CN106317652A - Ethylene-Propylene-Diene Monomer (EPDM)-silicone rubber blended thermal conductive rubber TIM and preparation method - Google Patents
Ethylene-Propylene-Diene Monomer (EPDM)-silicone rubber blended thermal conductive rubber TIM and preparation method Download PDFInfo
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- CN106317652A CN106317652A CN201610686066.XA CN201610686066A CN106317652A CN 106317652 A CN106317652 A CN 106317652A CN 201610686066 A CN201610686066 A CN 201610686066A CN 106317652 A CN106317652 A CN 106317652A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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- 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
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- 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
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Abstract
The invention discloses an EPDM-silicone rubber blended thermal conductive rubber TIM. The EPDM-silicone rubber blended thermal conductive rubber TIM comprises the following raw materials in parts by weight: 20 to 40 parts of silicone rubber matrixes, 55 to 75 parts of EPDM, 18 to 26 parts of aluminum nitride, 13 to 20 parts of dopamine, 20 to 35 parts of silver nitrate solutions with the concentration of 20 mmol/L, 1 to 3 parts of hydroxyl silicone oil, 2 to 5 parts of bi-2,5-curing agents, appropriate amounts of deionized water and Tris-HCl buffer solutions and 1.5 to 3 parts of gamma-aminopropyltriethoxysilane. According to the invention, oxidative polymerization of the dopamine is carried out on the surface of aluminium nitride to form a tightly adhered polydopamine layer, and silver nanoparticles are loaded on the surface of the polydopamine layer coating aluminium nitride, and silicone rubber is compounded and filled, so that high thermal conductivity and heat dissipation performances of the silicone rubber TIM are improved, and the EPDM-silicone rubber blended thermal conductive rubber TIM further has good flexibility, and tear strength and electric insulation properties.
Description
Technical field
The invention belongs to thermal interfacial material field, be specifically related to the heat conduction rubber of a kind of ethylene propylene diene rubber-silicone rubber
Glue thermal interfacial material and preparation method.
Background technology
Along with LED manufactures and the continuous progress of packaging technology, the power of LED is increasing.At present, commercialization is high-power
LED input power is typically at more than 1W, and chip area 1mm × 1mm, heat flow density is at 100W/cm2Above, cooling requirements is very
High.Heat passes to external environment condition from chip, if to pass through dry interface, gap, the warpage of substrate between interface all can affect key
Close and the heat radiation of local, form interface resistance.Along with LED is to high-power, high brightness development, interface resistance has become LED industry
One of difficult problem, it is necessary to solve from many-sides such as thermal interfacial material (TIM), radiator structures, and thermal interfacial material is to reduce greatly
One of effective means of Power LED lamps median surface thermal resistance.
Heat-conducting silicon rubber has the insulating properties of excellence, can fast and effeciently remove the heat that electronic equipment produces simultaneously
Amount, improves service life and the work efficiency of electronic equipment.High thermal conductivity silicone rubber is mainly filled-type thermally conductive rubber, by high score
Subbase body and high heat filling composition, wherein heat filling is main heat conduction carrier.Conventional heat filling has metal class, oxygen
Compound class, nitride-based, carbon compound etc..Wherein aluminium nitride high purity single crystal body theory thermal conductivity is up to 320W/ (m K), has
Reliably electrical insulation capability, relatively low dielectric loss and dielectric constant, be preferable heat filling, but due to the aluminium nitride moisture absorption after
Can be with water generation hydrolysis, the Al (OH) of generation3Thermal conducting path can be made to produce interrupt, and then affect the transmission of phonon, therefore
Doing finished product after heat conductance on the low side, even if using silane coupler to carry out surface process, cannot guarantee that 100% filling surface is wrapped
Cover.
The most another, Jiang Jinhong et al. in " dopamine surface-functionalized from poly-attachment behavior and the film " literary composition delivered,
Review dopamine progress in surface modification, to dopamine from poly-composite modification theory and surface-functionalized
The application of aspect is described above in detail.Under aqueous conditions, dopaminergic aoxidizes-cross-linking reaction, shape under the effect of dissolved oxygen
The poly-dopamine becoming strength to be attached to a series of solid material surfaces such as polymer, metal, pottery, glass, timber is combined thin layer,
And with there is reactivity poly-dopamine composite bed as platform, film is carried out further surface and modifies and can realize the merit of film
Energyization.
