CN106280468A - A kind of LED porous carbon microsphere/paraffin composite heat-conducting silicon rubber thermal interface material and preparation method - Google Patents

A kind of LED porous carbon microsphere/paraffin composite heat-conducting silicon rubber thermal interface material and preparation method Download PDF

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CN106280468A
CN106280468A CN201610684315.1A CN201610684315A CN106280468A CN 106280468 A CN106280468 A CN 106280468A CN 201610684315 A CN201610684315 A CN 201610684315A CN 106280468 A CN106280468 A CN 106280468A
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aluminium nitride
porous carbon
parts
silicon rubber
carbon microsphere
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夏云
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ANHUI HEHAN OPTOELECTRONICS TECHNOLOGY Co Ltd
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ANHUI HEHAN OPTOELECTRONICS TECHNOLOGY Co Ltd
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08L83/00Compositions 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
    • C08L83/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
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    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08Materials not undergoing a change of physical state when used
    • C09K5/14Solid materials, e.g. powdery or granular
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

Abstract

The open a kind of LED porous carbon microsphere/paraffin composite heat-conducting silicon rubber thermal interface material of the present invention, is made up of the raw material of following weight portion: silicone rubber matrix 45 65 parts, aluminium nitride 18 26 parts, dopamine 15 25 parts, the silver nitrate solution of 20mmol/L 22 32 parts, hydroxy silicon oil 1.5 3 parts, double 2,5 vulcanizing agents 24 parts, deionized water is appropriate, and Tris HCl buffer solution is appropriate, 0.2mol/L glucose solution 20 30 parts, acetone in proper, 36 parts of paraffin.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

A kind of LED porous carbon microsphere/paraffin composite heat-conducting silicon rubber thermal interface material and Preparation method
Technical field
The invention belongs to thermal interfacial material field, be specifically related to a kind of LED porous carbon microsphere/paraffin composite heat-conducting silicon 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 a kind of LED porous carbon microsphere/paraffin composite heat-conducting silicone rubber hot interface material Material and preparation method.
A kind of LED porous carbon microsphere/paraffin composite heat-conducting silicon rubber thermal interface material, by the raw material group of following weight portion Become: silicone rubber matrix 45-65 part, aluminium nitride 18-26 part, dopamine 15-25 part, silver nitrate solution 22-32 part of 20mmol/L, Hydroxy silicon oil 1.5-3 part, double-2,5 vulcanizing agent 2-4 parts, deionized water is appropriate, and Tris-HCl buffer solution is appropriate, 0.2mol/L Glucose solution 20-30 part, acetone in proper, paraffin 3-6 part.
Specifically comprise the following steps that
(1) preparation of porous carbon microsphere:
Take 0.2mol/L glucose solution, be placed in 100mL water heating kettle, after reacting 10-13 hour at 170-190 DEG C, cooling To room temperature, obtain dark brown suspension, after centrifugation successively with acetone, deionized water respectively product is carried out " ultrasonic-from The heart-separation " clean 3 times, after then product being dried 24 hours, in tube type resistance furnace make annealing treatment 20-40 minute (800 DEG C, Argon flow amount 300mL/min), i.e. obtain porous carbon microsphere;
(2) 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;
(3) 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;
(4) aluminium nitride that the nanometer silver obtained by step (3) is modified is joined in silicone rubber matrix, and adds hydroxy silicon oil, Vacuum kneader is mediated mixing 30-40 minute, add step (1) afterwards and obtain porous carbon microsphere, the paraffin mixing 20-of continuation 40 minutes, after taking-up, room temperature was 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 porous carbon microsphere/paraffin composite heat-conducting silicon rubber thermal interface 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) porous carbon materials prepared by the present invention has good spherical morphology, abundant pore structure and big specific surface Long-pending, by paraffin is carried out physical absorption, it is prepared for porous graphite carbon microspheres/paraffin composite heat interfacial material, it has relatively High thermal conductivity, heat conduction and heat radiation excellent performance.
Detailed description of the invention
A kind of LED porous carbon microsphere/paraffin composite heat-conducting silicon rubber thermal interface material, by following weight portion (kilogram) Raw material forms: silicone rubber matrix 60, aluminium nitride 24, dopamine 22, 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, 0.2mol/L glucose solution 26, acetone in proper, stone Wax 5.
Specifically comprise the following steps that
(1) preparation of porous carbon microsphere:
Take 0.2mol/L glucose solution, be placed in 100mL water heating kettle, after reacting 11 hours at 180 DEG C, be cooled to room temperature, Obtain dark brown suspension, after centrifugation, with acetone, deionized water, respectively product is carried out " ultrasonic-centrifugal-to separate " successively Clean 3 times, after then product being dried 24 hours, in tube type resistance furnace make annealing treatment 30 minutes (800 DEG C, argon flow amount 300mL/min), porous carbon microsphere is i.e. obtained;
(2) 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;
(3) 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;
(4) aluminium nitride that the nanometer silver obtained by step (3) is modified is joined in silicone rubber matrix, and adds hydroxy silicon oil, Vacuum kneader is mediated mixing 35 minutes, add step (1) afterwards and obtain porous carbon microsphere, mixing 30 points of paraffin continuation Clock, 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 porous carbon microsphere/paraffin composite heat-conducting silicon rubber thermal interface material.
Wherein, in step (1), the concentration of aqueous dopamine solution is 2g/L.
Test its performance data as follows: hardness 46shore A;Tearing strength 5.3kN/m;Heat conductivity 6.4W/ (m K); Specific insulation > 1013Ω·cm。

