CN106243727A - A kind of LED is acidified carbon nano tube modified high thermal conductive silicon rubber thermal interfacial material and preparation method - Google Patents
A kind of LED is acidified carbon nano tube modified high thermal conductive silicon rubber thermal interfacial material and preparation method Download PDFInfo
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- CN106243727A CN106243727A CN201610686053.2A CN201610686053A CN106243727A CN 106243727 A CN106243727 A CN 106243727A CN 201610686053 A CN201610686053 A CN 201610686053A CN 106243727 A CN106243727 A CN 106243727A
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Abstract
The present invention discloses the high thermal conductive silicon rubber thermal interfacial material that a kind of LED acidifying is carbon nano tube modified, is made up of the raw material of following weight portion: silicone rubber matrix 45 65 parts, aluminium nitride 22 32 parts, dopamine 15 25 parts, the silver nitrate solution of 20mmol/L 22 34 parts, hydroxy silicon oil 13 parts, double 2,5 vulcanizing agents 24 parts, deionized water is appropriate, and Tris HCl buffer solution is appropriate, CNT 16 22 parts, Graphene 10 15 parts, sulphuric acid/nitric acid mixed solution is appropriate.The present invention uses dopamine to form the poly-DOPA amine layer of close attachment in aln surface oxidation polymerization, simultaneously at the poly-DOPA amine layer area load Nano silver grain of cladding aluminium nitride, compounding filled silicon rubber, improve the high heat conduction and heat radiation performance of silicon rubber thermal interface material, there is good compliance, tearing strength and electrical insulation capability simultaneously.
Description
Technical field
The invention belongs to thermal interfacial material field, be specifically related to the high thermal conductive silicon that a kind of LED acidifying is carbon nano tube modified
Rubber 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 hot interface of high thermal conductive silicon rubber that a kind of LED acidifying is carbon nano tube modified
Material and preparation method.
The high thermal conductive silicon rubber thermal interfacial material that a kind of LED acidifying is carbon nano tube modified, by the raw material of following weight portion
Composition: silicone rubber matrix 45-65 part, aluminium nitride 22-32 part, dopamine 15-25 part, the silver nitrate solution 22-34 of 20mmol/L
Part, hydroxy silicon oil 1-3 part, double-2,5 vulcanizing agent 2-4 parts, deionized water is appropriate, and Tris-HCl buffer solution is appropriate, CNT
16-22 part, Graphene 10-15 part, sulphuric acid/nitric acid mixed solution 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) select caliber be 20-100nm, the CNT of a length of 10-50um in sulphuric acid/nitric acid mixed solution, carry out acid
Change processes and obtains acidifying CNT, stand-by；
(4) refining glue:
1., the aluminium nitride that the nanometer silver obtained by step (2) is modified is joined in silicone rubber matrix, and adds hydroxy silicon oil,
Mixing 30-40 minute is mediated in vacuum kneader；
2. add acidifying CNT that step (3) obtains, afterwards, Graphene continues mixing 20-40 minute, and the room of being cooled to stands
20-24 hour, obtain 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
The high thermal conductive silicon rubber thermal interfacial material that a kind of LED acidifying is carbon nano tube modified.
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) CNT after the present invention uses acidification is wrapped in graphene film interlayer, enhances structural stability,
Give its good pliability, improve material compactness, reduce interface contact heat resistance, there is high thermal conductivity.
Detailed description of the invention
The high thermal conductive silicon rubber thermal interfacial material that a kind of LED acidifying is carbon nano tube modified, by following weight portion (kilogram)
Raw material composition: silicone rubber matrix 60, aluminium nitride 28, dopamine 19, 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, CNT 20, Graphene 13, sulphuric acid/nitric acid
Mixed solution is appropriate.
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) select caliber be 20-100nm, the CNT of a length of 10-50um in sulphuric acid/nitric acid mixed solution, carry out acid
Change processes and obtains acidifying CNT, stand-by；
(4) refining glue:
1., the aluminium nitride that the nanometer silver obtained by step (2) is modified is joined in silicone rubber matrix, and adds hydroxy silicon oil,
Mixing 30-40 minute is mediated in vacuum kneader；
2. add acidifying CNT that step (3) obtains, afterwards, Graphene continues mixing 20-40 minute, and the room of being cooled to stands
20-24 hour, obtain 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
The high thermal conductive silicon rubber thermal interfacial material that a kind of LED acidifying is carbon nano tube modified.
Wherein, in step (1), the concentration of aqueous dopamine solution is 2g/L.
Test its performance data as follows: hardness 49shore A；Tearing strength 5.4kN/m；Heat conductivity 6.2W/ (m K)；
Specific insulation > 1013Ω·cm。
Claims (3)
1. the high thermal conductive silicon rubber thermal interfacial material that a LED acidifying is carbon nano tube modified, it is characterised in that by following weight
The raw material composition of part: silicone rubber matrix 45-65 part, aluminium nitride 22-32 part, dopamine 15-25 part, the silver nitrate of 20mmol/L is molten
Liquid 22-34 part, hydroxy silicon oil 1-3 part, double-2,5 vulcanizing agent 2-4 parts, deionized water is appropriate, and Tris-HCl buffer solution is appropriate,
CNT 16-22 part, Graphene 10-15 part, sulphuric acid/nitric acid mixed solution is appropriate.
2. it is acidified carbon nano tube modified high thermal conductive silicon rubber thermal interfacial material according to a kind of LED 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) select caliber be 20-100nm, the CNT of a length of 10-50um in sulphuric acid/nitric acid mixed solution, carry out acid
Change processes and obtains acidifying CNT, stand-by；
(4) refining glue:
1., the aluminium nitride that the nanometer silver obtained by step (2) is modified is joined in silicone rubber matrix, and adds hydroxy silicon oil,
Mixing 30-40 minute is mediated in vacuum kneader；
2. add acidifying CNT that step (3) obtains, afterwards, Graphene continues mixing 20-40 minute, and the room of being cooled to stands
20-24 hour, obtain 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
The high thermal conductive silicon rubber thermal interfacial material that a kind of LED acidifying is carbon nano tube modified.
3. it is acidified carbon nano tube modified high thermal conductive silicon rubber thermal interfacial material according to a kind of LED 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 |
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| CN107492664A (en) * | 2017-07-14 | 2017-12-19 | 中国第汽车股份有限公司 | Electrodes of lithium-ion batteries coating with heat sinking function |
| CN108051520A (en) * | 2017-12-15 | 2018-05-18 | 云南健牛生物科技有限公司 | A kind of method of aflatoxin B1 in detection tealeaves |
| CN110686589A (en) * | 2019-10-18 | 2020-01-14 | 南京理工大学 | High-sensitivity large-strain flexible strain sensor and preparation method thereof |
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| 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 (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107492664A (en) * | 2017-07-14 | 2017-12-19 | 中国第汽车股份有限公司 | Electrodes of lithium-ion batteries coating with heat sinking function |
| CN108051520A (en) * | 2017-12-15 | 2018-05-18 | 云南健牛生物科技有限公司 | A kind of method of aflatoxin B1 in detection tealeaves |
| CN110686589A (en) * | 2019-10-18 | 2020-01-14 | 南京理工大学 | High-sensitivity large-strain flexible strain sensor and preparation method thereof |
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Application publication date: 20161221 |