CN102153955A - Preparation method of heat conduction paster adopting fiber glass mesh as supporting structure - Google Patents
Preparation method of heat conduction paster adopting fiber glass mesh as supporting structure Download PDFInfo
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- CN102153955A CN102153955A CN2010105624569A CN201010562456A CN102153955A CN 102153955 A CN102153955 A CN 102153955A CN 2010105624569 A CN2010105624569 A CN 2010105624569A CN 201010562456 A CN201010562456 A CN 201010562456A CN 102153955 A CN102153955 A CN 102153955A
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Abstract
The invention discloses a preparation method of heat conduction paster, adopting a fiber glass mesh as a supporting structure. The preparation method comprises the steps of dissolving and formulating silicon rubber into silicon rubber solution, and sequentially adding vulcanizer, heat conduction filler and a silane coupling agent to formulate size with medium viscosity and fine coating performance by ultrasonic dispersion and ball-milling uniform mixing; and uniformly coating the size on the pretreated glass fiber mesh and obtaining the heat conduction paster through solvent volatilization, drying, moulding curing and trimming. The heat conduction paster has a high heat conduction rate and a small thermal expansion coefficient, is high in heat stability and soft, meets the requirement on an insulating property, and is convenient to use and disassemble since the surface of the paster has certain viscosity that can be adjusted within a certain range.
Description
Technical field
The present invention relates to a kind of preparation method who uses glass fiber mesh as the heat conduction paster of supporting structure.
Background technology
Along with the development of microelectronics, electronic devices and components are towards miniaturization, and are integrated, the multifunction development, and microelectronics industry is facing to the puzzlement of heat radiation bottleneck problem, and temperature raises, and the electronic component function reduces, reliability decrease, the life-span obviously reduces.Particularly in the LED encapsulation, the heat radiation difficulty has hindered the raising of LED lighting power greatly.Traditional heat radiation approach mainly contains three kinds: air-cooled, recirculated water cooling and finned, be subjected to the little restriction of volume, what generally use in the electronic material encapsulation at present is to install the heat abstractor heat radiation additional, heat abstractor is generally good metallic copper of heat conductivility and metallic aluminium, the heat that heat generating components produces is transmitted to copper base or aluminium base heating panel, in time heat is shed by increasing the thermal transpiration area.
The widespread use in microelectronics industry of this radiating mode, heat radiation is prerequisite with thermal conduction, studies show that the good thermal conductivity of thermal component can not guarantee that heat in time sheds, this is because there is big thermal resistance in the part that connects between heat generating components and the thermal component.The surface seems that there is many convex-concaves position in slick interface, demonstrate its connection clearly at microscopically between two parts that seem to fit tightly and have the slit, the slit is occupied by air when causing linking together, the thermal resistance of air is very big, and occupy the air circulation extreme difference in slit, easily produce localized hyperthermia, this is unfavorable for heat radiation.For solving the bad problem of interface heat transfer, need use heat interfacial material (Thermal interface materials) at the interface of heat generating components and thermal component, traditional heat interfacial material has two kinds: (1) heat-conducting silicone grease, adding heat conductive filler in various organic greases makes, heat-conducting silicone grease is when temperature is low, mobile poor, along with temperature raises, heat-conducting silicone grease begins to flow, can be full of the slit between the interface, as sealant, the heat-conducting silicone grease thermal conductivity far can significantly strengthen heat radiation far above air.Heat-conducting silicone grease is in the electron trade widespread use, but heat-conducting silicone grease has significant disadvantages, and higher viscosity makes that heat-conducting silicone grease is difficult to evenly be coated between the interface, studies show that then role is limited very little for heat-conducting silicone grease, applies blocked up meeting and causes the encapsulation difficulty.Heat-conducting silicone grease temperature mobile the increasing that raise might produce electronic component and pollute, even can cause short circuit, and residual grease is easy-clear etc. not.(2) heat conduction joint sealant, adding heat conductive filler in the Resins, epoxy makes, overall package heat generating components and thermal component preferably, heat conductive filler plays the effect of thermal conduction path simultaneously, but the poor thermal conductivity of this joint sealant, and be subjected to the influence of variation of ambient temperature after solidifying, both taken off split, the forfeiture heat conduction condition.
