CN106317887A - Polydopamine functionally modified high thermal conductive silicone rubber thermal interface material for LED and preparation method - Google Patents
Polydopamine functionally modified high thermal conductive silicone rubber thermal interface material for LED and preparation method Download PDFInfo
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- CN106317887A CN106317887A CN201610686070.6A CN201610686070A CN106317887A CN 106317887 A CN106317887 A CN 106317887A CN 201610686070 A CN201610686070 A CN 201610686070A CN 106317887 A CN106317887 A CN 106317887A
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- aluminium nitride
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
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Abstract
The invention discloses a polydopamine functionally modified high thermal conductive silicone rubber thermal interface material for an LED. The polydopamine functionally modified high thermal conductive silicone rubber thermal interface material comprises the following raw materials in parts by weight: 40 to 60 parts of silicone rubber matrixes, 20 to 30 parts of aluminium nitride, 15 to 25 parts of polydopamine, 20 to 35 parts of 20 mmol/L silver nitrate solution, 1 to 3 parts of hydroxyl silicone oil, 2 to 5 parts of a bis-2,5 vulcanizing agent, a suitable amount of deionized water and a suitable amount of Tris-HCl buffered solution. According to the polydopamine functionally modified high thermal conductive silicone rubber thermal interface material for the LED, the polydopamine is oxidized and polymerized on the surface of the aluminium nitride so as to form a closely attached polydopamine layer, and meanwhile, silver nano-particles are loaded on the surface of the polydopamine layer which coats the aluminium nitride, so that the aluminium nitride can be prevented from hydrolyzing effectively, and the excellent thermal conductivity of the aluminium nitride is guaranteed; the aluminium nitride and the silver nano-particles are compounded to fill the silicon rubber, so that high thermal conducting performance and radiating performance of the silicone rubber thermal interface material are improved; meanwhile, the polydopamine functionally modified high thermal conductive silicone rubber thermal interface material for the LED has high flexibility, tearing strength and electrical insulating property.
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 modifies with poly-Dopamine
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 a kind of LED hot interface of high thermal conductive silicon rubber that poly-Dopamine is modified
Material and preparation method.
The high thermal conductive silicon rubber thermal interfacial material that a kind of LED modifies with poly-Dopamine, by the raw material of following weight portion
Composition: silicone rubber matrix 40-60 part, aluminium nitride 20-30 part, dopamine 15-25 part, the silver nitrate solution 20-35 of 20mmol/L
Part, 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.
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) aluminium nitride that the nanometer silver obtained by step (2) is modified is joined in silicone rubber matrix, and adds hydroxy silicon oil,
Mediating in vacuum kneader mixing 30-40 minute, after taking-up, room temperature is placed 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
The heat-conducting silicon rubber thermal interfacial material that the poly-Dopamine of lamellar is 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.
Detailed description of the invention
The high thermal conductive silicon rubber thermal interfacial material that a kind of LED modifies with poly-Dopamine, by following weight portion (kilogram)
Raw material composition: silicone rubber matrix 55, aluminium nitride 25, dopamine 20, the silver nitrate solution 30 of 20mmol/L, hydroxy silicon oil 2,
Double-2,5 vulcanizing agents 3, deionized water is appropriate, and Tris-HCl buffer 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) aluminium nitride that the nanometer silver obtained by step (2) is modified is joined in silicone rubber matrix, and adds hydroxy silicon oil,
Mediating in vacuum kneader mixing 35 minutes, after taking-up, room temperature is placed 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), obtain lamellar and gather
The heat-conducting silicon rubber thermal interfacial material that Dopamine is modified.
Wherein, in step (1), the concentration of aqueous dopamine solution is 2g/L.
Test its performance data as follows: hardness 47shore A；Tearing strength 4.9kN/m；Heat conductivity 6.1W/ (m K)；
Specific insulation > 1013Ω·cm。
Claims (3)
1. the high thermal conductive silicon rubber thermal interfacial material that a LED modifies with poly-Dopamine, it is characterised in that by following weight
The raw material composition of part: silicone rubber matrix 40-60 part, aluminium nitride 20-30 part, dopamine 15-25 part, the silver nitrate of 20mmol/L is molten
Liquid 20-35 part, 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.
2. the high thermal conductive silicon rubber thermal interfacial material modified with poly-Dopamine 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) aluminium nitride that the nanometer silver obtained by step (2) is modified is joined in silicone rubber matrix, and adds hydroxy silicon oil,
Mediating in vacuum kneader mixing 30-40 minute, after taking-up, room temperature is placed 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
The high thermal conductive silicon rubber thermal interfacial material that the poly-Dopamine of lamellar is modified.
3. the high thermal conductive silicon rubber thermal interfacial material modified with poly-Dopamine 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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| Application Number | Priority Date | Filing Date | Title |
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| CN201610686070.6A CN106317887A (en) | 2016-08-19 | 2016-08-19 | Polydopamine functionally modified high thermal conductive silicone rubber thermal interface material for LED and preparation method |
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| CN201610686070.6A CN106317887A (en) | 2016-08-19 | 2016-08-19 | Polydopamine functionally modified high thermal conductive silicone rubber thermal interface material for LED and preparation method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107805179A (en) * | 2017-11-22 | 2018-03-16 | 中国工程物理研究院化工材料研究所 | Bionical face enhanced thermal conduction filler, preparation method and the application in PBX |
| WO2018161416A1 (en) | 2017-03-09 | 2018-09-13 | 宁波新瑞清科金属材料有限公司 | Liquid metal thermal interface material with melt-back property and preparation method thereof |
| CN109265762A (en) * | 2018-08-30 | 2019-01-25 | 北京石油化工学院 | A kind of core-shell structure silver-based heat-conductivity rubber composite material and preparation method thereof |
| CN110845282A (en) * | 2019-11-20 | 2020-02-28 | 中国工程物理研究院化工材料研究所 | Heat-conducting filler for directionally repairing structural defects, preparation method and composite energetic material |
| CN111138858A (en) * | 2019-12-31 | 2020-05-12 | 溧阳市天盛绝缘材料有限公司 | High-flame-retardant high-temperature-resistant magnetically-induced silicone rubber and preparation method thereof |
| CN114213850A (en) * | 2021-12-28 | 2022-03-22 | 江苏达胜高聚物股份有限公司 | High-thermal-conductivity silicone rubber cable material and preparation method and application thereof |
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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 (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018161416A1 (en) | 2017-03-09 | 2018-09-13 | 宁波新瑞清科金属材料有限公司 | Liquid metal thermal interface material with melt-back property and preparation method thereof |
| CN107805179A (en) * | 2017-11-22 | 2018-03-16 | 中国工程物理研究院化工材料研究所 | Bionical face enhanced thermal conduction filler, preparation method and the application in PBX |
| CN109265762A (en) * | 2018-08-30 | 2019-01-25 | 北京石油化工学院 | A kind of core-shell structure silver-based heat-conductivity rubber composite material and preparation method thereof |
| CN110845282A (en) * | 2019-11-20 | 2020-02-28 | 中国工程物理研究院化工材料研究所 | Heat-conducting filler for directionally repairing structural defects, preparation method and composite energetic material |
| CN111138858A (en) * | 2019-12-31 | 2020-05-12 | 溧阳市天盛绝缘材料有限公司 | High-flame-retardant high-temperature-resistant magnetically-induced silicone rubber and preparation method thereof |
| CN114213850A (en) * | 2021-12-28 | 2022-03-22 | 江苏达胜高聚物股份有限公司 | High-thermal-conductivity silicone rubber cable material and preparation method and application thereof |
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Application publication date: 20170111 |