obtain heat filling.
Embodiment 3
Step 1, by 90 parts of raw-silastic continuouslies (that is, silicone rubber matrix), 10 parts of silicone oil, 30 parts of heat fillings
(preparation method of heat filling is as described later) carries out first paragraph mixing 20 minutes at 65 DEG C；After be warming up to
80 DEG C carry out second segment mixing 20 minutes；
Step 2, raw material after mixing add 3 parts of 2,5-dimethyl-2,5-bis(t-butylperoxy) hexanes；
Step 3, at 160 DEG C, under pressure 90MPa hot-forming 60 minutes, i.e. obtain heat-conducting silicon rubber.
The preparation of heat filling
The preparation method of the heat filling in the present embodiment is as follows:
90 parts of dichlorosilanes, 6 parts of 3,6-dioxa-1,8-octanedithiol, 6 parts of BAPO are depended on by step (a)
Secondary join in tetrahydrofuran solution, be stirred at room temperature, after question response thing is completely dissolved, be kept stirring for shape
State is reacted 18 hours under the illumination that illumination wavelength is 365 nanometers.Vacuum removes tetrahydrochysene furan after completion of the reaction
Mutter, product is precipitated three times in normal hexane, utilize bag filter to dialyse in aqueous three days and remove not
Reaction mercaptan compound, be dissolved in ethanol solution after being dried under vacuum to constant weight, and with bubbling argon deaerate 30
Minute, obtain modified dichlorosilane solution.
The Cu powder that 2 parts of particle diameters are 10 microns is dissolved in the hydrochloric acid solution that concentration is 2% by step (b), stirring
Filter after 15 minutes, flush three times with isopropanol, dried at 30 DEG C in argon atmosphere, add
In the modified dichlorosilane solution that step (a) is prepared, dry at 30 DEG C after being stirred at room temperature 10 hours
Dry, obtain heat filling.
For the heat-conducting silicon rubber prepared by embodiment 1～3, according to american standard of testing material: ASTM
D5470 and ASTM D638, respectively test thermal conductivity and hot strength.Result is as shown in table 2 below.
Table 2
| Thermal conductivity (W/M K) | Hot strength (MPa) | |
| Embodiment 1 | 2 | 5 |
| Embodiment 2 | 4 | 8 |
| Embodiment 3 | 3 | 7 |
As can be seen from Table 2, heat-conducting silicon rubber prepared by the preparation method of the present invention, not only heat are utilized
Conductance is high, and hot strength is the highest.
Embodiment 4
The present embodiment provides preparation method (the preparation side of embodiment 1 of a kind of heat-conducting silicon rubber utilizing the present invention
Method) prepared by the first application scenario of silicone rubber.Refer to Fig. 1.Prop up at printed circuit board (PCB) 1 and metal
Heat-conducting silicon rubber 3 can be used between frame 2 to connect, thus both can ensure that the heat of printed circuit board (PCB) 1
It is transferred to rapidly metal rack 2, can ensure that again heat-conducting silicon rubber 3 is by printed circuit board (PCB) 1 and metal rack 2
Firmly connect.This kind of connected mode goes for the printed circuit board (PCB) 1 in laser projection device and metal
Connection between support 2.The heat transfer component that heat-conducting silicon rubber 3 is considered as in laser projection device.Fig. 1
In in order to understand each parts of performance, thus it is shown that printed circuit board (PCB) 1, metal rack 2 and they between
The decomposition view of heat-conducting silicon rubber 3, is not the view after connecting.
Embodiment 5
The present embodiment provides preparation method (the preparation side of embodiment 1 of a kind of heat-conducting silicon rubber utilizing the present invention
Method) prepared by the second application scenario of silicone rubber.Refer to Fig. 2.At printed circuit board (PCB) 1 and radiator
Heat-conducting silicon rubber 3 can be used between 4 to connect, thus both can ensure that the heat of printed circuit board (PCB) 1 was fast
Speed is transferred to radiator 4, can ensure that again heat-conducting silicon rubber 3 is between printed circuit board (PCB) 1 and radiator 4
Form bigger contact area, improve radiating effect.This kind of connected mode goes for laser projection device
In printed circuit board (PCB) 1 and radiator 4 between connection.Heat-conducting silicon rubber 3 is considered as in laser projection device
A heat transfer component.In order to understand each parts of performance in Fig. 2, thus it is shown that printed circuit board (PCB) 1, heat radiation
Device 4 and the decomposition view of the heat-conducting silicon rubber between them 3, be not the view after connecting.
