CN103436018A - High-toughness ultrathin heat-conducting silica gel gasket and preparation method thereof - Google Patents
High-toughness ultrathin heat-conducting silica gel gasket and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-toughness ultrathin heat-conducting silica gel gasket and a preparation method thereof. The high-toughness ultrathin heat-conducting silica gel gasket is prepared from the following raw materials in parts by weight: 5-30 parts of methylvinylsiloxane rubber, 10-50 parts of vinyl silicon oil, 10-100 parts of dimethyl silicon oil, 1-20 parts of MQ silicon resin, 300-1000 parts of modified aluminum oxide granule, 1-10 parts of silica gel reinforcing agent, 1-8 parts of hydrogen-containing silicon oil and 0.5-5 parts of catalyst. By using the organic silicon resin as a base material and aluminum oxide as a heat-conducting filling material, the improvement and treatment of the base and the treatment of the heat-conducting powder are performed to prepare the high-toughness heat-conducting silica gel with high heat conductivity coefficient. The heat-conducting silica gel gasket disclosed by the invention has the advantages of high mechanical properties, low thermal resistance and the like; and the preparation method can be used for preparing a heat-conducting silica gel of which the heat conductivity coefficient is 2.0W above, the thickness is 0.1mm and the tensile strength is 1.0Mpa.
Description
Technical field
The present invention relates to a kind of silica gel pad and preparation method thereof, be specifically related to ultra-thin heat conductive silica gel pad of a kind of high tenacity and preparation method thereof.
Background technology
Silicon rubber has high-low temperature resistant, high voltage withstanding, anti-ozone ageing, radiation resistance, highly air-permeable and lubricated wet goods media table is revealed to excellent unreactiveness.In addition, use temperature scope (50 ℃-250 ℃) broadness, it is good that performance is damaged in good springiness, anti creepage trace and galvanic corrosion, especially existing good hydrophobicity performance characteristics still after its surperficial contamination.Therefore, employing silicon rubber is heat conduction substrate, significant with the compound elastic heat conducting insulating material of making a kind of excellent properties of high heat conductive filler.
Heat conductive silica gel is as a kind of heat interfacial material, complete the heat transmission between heat generating components and scatterer position, the size of its thermal resistance is determining the effect that heat transmits, product thermal resistance relevant with its thickness to its thermal conductivity, under thermal conductivity is identical, the less thermal resistance of thickness is less.The inventor studies discovery, and the thermal resistance of thermal conductivity 4.0W1.5mm heat conductive silica gel is identical with the thermal resistance of thermal conductivity 1.0W0.3mm, and when being used in interface as heat conducting material, the heat transfer effect reached is identical.Current heat conductive silica gel pad on the market is the thinnest generally all more than 0.3mm, when thickness is less than 0.3mm, toughness and insufficient strength due to product, bring very large trouble to the operator, therefore in some specific occasion, reach reasonable radiating effect, must select high thermal conductive silicon glue product, increased cost.Therefore, to have the ultra-thin heat conductive silica gel pad of high tenacity be necessary in preparation.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide the ultra-thin heat conductive silica gel pad of a kind of high tenacity, by the improvement to the silicon rubber matrix with to the modification of powder body material, increase the intensity of silicon rubber matrix itself and the bonding force between silicon rubber matrix and powder, thereby reach the purpose of the intensity that improves the heat conductive silica gel pad.Heat conductive silica gel pad of the present invention has the advantages such as mechanical property is high, thermal resistance is low, and more than its thermal conductivity can reach 2.0W, thickness can be controlled in 0.1mm left and right, tensile strength 1.0MPa.
Another object of the present invention is to provide the preparation method of the ultra-thin heat conductive silica gel pad of a kind of high tenacity, to the improvement of silicon rubber matrix with to the modification of powder, realize improving the purpose of heat conductive silica gel gasket strength.
Realize that first purpose of the present invention can reach by taking following technical scheme:
The ultra-thin heat conductive silica gel pad of a kind of high tenacity is characterized in that being prepared from by following raw material by weight:
Methyl vinyl silicone rubber 5-30 part
Vinyl silicone oil 10-50 part
Dimethyl silicone oil 10-100 part
MQ silicone resin 1-20 part
Modified oxidized aluminum particulate 300-1000 part
Silica gel strengthening agent 1-10 part
Containing hydrogen silicone oil 1-8 part
Catalyzer 0.5-5 part.