Sheet material is than the easy processing of grease, and the thermally-conductive sheet that thermally-conductive silicone rubber or analogue are made is widely used in the various application.Thermally-conductive sheet is divided into two classes usually, the sheet material of the general purpose of selecting for easy processing intent and for bonding and soft sheet material that select.
Summary of the invention
The used heat conductive filler of the present invention is innovated on the basis of traditional heat conductive filler, has used aluminium sesquioxide micron particle commonly used, and the nano aluminum nitride of high heat conductance, particularly carbon copper-clad nano-complex particle use separately or mixing is used.For improving the dispersiveness of heat conductive filler in silicon rubber, the silicon rubber dissolving is mixed with silicone rubber solution, add vulcanizing agent, heat conductive filler, coupling agent utilizes ultrasonic dispersion that Nano filling is dispersed in the silicon rubber, further is uniformly dispersed with ball milled again.This blending means has remarkable advantages compared to traditional mechanical blending method, and the mechanical blending method can produce filling-material structure and destroy the fillers dispersed difficulty.Solvent for use of the present invention all can recycling, and is simple to operate, energy-conserving and environment-protective.Ultra-sonic dispersion has dispersion effect preferably to Nano filling, general 800W～1200W, and 20min～40min can reach the dispersion effect of homogeneous, obviously is better than the mechanical blending method, and ball milled further disperses filler, and fillers dispersed is uniform and stable.The use of high heat conductance filler has guaranteed the heat conductivility that paster is good, the solution method homodisperse filler, paster thermal conductivity uniformity, coating property is better, surfacing, stable performance.
A kind of glass fiber mesh that uses provided by the invention has the following steps as the preparation method of the heat conduction paster of supporting structure: silicon rubber is mixed with silicone rubber solution through dissolution with solvents; Add vulcanizing agent, heat conductive filler, coupling agent successively, through ultra-sonic dispersion, ball milling is even to fillers dispersed, obtain the silicon rubber slurry, be uniformly coated on through pretreated glass fibre the silicon rubber slurry online, be coated with the glass fiber mesh thorough drying of slurry, molded vulcanization moulding, deburring promptly obtain using the heat conduction paster of glass fiber mesh as supporting structure.
Above-mentioned silicon rubber is Shore A hardness less than the methyl vinyl silicone rubbers of 50 degree, and being mixed with silicon rubber through dissolution with solvents, to account for liquid quality fraction be 25%～40% silicone rubber solution, and described solvent is tetrahydrofuran (THF) or gasoline.Be accelerate dissolution speed, can suitably heat and cooperate stirring, but Heating temperature should be lower than 60 degrees centigrade, because tetrahydrofuran (THF), gasoline belong to inflammable and explosive substances.
Above-mentioned vulcanizing agent is two 2,5 vulcanizing agents, and consumption is 1.5%～4.0% of a silicon rubber weight.Suitably adjust according to curability and paster pliability.
Above-mentioned heat conductive filler is micron order aluminium sesquioxide particle, aluminum nitride nanometer particle or carbon copper-clad nanoparticle; Micron order aluminium sesquioxide particle, aluminum nitride nanometer particle or carbon copper-clad nanoparticle are used alone or as a mixture, and the total mass of heat conductive filler should be less than or equal to 30% of silicon rubber weight.
Above-mentioned coupling agent is silane resin acceptor kh-550, DOW CORNING Z-6020 or DOW CORNING Z-6040, and consumption is 0.5%～2% of a heat conductive filler gross weight.
Above-mentioned ultra-sonic dispersion time 20min～40min, power 800w～1200w; Rotational speed of ball-mill 100r/min, time ball milling 2h～24h.Fillers dispersed evenly gets final product.
It is dry that the glass fiber mesh of the intact slurry of above-mentioned coating is put into drying installation, eliminates solvent, 60 ℃ of drying temperatures, time of drying 8h.