Therefore, the present invention utilizes poly-dopamine to be coated with aluminium nitride, improves its thermal conductivity, and a kind of heat conductivity of preparation is high, absolutely
The high thermal conductive silicon rubber thermal interfacial material that edge performance is good, the poly-Dopamine of good stability is modified.
Summary of the invention
For above-mentioned deficiency, the present invention provides the heat conductive rubber hot interface material of a kind of ethylene propylene diene rubber-silicone rubber
Material and preparation method.
The heat conductive rubber thermal interfacial material of a kind of ethylene propylene diene rubber-silicone rubber, by the raw material group of following weight portion
Become: silicone rubber matrix 20-40 part, ethylene propylene diene rubber 55-75 part, aluminium nitride 18-26 part, dopamine 13-20 part, 20mmol/L
Silver nitrate solution 20-35 part, hydroxy silicon oil 1-3 part, double-2,5 vulcanizing agent 2-5 parts, deionized water is appropriate, and Tris-HCl buffers
Solution is appropriate, gamma-aminopropyl-triethoxy-silane 1.5-3 part.
Specifically comprise the following steps that
(1) preparation of poly-Dopamine modification aluminium nitride:
Being added by aluminium nitride in deionized water, in ultrasonic container, ultrasonic disperse 30-50 minute, is subsequently adding aqueous dopamine solution
Uniform by magnetic stirrer, regulating its pH value with Tris-HCl buffer solution is 8.5, stirs sample reaction at ambient temperature
20-24 hour filter, deionized water wash becomes colorless to filtrate, in drying baker 50-70 DEG C dry 20-24 hour, gained produce
Product are the aluminium nitride of Surface coating poly-DOPA amine layer；
(2) preparation of the aluminium nitride that nanometer silver is modified:
Poly-Dopamine step (1) obtained is modified aluminium nitride and is immersed in the silver nitrate solution of 20mmol/L, in stirring
Under state, centrifugal after reacting 6-10 hour, it is washed with deionized, nitrogen dries up, and obtains the aluminium nitride that nanometer silver is modified；
(3) refining glue:
1., by ethylene propylene diene rubber together with silicone rubber matrix on twin-screw extruder mixing to hard-pressed bale preliminary roller, add γ-ammonia
Propyl-triethoxysilicane and hydroxy silicon oil, mixing 40-60 minute；
2. the aluminium nitride adding the nanometer silver modification obtained by step (2), afterwards continues mixing 20-30 minute, and discharging is cooled to
Room temperature, stands 20-24 hour, obtains heat-conducting silicon rubber elastomeric compound；
(4) by the elastomeric compound obtained by step (3) on twin shaft mixing roll thin logical 4-6 time, thin logical during add double-2,5 sulfur
Agent, after thin pass-out sheet, at 160-190 DEG C, hot press moulding vulcanizes 10-30 minute, obtains the sheet silicon glue material of forming；
(5) by sheet silicon glue material post-cure 3-5 hour at 190-220 DEG C of the forming obtained by step (4), obtain
A kind of heat conductive rubber thermal interfacial material of ethylene propylene diene rubber-silicone rubber.
Wherein, in described step (1), the concentration of aqueous dopamine solution is 1.5-2.5g/L.
The present invention compared with prior art has the advantage that
(1) in aqueous, the most oxidized generation of the catechol group of dopamine has the dopamine of adjacent benzene two quinone structure
Naphtoquinone compounds, occurs anti-dismutation reaction to produce Semiquinone Radicals then, and then coupling forms cross-bond, simultaneously at aln surface
Form the poly-DOPA amine layer of close attachment, effectively prevent aluminium nitride from hydrolyzing, ensure the thermal conductivity that aluminium nitride is excellent, improve silicon
The high heat conduction and heat radiation performance of rubber thermal interfacial material.
(2) catechol group and the quinoid group on poly-dopamine surface has complexing to silver ion, makes silver ion
Absorption is on its surface, and the most poly-dopamine utilizes the oxidation-reduction quality silver ion in-situ chemical reduction by absorption of surface phenolic hydroxyl group
Becoming Nano silver grain to be fixed on the poly-DOPA amine layer surface of cladding aluminium nitride, heat carrier cording has higher compactness, in order to fill out
Filling silicone rubber makes product have higher heat-conductivity, and has good compliance, tearing strength and electrical insulation capability simultaneously.