In preferred scheme, the ultra-thin heat conductive silica gel pad of high tenacity of the present invention is prepared from by following raw material by weight:
15 parts of methyl vinyl silicone rubbers
25 parts of vinyl silicone oils
45 parts of dimethyl silicone oils
MQ silicone resin 1-20 part
Modified oxidized aluminum particulate 300-1000 part
Silica gel strengthening agent 1-10 part
Containing hydrogen silicone oil 1-8 part
Catalyzer 0.5-5 part.
The ultra-thin heat conductive silica gel pad of high tenacity of the present invention thermal conductivity will be more than 2.0W, and thickness 0.1mm, more than tensile strength 1.0MPa.
Prepared by the following method by modified oxidized aluminum particulate of the present invention: the anhydrous alcohol solution that is 95% by mass concentration by the silane coupling agent of 0.2-2 weight part is configured to the silane coupling agent alcoholic solution that mass concentration is 3%-10%, is stirred to coupling agent and all dissolves; The Spherical alumina particles of 400-700 parts by weight is joined in the silane coupling agent alcoholic solution, after stirring, dry, obtain modified oxidized aluminum particulate; After modification, the surfactivity of Spherical alumina particles increases, and is conducive to improve the bonding force of powder and silicon rubber matrix, thereby reaches the heat conduction function that improves the heat conductive silica gel pad.Described silane coupling agent is one or several in KH-550, KH-560, KH-570 and KH-580;
In the present invention; the Spherical alumina particles that the Spherical alumina particles of two kinds of different-grain diameters is mixed to also modification more is conducive to the formation of passage of heat with respect to the modified spherical alumina particle of single a kind of particle diameter; preferably; described modified oxidized aluminum particulate comprises the Spherical alumina particles of two kinds of particle diameters of 3-10 μ m and 20-60 μ m; their mass ratio is (2-5): (5-8), the speed and the quantity that form passage of heat are the most reasonable.
Vinyl silicone oil medium vinyl content is mainly hardness and the compression ratio of controlling finished product, contents of ethylene crosses that I haven't seen you for ages causes finished product hardness higher, reduce the snappiness of finished product, therefore, in order to obtain the ultra-thin heat conductive silica gel pad of high tenacity of the present invention, preferably, the 15-22% that described vinyl silicone oil medium vinyl content is the vinyl silicone oil gross weight.
Dimethyl-silicon oil viscosity too conference causes the viscosity of base-material excessive, after vulcanisation step, can cause the hardness of product excessive, can't obtain the ultra-thin heat conductive silica gel pad of high tenacity, and if the dimethyl-silicon oil viscosity is too little, be difficult to moulding in vulcanisation step, therefore, the dimethyl-silicon oil viscosity that adopted in the present invention is 100-500cps.
MQ silicone resin of the present invention is the thermoset polysiloxane polymer with highly cross-linked structure.Silicone resin molecule side group is mainly methyl, introduce phenyl and can improve thermo-elasticity and cementability, the compatibility of improvement and organic polymer and pigment, introduce the carbon functional group can with more organic compound reactions, improvement is cementability to base material, the molecular weight of silicone resin is decision self and the reacted thermo-elasticity of phenyl and close-burning key factor, therefore, obtain the ultra-thin heat conductive silica gel pad of high tenacity of the present invention, the molecular weight of preferred MQ silicone resin is 5-20 ten thousand, viscosity 4000-10000cpas.
In the present invention, the reinforcing property that there is height as the nano-scale white carbon black of silica gel strengthening agent.The nano-scale white carbon black of the 20-500um adopted in the present invention, can effectively improve tensile strength and the tensile yield of finished product, and the physical strength of its product and anti-tear index are significantly improved.
The contriver studies discovery, and in base-material, the hydrogen content of containing hydrogen silicone oil determines its adding proportion in base-material and follow-up vulcanization rate and the hardness of the finished product.The raising of hydrogen content, vulcanization rate is accelerated, and product hardness can increase, and the hydrogen content of the containing hydrogen silicone oil that the present invention adopts is the 1-3% that accounts for the containing hydrogen silicone oil gross weight, just can control the hardness of vulcanization rate and product in moderate scope.
In order to reduce curing temperature, obtain the ultra-thin heat conductive silica gel pad of high tenacity, the catalyzer adopted in the present invention is the platinum acid chloride solution that effective content is 0.1-0.5%.