Above-mentioned glass fiber mesh pretreatment process is that the vitriol oil or concentrated nitric acid or the two mixing acid soak glass fiber mesh 4h～24h.Look the coating performance choose reasonable.
Above-mentioned sulfide stress is 10MPa～20MPa, 160 ℃～190 ℃ of curing temperatures, time 8min～12min.
Beneficial effect of the present invention:
The heat conduction paster thin thickness that the present invention makes, there is the layer of glass net centre, plays the effect of enhance heat transfer, simultaneously as supporting structure, can prepare larger area heat conduction paster.By solution method, in conjunction with ultra-sonic dispersion and ball milling uniform filling is dispersed in the silicon rubber slurry, the control slurry concentration is uniformly coated on through etched glass fibre slurry online.Through forming more projection and groove above the etched glass fibre twine of strong acid, this structure makes the silicon rubber slurry to be coated in preferably on the glass fibre twine, and coating performance improves greatly.One of heat conductive filler of the present invention carbon copper-clad nano-complex particle is a kind of nanoparticle of novel structure, outer carbon is complete has wrapped inner layer metal copper, the high thermal conductivity that had both had copper nano-particle, outer carbon again can the limit copper nanoparticle thermal expansion, reduce the thermal expansion of paster.The theoretical thermal conductivity that studies show that carbon nanotube is 3000W/m.K, the thermal conductivity 320W/m.K of aluminium nitride, and the thermal conductivity of aluminium sesquioxide is 30W/m.K, as heat conductive filler, plays the effect of passage of heat in silicon rubber inside.Silicon rubber has excellent chemical stability among the present invention, and heat decomposition temperature is higher, and vulcanisation operation is simple, the heat conduction paster smooth surface of preparation has certain viscosity, can fit tightly between heat generating components and thermal component, thin thickness, matter is soft, and there is glass fiber mesh inside as supporting structure, dismantles simple noresidue and pollutes, thermal expansivity is lower, be in same rank with metallic aluminium, in heat transfer process, can cooperate preferably, prevent that thermal expansion from producing distortion and new slit.DSC-TGA test shows heat conduction paster can be at 180 ℃ of following life-time service.
Embodiment
The following examples just are used for describing in detail superiority of the present invention, and the manufacturing and the application of heat conduction paster material of the present invention are not limited to this.
Embodiment 1
(1) 30g silicon rubber is dissolved in the 90g tetrahydrofuran (THF), is mixed with 25% silicone rubber solution, adds two 2, the 5 silicon rubber vulcanization agent of 1.0g, stirs.
(2) in step (1), add 4g micron order aluminium sesquioxide, 2g nanometer AlN heat conductive filler, add the 0.015g silane resin acceptor kh-550.
(3) mixed solution ultra-sonic dispersion 20min in the step (2), power 800W.
(4) mixed solution is put into ball grinder ball milling 24h in the step (3), obtains the finely dispersed silicon rubber slurry of heat conductive filler.
(5) soak glass fiber mesh 4h with the vitriol oil, obtain pretreated glass fiber mesh.
(6) slurry that obtains of step (4) is uniformly coated on step (5) through pretreated glass fiber mesh.
(7) glass fibre that is coated with silicon rubber that obtains of step (6) is put into the vacuum drying oven oven dry, 60 ℃ of drying temperatures, time of drying 8h.
(8) do not vulcanize paster in the step (7) and vulcanize on vulcanizing press, sulfide stress is 20MPa, 190 ℃ of curing temperatures, and time 8min, product promptly gets the heat conduction paster through deburring.
Embodiment 2
(1) 30g silicon rubber is dissolved in the 70g tetrahydrofuran (THF), is mixed with 30% silicone rubber solution, adds two 2, the 5 silicon rubber vulcanization agent of 0.6g, stirs.
(2) in step (1), add 6g carbon copper-clad nanoparticle heat conductive filler, add 0.06g silane coupling agent DOW CORNING Z-6020.
(3) mixed solution ultra-sonic dispersion 30min in the step (2), power 1200W.