(3) ethylene propylene diene rubber has good tolerance to cold, thermostability, resistance to acids and bases, electric insulating quality and higher machine
Tool intensity, price ratio is less expensive in addition, and the present invention uses silicone rubber and ethylene propylene diene rubber and with reducing the hot interface of silicone rubber
The cost of material, and be effectively improved the mechanical strength of product, the electric property after water-fast vapor permeability and immersion.
Detailed description of the invention
The heat conductive rubber thermal interfacial material of a kind of ethylene propylene diene rubber-silicone rubber, by following weight portion (kilogram)
Raw material forms: silicone rubber matrix 30, ethylene propylene diene rubber 65, aluminium nitride 23, dopamine 17, the silver nitrate solution of 20mmol/L
28, hydroxy silicon oil 2, double-2,5 vulcanizing agents 4, deionized water is appropriate, and Tris-HCl buffer solution is appropriate, γ-aminopropyl three ethoxy
Base silane 2.
Specifically comprise the following steps that
(1) preparation of poly-Dopamine modification aluminium nitride:
Aluminium nitride is added in deionized water, ultrasonic disperse 40 minutes in ultrasonic container, be subsequently adding aqueous dopamine solution and use
Magnetic stirrer is uniform, and regulating its pH value with Tris-HCl buffer solution is 8.5, and stirring sample at ambient temperature, to react 24 little
Time filter, deionized water wash becomes colorless to filtrate, in drying baker 60 DEG C be dried 24 hours, obtain the poly-dopamine of Surface coating
The aluminium nitride of layer；
(2) preparation of the aluminium nitride that nanometer silver is modified:
Poly-Dopamine step (1) obtained is modified aluminium nitride and is immersed in the silver nitrate solution of 20mmol/L, in stirring
Under state, centrifugal after reacting 9 hours, it is washed with deionized, nitrogen dries up, and obtains the aluminium nitride that nanometer silver is modified；
(3) refining glue:
1., by ethylene propylene diene rubber together with silicone rubber matrix on twin-screw extruder mixing to hard-pressed bale preliminary roller, add γ-ammonia
Propyl-triethoxysilicane and hydroxy silicon oil, mixing 50 minutes；
2. the aluminium nitride adding the nanometer silver modification obtained by step (2), afterwards continues mixing 25 minutes, and discharging is cooled to room
Temperature, stands 24 hours, obtains heat-conducting silicon rubber elastomeric compound；
(4) by the elastomeric compound obtained by step (3) on twin shaft mixing roll thin logical 6 times, thin logical during add double-2,5 sulfurations
Agent, after thin pass-out sheet, at 170 DEG C, hot press moulding vulcanizes 20 minutes, obtains the sheet silicon glue material of forming；
(5) by sheet silicon glue material post-cure 4 hours at 200 DEG C of the forming obtained by step (4), a kind of three are obtained
The heat conductive rubber thermal interfacial material of unit's EP rubbers-silicone rubber.
Wherein, in step (1), the concentration of aqueous dopamine solution is 2g/L.
Test its performance data as follows: hardness 49shore A；Tearing strength 5.1kN/m；Heat conductivity 6.2W/ (m K)；
Specific insulation > 1013Ω·cm。
Claims (3)
1. the heat conductive rubber thermal interfacial material of ethylene propylene diene rubber-silicone rubber, it is characterised in that by following weight portion
Raw material composition: silicone rubber matrix 20-40 part, ethylene propylene diene rubber 55-75 part, aluminium nitride 18-26 part, dopamine 13-20 part,
Silver nitrate solution 20-35 part of 20mmol/L, hydroxy silicon oil 1-3 part, double-2,5 vulcanizing agent 2-5 parts, deionized water is appropriate,
Tris-HCl buffer solution is appropriate, gamma-aminopropyl-triethoxy-silane 1.5-3 part.