The preparation method of the ultra-thin heat conductive silica gel pad of high tenacity of the present invention, it comprises the following steps in turn:
1) improvement of silicon rubber matrix and processing: vinyl silicone oil, dimethyl silicone oil, MQ silicone resin and silica gel toughener are uniformly mixed; colloid mixture called after modification after stirring strengthens silicone oil; methyl vinyl silicone rubber and modification are strengthened to silicone oil and add in mill and ground, obtain the silicon rubber matrix;
2) being uniformly mixed of silicon rubber matrix and alumina particle: modified oxidized aluminum particulate is joined in the silicon rubber matrix through improving and processing, after stirring, then add containing hydrogen silicone oil and catalyzer, high-speed stirring in homogenizer, stirring velocity is 1500-3000rpm, obtains base-material;
3) vacuumize: the base-material stirred is placed in vacuum machine and vacuumized, and the bubble that makes to be mixed in base-material is drawn out of fully;
4) sulfidization molding: by base-material coldmoulding, by cooling after hot-air vulcanization, obtain the ultra-thin heat conductive silica gel pad of high tenacity.
Preferably, in step 1), the stirring that makes modification enhancing silicone oil is stirred by high speed dispersor, and the temperature of stirring is 100-200 ℃, and stirring velocity is 1500-3000rpm, and churning time is 0.5-2h;
Preferably, in step 4), vulcanize as hot-air vulcanization, curing temperature is 100-180 ℃, and curing time is: 10-30min.
Beneficial effect of the present invention is:
The ultra-thin heat conductive silica gel pad of high tenacity of the present invention is by the improvement to the silicon rubber matrix with to the modification of powder body material, increase the intensity of silicon rubber matrix itself and the bonding force between silicon rubber matrix and powder, again by adding the silica gel strengthening agent to improve the tensile strength of finished product, thereby reach the purpose of the obdurability that improves the heat conductive silica gel pad.Heat conductive silica gel pad of the present invention has the advantages such as mechanical property is high, thermal resistance is low, and more than its thermal conductivity can reach 2.0W, thickness can be controlled in 0.1mm left and right, tensile strength 1.0MPa.
Embodiment
Below, in conjunction with embodiment, the present invention is described further:
Case study on implementation 1:
The ultra-thin heat conductive silica gel pad of a kind of high-strong toughness is prepared from according to following steps:
(1) improvement of silicon rubber matrix and processing: by the silica gel toughener mixing and stirring of the MQ silicone resin of the dimethyl silicone oil of the vinyl silicone oil of 20 weight parts, 30 weight parts, 5 weight parts and 3 weight parts, colloid mixture called after modification after stirring strengthens silicone oil, add mill to be ground the methyl vinyl silicone rubber of 10 weight parts and modification enhancing silicone oil, obtain the silicon rubber matrix.
(2) being uniformly mixed of silicon rubber matrix and alumina particle: the modified oxidized aluminum particulate that the ratio that is 3:5 according to mass ratio by the Spherical alumina particles of two kinds of particle diameters of 3-10 μ m and 20-60 μ m mixes joins in the silicon rubber matrix through improving and processing, after stirring in homogenizer, add again the containing hydrogen silicone oil of 2.5 weight parts and the catalyzer of 0.5 weight part, high-speed stirring, stirring velocity is 1500rpm, obtains base-material;
Wherein, being prepared as of modified oxidized aluminum particulate: the anhydrous alcohol solution that is 95% by mass concentration by the silane coupling agent of 0.2-2 weight part is configured to the silane coupling agent alcoholic solution that mass concentration is 3%-10%, is stirred to coupling agent and all dissolves; The Spherical alumina particles of 400 parts by weight is joined in the silane coupling agent alcoholic solution, after stirring, dry, obtain modified oxidized aluminum particulate;
(3) vacuumize: the base-material stirred is placed in vacuum machine and vacuumized, and the bubble that makes to be mixed in base-material is drawn out of fully;
(4) sulfidization molding: by base-material coldmoulding, cooling after the hot-air vulcanization 10-30min that is 100-180 ℃ by curing temperature, obtain the ultra-thin heat-conducting silica gel sheet of high-strong toughness.
Use standard ISO-22007-2 Hot Disk thermal constant analyser to be measured the heat conductive silica gel thermal conductivity, the thermal conductivity recorded is 2.26W, use standard P EACOCK thickness piece to be measured heat conductive silica gel thickness, the heat conductive silica gel thickness recorded is 0.18mm, use the standard tension trier to be measured the tensile strength of heat conductive silica gel, the heat conductive silica gel tensile strength recorded is 0.99MPa.
Case study on implementation 2:
The ultra-thin heat conductive silica gel pad of a kind of high-strong toughness is prepared from according to following steps:
(1) improvement of silicon rubber matrix and processing: by the silica gel toughener mixing and stirring of the MQ silicone resin of the dimethyl silicone oil of the vinyl silicone oil of 25 weight parts, 45 weight parts, 10 weight parts and 5 weight parts, colloid mixture called after modification after stirring strengthens silicone oil, add mill to be ground the methyl vinyl silicone rubber of 15 weight parts and modification enhancing silicone oil, obtain the silicon rubber matrix.
