CN106317880A - High-durability high-heat-conductivity silicone rubber thermal interface material for LED and preparation method - Google Patents
High-durability high-heat-conductivity silicone rubber thermal interface material for LED and preparation method Download PDFInfo
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Abstract
The invention discloses a high-durability high-heat-conductivity silicone rubber thermal interface material for an LED. The material is prepared from, by weight, 40-60 parts of silicone rubber matrix, 20-30 parts of aluminum nitride, 15-25 parts of dopamine, 20-35 parts of silver nitrate solution with concentration of 20 mmol/L, 1-3 parts of hydroxyl silicone oil, 2-5 parts of bis-2,5-vulcanizing agent, a proper amount of deionized water, a proper amount of Tris-HCl buffer solution, 3-5 parts of white carbon black, 2-4 parts of quartz powder, 0.5-1.5 parts of hexamethyl-disilazane and a proper amount of glycol. Dopamine is oxidized and polymerized on the surface of aluminum nitride to form a closely attached polydopamine layer, meanwhile silver nanoparticles are loaded on the surface of the polydopamine layer wrapping aluminum nitride and combined with filling silicone rubber, the high heat conductivity and cooling performance of the silicone rubber thermal interface material are improved, and the material has high smoothness, tear strength and electric insulating performance.
Description
Technical field
The invention belongs to thermal interfacial material field, be specifically related to a kind of hot interface of LED high-durability high thermal conductive silicon rubber
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 a kind of LED high-durability high thermal conductive silicon rubber thermal interfacial material and system
Preparation Method.
A kind of LED high-durability high thermal conductive silicon rubber thermal interfacial material, is made up of the raw material of following weight portion: silicone rubber
Matrix 40-60 part, aluminium nitride 20-30 part, dopamine 15-25 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, and Tris-HCl buffer solution is appropriate, white carbon 3-5 part, silica flour
2-4 part, hexamethyldisiloxane 0.5-1.5 part, ethylene glycol is appropriate.
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) hexamethyldisiloxane is joined in the ethylene glycol of 45-60 DEG C and make the solution that concentration is 10-15%, add afterwards
White carbon, after submergence completely, high speed dispersion stirs 20-40 minute, removes solvent, obtains surface-treated white carbon；
(4) aluminium nitride that the nanometer silver obtained by step (2) is modified is joined in silicone rubber matrix, and adds hydroxy silicon oil,
Vacuum kneader is mediated mixing 30-40 minute, add white carbon, silica flour that step (3) surface treated is crossed afterwards, continue
Mixing 20-40 minute of continuous kneading, after taking-up, room temperature is placed 20-24 hour, obtains heat-conducting silicon rubber elastomeric compound；
(5) by the elastomeric compound obtained by step (4) 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；
(6) by sheet silicon glue material post-cure 3-5 hour at 190-220 DEG C of the forming obtained by step (5), obtain
A kind of LED high-durability high thermal conductive silicon rubber thermal interfacial material.
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) present invention uses hexamethyldisiloxane process white carbon that its surface texture can be allowed farthest to uphold, with
Ensureing that its effective contact area is maximum, thermally conductive pathways is the shortest, reaches optimal heat-conducting effect, white carbon, silica flour and nanometer
The aluminium nitride mixing of modified by silver, not only obtains piling up closely knit heat carrier, and heat transfer contact area is also significantly increased, tool
Excellent heat conductivility.
Detailed description of the invention
A kind of LED high-durability high thermal conductive silicon rubber thermal interfacial material, is made up of the raw material of following weight portion (kilogram):
Silicone rubber matrix 55, aluminium nitride 25, dopamine 20, the silver nitrate solution 28 of 20mmol/L, hydroxy silicon oil 2, double-2,5 vulcanizing agents
3, deionized water is appropriate, and Tris-HCl buffer solution is appropriate, white carbon 4, silica flour 3, hexamethyldisiloxane 1, and ethylene glycol is fitted
Amount.
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) hexamethyldisiloxane is joined in the ethylene glycol of 50 DEG C and make the solution that concentration is 10%, add Linesless charcoal afterwards
Black, after submergence completely, high speed dispersion stirs 30 minutes, removes solvent, obtains surface-treated white carbon；
(4) aluminium nitride that the nanometer silver obtained by step (2) is modified is joined in silicone rubber matrix, and adds hydroxy silicon oil,
Vacuum kneader is mediated mixing 35 minutes, add white carbon, silica flour that step (3) surface treated is crossed afterwards, continue
Mediating mixing 30 minutes, after taking-up, room temperature is placed 24 hours, obtains heat-conducting silicon rubber elastomeric compound；
(5) by the elastomeric compound obtained by step (4) 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；
(6) by sheet silicon glue material post-cure 4 hours at 200 DEG C of the forming obtained by step (5), one is obtained
LED high-durability high thermal conductive silicon rubber thermal interfacial material.