(4) mixed solution is put into ball grinder ball milling 2h in the step (3), obtains the finely dispersed silicon rubber slurry of heat conductive filler.
(5) soak glass fiber mesh 24h with the vitriol oil, obtain pretreated glass fiber mesh.
(6) slurry that obtains of step (4) is uniformly coated on step (5) through pretreated glass fiber mesh.
(7) glass fibre that is coated with silicon rubber that obtains of step (6) is put into the vacuum drying oven oven dry, 60 ℃ of temperature, time of drying 8h.
(8) do not vulcanize paster in the step (7) and vulcanize on vulcanizing press, sulfide stress is 14MPa, 160 ℃ of curing temperatures, and time 10min, product promptly gets the heat conduction paster through deburring.
Embodiment 3
(1) 30g silicon rubber is dissolved in the 45g tetrahydrofuran (THF), is mixed with 40% silicone rubber solution, adds two 2, the 5 silicon rubber vulcanization agent of 0.45g, stirs.
(2) in step (1), add 9g nanometer AlN particle heat conductive filler, add 0.045g silane coupling agent DOW CORNING Z-6040.
(3) mixed solution ultra-sonic dispersion 40min in the step (2), power 1200W.
(4) mixed solution is put into ball grinder ball milling 24h in the step (3), obtains the finely dispersed silicon rubber slurry of heat conductive filler.
(5) soak glass fiber mesh 20h with the vitriol oil and concentrated nitric acid mixed strong acids, obtain pretreated glass fiber mesh.
(6) slurry that obtains of step (4) is uniformly coated on step (5) through pretreated glass fiber mesh.
(7) glass fibre that is coated with silicon rubber that obtains of step (6) is put into vacuum drying oven oven dry, 60 degrees centigrade of temperature, 8h.
(8) do not vulcanize paster in the step (7) and vulcanize on vulcanizing press, sulfide stress is 10MPa, 180 ℃ of curing temperatures, and time 9min, product promptly gets the heat conduction paster through deburring.
Embodiment 4
(1) 30g silicon rubber is dissolved in 70g gasoline, is mixed with 30% silicone rubber solution, adds two 2, the 5 silicon rubber vulcanization agent of 0.6g, stirs.
(2) adding 1.5g nano aluminum nitride and 4.5g micron order aluminium sesquioxide are led particle in step (1), and the hot filler of 1.5g carbon copper-clad nanoparticle adds the 0.15g silane resin acceptor kh-550.
(3) mixed solution ultra-sonic dispersion 30min in the step (2), power 1000W.
(4) mixed solution is put into ball grinder ball milling 20h in the step (3), obtains the finely dispersed silicon rubber slurry of heat conductive filler.
(5) soak glass fiber mesh 14h with the vitriol oil, obtain pretreated glass fiber mesh.
(6) slurry that obtains of step (4) is uniformly coated on step (5) through pretreated glass fiber mesh.
(7) glass fibre that is coated with silicon rubber that obtains of step (6) is put into the vacuum drying oven oven dry, 60 ℃ of drying temperatures, time of drying 8h.
(8) do not vulcanize paster in the step (7) and vulcanize on vulcanizing press, sulfide stress is 12MPa, 170 ℃ of curing temperatures, and time 8min, product promptly gets the heat conduction paster through deburring.
Embodiment 5
(1) 30g silicon rubber is dissolved in the 70g gasoline, is mixed with 30% silicone rubber solution, adds two 2, the 5 silicon rubber vulcanization agent of 1.2g, stirs.
(2) in step (1), add 4.5g carbon copper-clad nanoparticle and 4.5g micron order aluminium sesquioxide particle heat conductive filler, add the 0.1g coupling agent but healthy and free from worry Z-6040.
(3) mixed solution ultra-sonic dispersion 40min in the step (2), power 800W.
(4) mixed solution is put into ball grinder ball milling 4h in the step (3), obtains the finely dispersed silicon rubber slurry of heat conductive filler.