(2) being uniformly mixed of silicon rubber matrix and alumina particle: the modified oxidized aluminum particulate that the ratio that is 3:7 according to mass ratio by the Spherical alumina particles of two kinds of particle diameters of 3-10 μ m and 20-60 μ m mixes joins in the silicon rubber matrix through improving and processing, after stirring in homogenizer, add again the containing hydrogen silicone oil of 4 weight parts and the catalyzer of 2 weight parts, high-speed stirring, stirring velocity is 3000rpm, obtains base-material;
Wherein, being prepared as of modified oxidized aluminum particulate: the anhydrous alcohol solution that is 95% by mass concentration by the silane coupling agent of 0.2-2 weight part is configured to the silane coupling agent alcoholic solution that mass concentration is 3%-10%, is stirred to coupling agent and all dissolves; The Spherical alumina particles of 700 parts by weight is joined in the silane coupling agent alcoholic solution, after stirring, dry, obtain modified oxidized aluminum particulate;
(3) vacuumize: the base-material stirred is placed in vacuum machine and vacuumized, and the bubble that makes to be mixed in base-material is drawn out of fully;
(4) sulfidization molding: by base-material coldmoulding, cooling after the hot-air vulcanization 10-30min that is 100-180 ℃ by curing temperature, obtain the ultra-thin heat-conducting silica gel sheet of high-strong toughness.
Use standard ISO-22007-2 Hot Disk thermal constant analyser to be measured the heat conductive silica gel thermal conductivity, the thermal conductivity recorded is 2.5W, use standard P EACOCK thickness piece to be measured heat conductive silica gel thickness, the heat conductive silica gel thickness recorded is 0.11mm, use the standard tension trier to be measured the tensile strength of heat conductive silica gel, the heat conductive silica gel tensile strength recorded is 1.2MPa.
Case study on implementation 3:
The ultra-thin heat conductive silica gel pad of a kind of high-strong toughness is prepared from according to following steps:
(1) improvement of silicon rubber matrix and processing: by the silica gel toughener mixing and stirring of the MQ silicone resin of the dimethyl silicone oil of the vinyl silicone oil of 45 weight parts, 70 weight parts, 15 weight parts and 8 weight parts, colloid mixture called after modification after stirring strengthens silicone oil, add mill to be ground the methyl vinyl silicone rubber of 25 weight parts and modification enhancing silicone oil, obtain the silicon rubber matrix.
(2) being uniformly mixed of silicon rubber matrix and alumina particle: the modified oxidized aluminum particulate that the ratio that is 5:8 according to mass ratio by the Spherical alumina particles of two kinds of particle diameters of 3-10 μ m and 20-60 μ m mixes joins in the silicon rubber matrix through improving and processing, after stirring in homogenizer, add again the containing hydrogen silicone oil of 7 weight parts and the catalyzer of 4 weight parts, high-speed stirring, stirring velocity is 2500rpm, obtains base-material;
Wherein, being prepared as of modified oxidized aluminum particulate: the anhydrous alcohol solution that is 95% by mass concentration by the silane coupling agent of 0.2-2 weight part is configured to the silane coupling agent alcoholic solution that mass concentration is 3%-10%, is stirred to coupling agent and all dissolves; The Spherical alumina particles of 600 parts by weight is joined in the silane coupling agent alcoholic solution, after stirring, dry, obtain modified oxidized aluminum particulate;
(3) vacuumize: the base-material stirred is placed in vacuum machine and vacuumized, and the bubble that makes to be mixed in base-material is drawn out of fully;
(4) sulfidization molding: by base-material coldmoulding, cooling after the hot-air vulcanization 10-30min that is 100-180 ℃ by curing temperature, obtain the ultra-thin heat-conducting silica gel sheet of high-strong toughness.
Use standard ISO-22007-2 Hot Disk thermal constant analyser to be measured the heat conductive silica gel thermal conductivity, the thermal conductivity recorded is 2.03W, use standard P EACOCK thickness piece to be measured heat conductive silica gel thickness, the heat conductive silica gel thickness recorded is 0.15mm, use the standard tension trier to be measured the tensile strength of heat conductive silica gel, the heat conductive silica gel tensile strength recorded is 1.12MPa.
For a person skilled in the art, can make other various corresponding changes and distortion according to technical scheme described above and design, and these all changes and the distortion all should belong to the protection domain of the claims in the present invention within.