Wherein, in step (1), the concentration of aqueous dopamine solution is 2g/L.
Test its performance data as follows: hardness 48shore A；Tearing strength 5.5kN/m；Heat conductivity 5.9W/ (m K)；
Specific insulation > 1013Ω·cm。
Claims (3)
1. a LED high-durability high thermal conductive silicon rubber thermal interfacial material, it is characterised in that by the raw material group of following weight portion
Become: silicone rubber matrix 40-60 part, aluminium nitride 20-30 part, dopamine 15-25 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, and Tris-HCl buffer solution is appropriate, white carbon 3-5
Part, silica flour 2-4 part, hexamethyldisiloxane 0.5-1.5 part, ethylene glycol is appropriate.
2. according to the preparation method of a kind of LED high-durability high thermal conductive silicon rubber thermal interfacial material described in claims 1,
It is characterized 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) hexamethyldisiloxane is joined in the ethylene glycol of 45-60 DEG C and make the solution that concentration is 10-15%, add afterwards
White carbon, after submergence completely, high speed dispersion stirs 20-40 minute, removes solvent, obtains surface-treated white carbon；
(4) aluminium nitride that the nanometer silver obtained by step (2) is modified is joined in silicone rubber matrix, and adds hydroxy silicon oil,
Vacuum kneader is mediated mixing 30-40 minute, add white carbon, silica flour that step (3) surface treated is crossed afterwards, continue
Mixing 20-40 minute of continuous kneading, after taking-up, room temperature is placed 20-24 hour, obtains heat-conducting silicon rubber elastomeric compound；
(5) by the elastomeric compound obtained by step (4) 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；
(6) by sheet silicon glue material post-cure 3-5 hour at 190-220 DEG C of the forming obtained by step (5), obtain
A kind of LED high-durability high thermal conductive silicon rubber thermal interfacial material.
3. according to the preparation method of a kind of LED high-durability high thermal conductive silicon rubber thermal interfacial material described in claims 2,
It is characterized in that, in described step (1), the concentration of aqueous dopamine solution is 1.5-2.5g/L.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107170508A (en) * | 2017-05-14 | 2017-09-15 | 常州市奥普泰克光电科技有限公司 | A kind of preparation method of conductive silver paste |
| CN107189495A (en) * | 2017-06-29 | 2017-09-22 | 铜陵市永创变压器电子有限公司 | A kind of dopamine coats nano-silicon dioxide modified conductive and heat-conductive glass fiber compound material and preparation method thereof |
| CN113698767A (en) * | 2021-09-06 | 2021-11-26 | 沅陵县成瑞祥粉体材料科技有限公司 | Novel high-performance silicon rubber for insulator and preparation method |
| CN117304575A (en) * | 2023-11-29 | 2023-12-29 | 瑞金市索梦得新材料科技有限公司 | Ti (titanium) 3 C 2 T x Preparation method and application of-Mxene@polydopamine-nano silver composite material |
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| CN102220006A (en) * | 2011-04-28 | 2011-10-19 | 天津大学 | Mixed filling type thermal conductive silicone rubber composite and preparation method thereof |
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2016
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| CN102220006A (en) * | 2011-04-28 | 2011-10-19 | 天津大学 | Mixed filling type thermal conductive silicone rubber composite and preparation method thereof |
| 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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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107170508A (en) * | 2017-05-14 | 2017-09-15 | 常州市奥普泰克光电科技有限公司 | A kind of preparation method of conductive silver paste |
| CN107170508B (en) * | 2017-05-14 | 2019-01-18 | 马鞍山市泰博化工科技有限公司 | A kind of preparation method of conductive silver paste |
| CN107189495A (en) * | 2017-06-29 | 2017-09-22 | 铜陵市永创变压器电子有限公司 | A kind of dopamine coats nano-silicon dioxide modified conductive and heat-conductive glass fiber compound material and preparation method thereof |
| CN113698767A (en) * | 2021-09-06 | 2021-11-26 | 沅陵县成瑞祥粉体材料科技有限公司 | Novel high-performance silicon rubber for insulator and preparation method |
| CN117304575A (en) * | 2023-11-29 | 2023-12-29 | 瑞金市索梦得新材料科技有限公司 | Ti (titanium) 3 C 2 T x Preparation method and application of-Mxene@polydopamine-nano silver composite material |
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Application publication date: 20170111 |