2. according to the heat conductive rubber thermal interfacial material of a kind of ethylene propylene diene rubber-silicone rubber described in claims 1
Preparation method, it is characterised in that specifically comprise the following steps that
(1) preparation of poly-Dopamine modification aluminium nitride:
Being added by aluminium nitride in deionized water, in ultrasonic container, ultrasonic disperse 30-50 minute, is subsequently adding aqueous dopamine solution
Uniform by magnetic stirrer, regulating its pH value with Tris-HCl buffer solution is 8.5, stirs sample reaction at ambient temperature
20-24 hour filter, deionized water wash becomes colorless to filtrate, in drying baker 50-70 DEG C dry 20-24 hour, gained produce
Product are the aluminium nitride of Surface coating poly-DOPA amine layer；
(2) preparation of the aluminium nitride that nanometer silver is modified:
Poly-Dopamine step (1) obtained is modified aluminium nitride and is immersed in the silver nitrate solution of 20mmol/L, in stirring
Under state, centrifugal after reacting 6-10 hour, it is washed with deionized, nitrogen dries up, and obtains the aluminium nitride that nanometer silver is modified；
(3) refining glue:
1., by ethylene propylene diene rubber together with silicone rubber matrix on twin-screw extruder mixing to hard-pressed bale preliminary roller, add γ-ammonia
Propyl-triethoxysilicane and hydroxy silicon oil, mixing 40-60 minute；
2. the aluminium nitride adding the nanometer silver modification obtained by step (2), afterwards continues mixing 20-30 minute, and discharging is cooled to
Room temperature, stands 20-24 hour, obtains heat-conducting silicon rubber elastomeric compound；
(4) by the elastomeric compound obtained by step (3) on twin shaft mixing roll thin logical 4-6 time, thin logical during add double-2,5 sulfur
Agent, after thin pass-out sheet, at 160-190 DEG C, hot press moulding vulcanizes 10-30 minute, obtains the sheet silicon glue material of forming；
(5) by sheet silicon glue material post-cure 3-5 hour at 190-220 DEG C of the forming obtained by step (4), obtain
A kind of heat conductive rubber thermal interfacial material of ethylene propylene diene rubber-silicone rubber.
3. according to the heat conductive rubber thermal interfacial material of a kind of ethylene propylene diene rubber-silicone rubber described in claims 2
Preparation method, it is characterised in that in described step (1), the concentration of aqueous dopamine solution is 1.5-2.5g/L.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108219299A (en) * | 2018-02-05 | 2018-06-29 | 哈尔滨理工大学 | A kind of preparation method of ethylene-propylene-diene monomer matrix cable accessory material and its ethylene-propylene-diene monomer matrix cable accessory material |
| CN108968703A (en) * | 2017-06-01 | 2018-12-11 | 佛山市顺德区美的电热电器制造有限公司 | Pot and cooking apparatus in ceramic inserts metal |
| CN110467779A (en) * | 2019-07-25 | 2019-11-19 | 安徽电缆股份有限公司 | A kind of harsh cable high-performance synthetic rubber of three generations's nuclear power station and preparation method thereof |
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| CN101284925A (en) * | 2008-05-23 | 2008-10-15 | 山东大学 | Silastic/EPD combined heat-conducting rubber and method for preparing same |
| CN105112894A (en) * | 2015-08-31 | 2015-12-02 | 华南理工大学 | Method for conducting surface chemical copper plating on inorganic particles through dopamine |
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2016
- 2016-08-19 CN CN201610686066.XA patent/CN106317652A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101284925A (en) * | 2008-05-23 | 2008-10-15 | 山东大学 | Silastic/EPD combined heat-conducting rubber and method for preparing same |
| CN105112894A (en) * | 2015-08-31 | 2015-12-02 | 华南理工大学 | Method for conducting surface chemical copper plating on inorganic particles through dopamine |
Non-Patent Citations (1)
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| 周文英等: "《导热高分子材料》", 30 April 2014, 国防工业出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108968703A (en) * | 2017-06-01 | 2018-12-11 | 佛山市顺德区美的电热电器制造有限公司 | Pot and cooking apparatus in ceramic inserts metal |
| CN108219299A (en) * | 2018-02-05 | 2018-06-29 | 哈尔滨理工大学 | A kind of preparation method of ethylene-propylene-diene monomer matrix cable accessory material and its ethylene-propylene-diene monomer matrix cable accessory material |
| CN110467779A (en) * | 2019-07-25 | 2019-11-19 | 安徽电缆股份有限公司 | A kind of harsh cable high-performance synthetic rubber of three generations's nuclear power station and preparation method thereof |
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Application publication date: 20170111 |