Claims (12)
1. the ultra-thin heat-conducting pad of high tenacity is characterized in that being prepared from by following raw material by weight:
Methyl vinyl silicone rubber 5-30 part
Vinyl silicone oil 10-50 part
Dimethyl silicone oil 10-100 part
MQ silicone resin 1-20 part
Modified oxidized aluminum particulate 300-1000 part
Silica gel strengthening agent 1-10 part
Containing hydrogen silicone oil 1-8 part
Catalyzer 0.5-5 part.
2. the ultra-thin heat-conducting pad of high tenacity according to claim 1 is characterized in that being prepared from by following raw material by weight:
15 parts of methyl vinyl silicone rubbers
25 parts of vinyl silicone oils
45 parts of dimethyl silicone oils
MQ silicone resin 1-20 part
Modified oxidized aluminum particulate 300-1000 part
Silica gel strengthening agent 1-10 part
Containing hydrogen silicone oil 1-8 part
Catalyzer 0.5-5 part.
3. the ultra-thin heat-conducting pad of high tenacity according to claim 1, it is characterized in that: described modified oxidized aluminum particulate is to prepare by the following method: the anhydrous alcohol solution that is 95% by mass concentration by the silane coupling agent of 0.2-2 weight part is configured to the silane coupling agent alcoholic solution that mass concentration is 3%-10%, is stirred to coupling agent and all dissolves; The Spherical alumina particles of 400-700 parts by weight is joined in the silane coupling agent alcoholic solution, after stirring, dry, obtain modified oxidized aluminum particulate.
4. the ultra-thin heat-conducting pad of high tenacity according to claim 1, it is characterized in that: described modified oxidized aluminum particulate comprises the Spherical alumina particles of two kinds of particle diameters of 3-10 μ m and 20-60 μ m, and the mass ratio of above-mentioned two kinds of particles is (2-5): (5-8).
5. the ultra-thin heat-conducting pad of high tenacity according to claim 1, it is characterized in that: described vinyl silicone oil viscosity is 1500-3000cps, the content of vinyl is 0.1-0.25%.
6. the ultra-thin heat-conducting pad of high tenacity according to claim 1, it is characterized in that: described dimethyl-silicon oil viscosity is 100-500cps.
7. the ultra-thin heat-conducting pad of high tenacity according to claim 1, it is characterized in that: described MQ silicone resin molecular weight is 5-20 ten thousand, and viscosity is 4000-10000cPas.
8. the ultra-thin heat-conducting pad of high tenacity according to claim 1, it is characterized in that: described silica gel strengthening agent is nano-scale white carbon black, median size is 20-500um.
9. the ultra-thin heat conductive silica gel pad of high tenacity according to claim 1, it is characterized in that: the hydrogen content of described containing hydrogen silicone oil is the 1-3% that accounts for containing hydrogen silicone oil weight.
10. according to the preparation method of the ultra-thin heat conductive silica gel pad of the described high tenacity of any one in claim 1-9, it is characterized in that it comprises the following steps in turn:
1) improvement of silicon rubber matrix and processing: vinyl silicone oil, dimethyl silicone oil, MQ silicone resin and silica gel toughener are uniformly mixed; colloid mixture called after modification after stirring strengthens silicone oil; methyl vinyl silicone rubber and modification are strengthened to silicone oil and add in mill and ground, obtain the silicon rubber matrix;
2) being uniformly mixed of silicon rubber matrix and alumina particle: modified oxidized aluminum particulate is joined in the silicon rubber matrix through improving and processing; after stirring in homogenizer; add again containing hydrogen silicone oil and catalyzer, high-speed stirring, stirring velocity 1500-3000rpm; Obtain base-material;
3) vacuumize: the base-material stirred is placed in vacuum machine and vacuumized, and the bubble that makes to be mixed in base-material is drawn out of fully;
4) sulfidization molding: by base-material coldmoulding, by cooling after hot-air vulcanization, curing temperature is 100-180 ℃, and curing time is: 10-30min; Obtain the ultra-thin heat conductive silica gel pad of high tenacity.
11. the preparation method of the ultra-thin heat conductive silica gel pad of high tenacity according to claim 10 is characterized in that: in step 1), the stirring that makes modification enhancing silicone oil is stirred by high speed dispersor, and stirring velocity is 1500-3000rpm; The temperature stirred is 100-200 ℃, and churning time is 0.5-2h.
12. the preparation method of the ultra-thin heat conductive silica gel pad of high tenacity according to claim 10 is characterized in that: in step 4), vulcanize as hot-air vulcanization, curing temperature is 100-180 ℃, and curing time is: 10-30min.
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