Embodiment 6
The present embodiment provides preparation method (the preparation side of embodiment 1 of a kind of heat-conducting silicon rubber utilizing the present invention
Method) prepared by the third application scenario of silicone rubber.Refer to Fig. 3.Such as in laser projection device
It is usually mounted with radiator 4 on fluorescent material wheel motor 5 and is beneficial to the heat radiation of fluorescent material wheel motor 5.Now,
If connecting fluorescent material wheel motor 5 and radiator 4 by heat-conducting silicon rubber 3, the most both can ensure that fluorescence
The heat of powder wheel motor 5 is transferred to rapidly radiator 4, can ensure that again heat-conducting silicon rubber 3 is taken turns at fluorescent material
Form bigger contact area between motor 5 and radiator 4, improve radiating effect.Heat-conducting silicon rubber 3 regards
For a heat transfer component in laser projection device.In order to understand each parts of performance in Fig. 3, thus it is shown that glimmering
Light powder wheel motor 5, radiator 4 and the decomposition view of the heat-conducting silicon rubber between them 3, be not even
View after connecing.
Embodiment 7
The present embodiment provides preparation method (the preparation side of embodiment 1 of a kind of heat-conducting silicon rubber utilizing the present invention
Method) prepared by the 4th kind of application scenario of silicone rubber.Refer to Fig. 4.Such as in laser projection device
It is provided with between structural member 6 and total internal reflection prism (Total internal reflection prism is called for short TIR) 7
Heat-conducting silicon rubber 3.Heat-conducting silicon rubber 3 both can ensure that structural member 6 and the connection of total internal reflection prism 7,
The rapid transmission of heat can be realized again.Described structural member 6 predominantly load-carrying member, it is suitable preferably to have
Strength and stiffness.The heat transfer component that heat-conducting silicon rubber 3 is considered as in laser projection device.In Fig. 4 in order to
Clearly show each parts, thus it is shown that structural member 6, total internal reflection prism 7 and the thermal conductive silicon between them
The decomposition view of rubber 3, is not the view after connecting.
Embodiment 8
The present embodiment provides preparation method (the preparation side of embodiment 1 of a kind of heat-conducting silicon rubber utilizing the present invention
Method) prepared by the 5th kind of application scenario of silicone rubber.Refer to Fig. 5.Such as in laser projection device
Heat-conducting silicon rubber 3 it is provided with between laser instrument 8 and liquid cold head 9.Heat-conducting silicon rubber 3 both can connect laser
Device 8 and liquid cold head 9, can be rapidly transferred to liquid cold head 9 by heat produced by laser instrument 8 again, thus
Liquid cold head 9 can be made full use of laser instrument 8 is cooled down, it is ensured that laser instrument 8 operation steady in a long-term.Lead
The heat transfer component that hot silicone rubber 3 is considered as in laser projection device.In order to understand each parts of performance in Fig. 5,
It is illustrated that laser instrument 8, liquid cold head 9 and the decomposition view of the heat-conducting silicon rubber between them 3, not
It it is the view after connecting.
Although technical scheme being illustrated in conjunction with detailed description of the invention and specific embodiment, but
It is to those skilled in the art, on the premise of without departing from spirit and principles of the present invention, it is also possible to
Make various modifications and changes.Therefore, these modifications and changes should be considered as protection scope of the present invention it
In.
Claims (11)
1. a preparation method for heat-conducting silicon rubber, comprises the steps of
Step 1, heat filling is dispersed in silicone rubber matrix；
Step 2, vulcanizing agent is dispersed in described silicone rubber matrix；
Step 3, described vulcanizing agent and described silicone rubber matrix is made to crosslink reaction and obtain heat-conducting silicon rubber；
Wherein, described heat filling is to be prepared as follows the heat filling obtained；
Step (a): make the silane chloride containing at least one double bond, the mercaptan compound of excess and light draw
Send out agent to react under conditions of illumination in the first organic solvent, obtain the first reactant, then remove first
Organic solvent and unreacted mercaptan compound obtain the second reactant, and the second reactant is dissolved in second has
In machine solvent, obtain the solution of the second reactant；
Step (b): make metal dust be dispersed in the solution of described second reactant, then remove described second
The second organic solvent in the solution of reactant；Obtain the compound of described metal dust and described second reactant
Body, described complex is heat filling.
The preparation method of heat-conducting silicon rubber the most according to claim 1, it is characterised in that described silicon rubber
The weight average molecular weight of gum base body is 150,000～1,000,000；Vinyl molar content in described silicone rubber matrix
It is 0.05%～2%；Described silicone rubber matrix is type siloxane silicone rubber matrix.