(5) soak glass fiber mesh 10h with concentrated nitric acid, obtain pretreated glass fiber mesh.
(6) slurry that obtains of step (4) is uniformly coated on step (5) through pretreated glass fiber mesh.
(7) glass fibre that is coated with silicon rubber that obtains of step (6) is put into the vacuum drying oven oven dry, 60 ℃ of drying temperatures, time of drying 8h.
(8) do not vulcanize paster in the step (7) and vulcanize on vulcanizing press, sulfide stress is 20MPa, 160 ℃ of curing temperatures, and time 12min, product promptly gets the heat conduction paster through deburring.
Claims (9)
1. a preparation method who uses glass fiber mesh as the heat conduction paster of supporting structure is characterized in that this method has the following steps: silicon rubber is mixed with silicone rubber solution through dissolution with solvents; Add vulcanizing agent, heat conductive filler, coupling agent successively, through ultra-sonic dispersion, ball milling is even to fillers dispersed, obtain the silicon rubber slurry, be uniformly coated on through pretreated glass fibre the silicon rubber slurry online, be coated with the glass fiber mesh thorough drying of slurry, molded vulcanization moulding, deburring promptly obtain using the heat conduction paster of glass fiber mesh as supporting structure.
2. preparation method according to claim 1, it is characterized in that: above-mentioned silicon rubber is the methyl vinyl silicone rubber of Shore A hardness less than 50 degree, being mixed with silicon rubber through dissolution with solvents, to account for liquid quality fraction be 25%～40% silicone rubber solution, and described solvent is tetrahydrofuran (THF) or gasoline.
3. preparation method according to claim 1 is characterized in that: above-mentioned vulcanizing agent is two 2,5 vulcanizing agents, and consumption is 1.5%～4.0% of a silicon rubber weight.
4. preparation method according to claim 1 is characterized in that: above-mentioned heat conductive filler is micron order aluminium sesquioxide particle, aluminum nitride nanometer particle or carbon copper-clad nanoparticle; Micron order aluminium sesquioxide particle, aluminum nitride nanometer particle or carbon copper-clad nanoparticle are used alone or as a mixture, and the total mass of heat conductive filler should be less than or equal to 30% of silicon rubber weight.
5. preparation method according to claim 1 is characterized in that: above-mentioned coupling agent is silane resin acceptor kh-550, DOW CORNING Z-6020 or DOW CORNING Z-6040, and consumption is 0.5%～2% of a heat conductive filler gross weight.
6. preparation method according to claim 1 is characterized in that: above-mentioned ultra-sonic dispersion time 20min～40min, power 800w～1200w; Rotational speed of ball-mill 100r/min, time ball milling 2h～24h.
7. preparation method according to claim 1 is characterized in that: it is dry that the glass fiber mesh of the intact slurry of above-mentioned coating is put into drying installation, eliminates solvent, 60 ℃ of drying temperatures, time of drying 8h.
8. preparation method according to claim 1 is characterized in that: above-mentioned glass fiber mesh pretreatment process is that the vitriol oil or concentrated nitric acid or the two mixing acid soak glass fiber mesh 4h～24h.
9. preparation method according to claim 1 is characterized in that: above-mentioned sulfide stress is 10MPa～20MPa, 160 ℃～190 ℃ of curing temperatures, time 8min～12min.