Claims (3)

1. LED porous carbon microsphere/paraffin composite heat-conducting silicon rubber thermal interface material, it is characterised in that by following weight The raw material composition of part: silicone rubber matrix 45-65 part, aluminium nitride 18-26 part, dopamine 15-25 part, the silver nitrate of 20mmol/L is molten Liquid 22-32 part, hydroxy silicon oil 1.5-3 part, double-2,5 vulcanizing agent 2-4 parts, deionized water is appropriate, and Tris-HCl buffer solution is fitted Amount, 0.2mol/L glucose solution 20-30 part, acetone in proper, paraffin 3-6 part.
2. according to a kind of LED porous carbon microsphere/paraffin composite heat-conducting silicon rubber thermal interface material described in claims 1 Preparation method, it is characterised in that specifically comprise the following steps that
(1) preparation of porous carbon microsphere:
Take 0.2mol/L glucose solution, be placed in 100mL water heating kettle, after reacting 10-13 hour at 170-190 DEG C, cooling To room temperature, obtain dark brown suspension, after centrifugation successively with acetone, deionized water respectively product is carried out " ultrasonic-from The heart-separation " clean 3 times, after then product being dried 24 hours, in tube type resistance furnace make annealing treatment 20-40 minute (800 DEG C, Argon flow amount 300mL/min), i.e. obtain porous carbon microsphere;
(2) 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;
(3) 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;
(4) aluminium nitride that the nanometer silver obtained by step (3) is modified is joined in silicone rubber matrix, and adds hydroxy silicon oil, Vacuum kneader is mediated mixing 30-40 minute, add step (1) afterwards and obtain porous carbon microsphere, the paraffin mixing 20-of continuation 40 minutes, after taking-up, room temperature was 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 porous carbon microsphere/paraffin composite heat-conducting silicon rubber thermal interface material.
3. according to a kind of LED porous carbon microsphere/paraffin composite heat-conducting silicon rubber thermal interface material 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.
CN201610684315.1A 2016-08-18 2016-08-18 A kind of LED porous carbon microsphere/paraffin composite heat-conducting silicon rubber thermal interface material and preparation method Pending CN106280468A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109913183A (en) * 2019-04-12 2019-06-21 哈尔滨理工大学 A kind of insulating heat-conductive preparation of sections method with phase-change characteristic
CN114196208A (en) * 2021-12-21 2022-03-18 武汉誉辰电子科技有限公司 Manufacturing process of high-toughness heat-conducting silica gel
CN114634675A (en) * 2022-03-24 2022-06-17 西北工业大学 Method for preparing heat-insulating material by using polydopamine-modified carbon nano tube
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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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)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109913183A (en) * 2019-04-12 2019-06-21 哈尔滨理工大学 A kind of insulating heat-conductive preparation of sections method with phase-change characteristic
CN114196208A (en) * 2021-12-21 2022-03-18 武汉誉辰电子科技有限公司 Manufacturing process of high-toughness heat-conducting silica gel
CN114634675A (en) * 2022-03-24 2022-06-17 西北工业大学 Method for preparing heat-insulating material by using polydopamine-modified carbon nano tube
CN114634675B (en) * 2022-03-24 2023-09-26 西北工业大学 Method for preparing heat insulation material by using polydopamine modified carbon nano tube
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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