The preparation method of heat-conducting silicon rubber the most according to claim 1, it is characterised in that described silicon rubber
The number of gum base body and heat filling is respectively 100 parts and 10～40 parts；The number of described vulcanizing agent is 0.3～5
Part.
The preparation method of heat-conducting silicon rubber the most according to claim 1, it is characterised in that in described step
In rapid 1, after being dispersed in silicone rubber matrix by heat filling, carry out comprising first paragraph mixing and second
The two-stage mixing that section is mixing；The mixing condition of described first paragraph be temperature be 60～70 DEG C, the time is 5～30 points
Clock；The mixing condition of described second segment be temperature be 75～85 DEG C, the time is 5～30 minutes.
The preparation method of heat-conducting silicon rubber the most according to claim 1, it is characterised in that in described step
In rapid 2, described vulcanizing agent is 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane；In step 3, institute
State the condition of cross-linking reaction be temperature be 150～170 DEG C, pressure is 10～100MPa, and the retention time is 10～80
Minute.
The preparation method of heat-conducting silicon rubber the most according to claim 1, it is characterised in that in described step
Suddenly, in (a), the described silane chloride containing at least one double bond is the dichlorosilane with following structure:
Wherein, R1Or R2It it is the group with at least one-C=C-double bond；
In described step (a), described mercaptan compound is 3,6-dioxa-1,8-octanedithiol；
In described step (a), described light trigger is double acylphosphine oxides with following structural formula:
In described step (a), the condition of described illumination is to be irradiated under the light that wavelength is 365 nanometers；
In described step (a), described first organic solvent is oxolane；
In described step (a), described second organic solvent is ethanol；
In described step (b), described metal dust is to utilize acid to carry out surface-treated metal dust.
The preparation method of heat-conducting silicon rubber the most according to claim 6, it is characterised in that in described step
Suddenly, in (b), described acid is hydrochloric acid or sulphuric acid；Described metal dust selected from copper powder, iron powder, bronze, argentum powder,
Zinc powder or a combination thereof.
The preparation method of heat-conducting silicon rubber the most according to claim 1, it is characterised in that in described step
Suddenly, in (b), the particle diameter of described metal dust is 200 nanometers～20 microns.
The preparation method of heat-conducting silicon rubber the most according to claim 1, it is characterised in that in described step
Suddenly, in (b), the mode removing the second organic solvent in the solution of described second reactant is to protect at noble gas
Protect down and be dried；Described dry temperature is 30～35 DEG C.
10. a heat-conducting silicon rubber, it is for being prepared by the heat-conducting silicon rubber according to any one of claim 1～9
Method prepares.
11. 1 kinds of laser projection device, it is characterised in that include the heat-conducting silicon rubber described in claim 10
As heat transfer component.
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| CN107365456A (en) * | 2017-09-15 | 2017-11-21 | 厦门万新橡胶有限公司 | A kind of novel graphite alkene is modified heat conductive rubber |
| CN111174966A (en) * | 2020-01-06 | 2020-05-19 | 中国科学院微电子研究所 | Heat radiation structure and capacitive pressure sensor |
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|---|---|---|---|---|
| CN101597430B (en) * | 2009-07-03 | 2011-05-11 | 广东信力特种橡胶制品有限公司 | Preparation method of filled-type thermally conductive silicone rubber composite material |
| CN102827480A (en) * | 2012-09-03 | 2012-12-19 | 华东理工大学 | Method for preparing high-heat-conducting silicon rubber compound material |
| CN104262971A (en) * | 2014-08-28 | 2015-01-07 | 华南理工大学 | High heat conductive thermally-vulcanized silicone rubber composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101597430B (en) * | 2009-07-03 | 2011-05-11 | 广东信力特种橡胶制品有限公司 | Preparation method of filled-type thermally conductive silicone rubber composite material |
| CN102827480A (en) * | 2012-09-03 | 2012-12-19 | 华东理工大学 | Method for preparing high-heat-conducting silicon rubber compound material |
| CN104262971A (en) * | 2014-08-28 | 2015-01-07 | 华南理工大学 | High heat conductive thermally-vulcanized silicone rubber composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107365456A (en) * | 2017-09-15 | 2017-11-21 | 厦门万新橡胶有限公司 | A kind of novel graphite alkene is modified heat conductive rubber |
| CN111174966A (en) * | 2020-01-06 | 2020-05-19 | 中国科学院微电子研究所 | Heat radiation structure and capacitive pressure sensor |
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