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Cited By (10)
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| CN106415883A (en) * | 2014-06-12 | 2017-02-15 | 戴姆勒股份公司 | Separator for an electrochemical store, method for producing electrode materials, and electrochemical energy store |
| CN106956447A (en) * | 2016-01-11 | 2017-07-18 | 湖北航天化学技术研究所 | A kind of slim silicon rubber-fabric joint product and its molding sulfidization molding technique |
| CN107079753A (en) * | 2017-04-27 | 2017-08-22 | 江苏华昌织物有限公司 | A kind of fly net for changing shape of a mesh with gradient of temperature |
| CN108178929A (en) * | 2018-01-24 | 2018-06-19 | 无锡市辉英电力电子有限公司 | A kind of insulation silica gel material and new energy car battery heating plate silica gel cloth |
| FR3060601A1 (en) * | 2016-12-20 | 2018-06-22 | Commissariat A L'energie Atomique Et Aux Energies Alternatives | ADHESIVE COMPOSITION AND ITS USE IN ELECTRONICS |
| CN108758389A (en) * | 2018-08-11 | 2018-11-06 | 宁波赛福实验仪器有限公司 | One plant growth illumination module |
| CN110349926A (en) * | 2019-07-18 | 2019-10-18 | 深圳前海量子翼纳米碳科技有限公司 | A method of reducing liquid metal for conducting heat piece thermal resistance |
| CN111073532A (en) * | 2019-12-04 | 2020-04-28 | 江阴天广科技有限公司 | Anti-corrosion wrapping belt |
| CN111732931A (en) * | 2020-06-29 | 2020-10-02 | 王朝鹏 | Heat-conducting adhesive silica gel |
| CN112852168A (en) * | 2021-01-14 | 2021-05-28 | 广东信力科技股份有限公司 | Preparation method of heat-conducting silicone rubber composite material suitable for rail transit |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106415883A (en) * | 2014-06-12 | 2017-02-15 | 戴姆勒股份公司 | Separator for an electrochemical store, method for producing electrode materials, and electrochemical energy store |
| US10290846B2 (en) | 2014-06-12 | 2019-05-14 | Daimler Ag | Separator for an electrochemical storage system, method for the production of an electrode material and electrochemical energy storage system |
| CN106956447A (en) * | 2016-01-11 | 2017-07-18 | 湖北航天化学技术研究所 | A kind of slim silicon rubber-fabric joint product and its molding sulfidization molding technique |
| CN106956447B (en) * | 2016-01-11 | 2019-03-22 | 湖北航天化学技术研究所 | A kind of slim silicon rubber-fabric joint product and its molding sulfidization molding technique |
| FR3060601A1 (en) * | 2016-12-20 | 2018-06-22 | Commissariat A L'energie Atomique Et Aux Energies Alternatives | ADHESIVE COMPOSITION AND ITS USE IN ELECTRONICS |
| EP3339392A1 (en) * | 2016-12-20 | 2018-06-27 | Commissariat à l'Energie Atomique et aux Energies Alternatives | Adhesive composition and use thereof in electronics |
| CN107079753A (en) * | 2017-04-27 | 2017-08-22 | 江苏华昌织物有限公司 | A kind of fly net for changing shape of a mesh with gradient of temperature |
| CN107079753B (en) * | 2017-04-27 | 2020-10-30 | 江苏华昌织物有限公司 | Insect-proof net with mesh shape changed along with temperature rise and fall |
| CN108178929A (en) * | 2018-01-24 | 2018-06-19 | 无锡市辉英电力电子有限公司 | A kind of insulation silica gel material and new energy car battery heating plate silica gel cloth |
| CN108758389A (en) * | 2018-08-11 | 2018-11-06 | 宁波赛福实验仪器有限公司 | One plant growth illumination module |
| CN108758389B (en) * | 2018-08-11 | 2024-04-12 | 宁波赛福实验仪器有限公司 | Plant growth illumination module |
| CN110349926A (en) * | 2019-07-18 | 2019-10-18 | 深圳前海量子翼纳米碳科技有限公司 | A method of reducing liquid metal for conducting heat piece thermal resistance |
| CN110349926B (en) * | 2019-07-18 | 2021-01-08 | 深圳前海量子翼纳米碳科技有限公司 | Method for reducing thermal resistance of liquid metal heat conducting fin |
| CN111073532A (en) * | 2019-12-04 | 2020-04-28 | 江阴天广科技有限公司 | Anti-corrosion wrapping belt |
| CN111732931A (en) * | 2020-06-29 | 2020-10-02 | 王朝鹏 | Heat-conducting adhesive silica gel |
| CN112852168A (en) * | 2021-01-14 | 2021-05-28 | 广东信力科技股份有限公司 | Preparation method of heat-conducting silicone rubber composite material suitable for rail transit |
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