CN113402887B - High-adhesion heat-conducting silica gel sheet and manufacturing process thereof - Google Patents
High-adhesion heat-conducting silica gel sheet and manufacturing process thereof Download PDFInfo
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- CN113402887B CN113402887B CN202110708923.2A CN202110708923A CN113402887B CN 113402887 B CN113402887 B CN 113402887B CN 202110708923 A CN202110708923 A CN 202110708923A CN 113402887 B CN113402887 B CN 113402887B
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- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
Abstract
The invention relates to the technical field of silica gel sheets, in particular to a high-adhesion heat-conducting silica gel sheet and a manufacturing process thereof, wherein the high-adhesion heat-conducting silica gel sheet comprises a component A and a component B, and the component A comprises the following raw materials: vinyl-terminated polymethylvinyl siloxane, hydrogen-containing methyl silicone oil, modified boron carbide, methyl vinyl MQ high-viscosity silicon resin, allyl glycidyl ether and a silane coupling agent; the component B comprises the following raw materials: vinyl-terminated polymethylvinylsiloxane, hydrogenous methyl silicone oil, modified carbon fiber and aluminum oxide; the component A is added, and the methyl vinyl MQ high-viscosity silicon resin and the allyl glycidyl ether are added, so that the bonding strength of the cured component A is improved; and finally, the component A, the component B and the component A are adopted to form a composite interlayer framework, the bonding strength of the component A after curing is better, the strength of the component B after curing is better, the composite interlayer framework ensures the high adhesiveness and the overall strength of the silica gel sheet, and the practicability is good.
Description
Technical Field
The invention relates to the technical field of silicone sheets, in particular to a high-adhesion heat-conducting silicone sheet and a manufacturing process thereof.
Background
In daily life, people can be widely applied to various electronic products, because the temperature of electronic components in the electronic products is increased during use, and heat dissipation of the electronic components is needed. For this reason, a fan for heat dissipation is usually disposed in an electronic product having a large volume, but a heat dissipation element having a smaller volume needs to be disposed for heat dissipation in an electronic product having a small volume because of insufficient internal space of the product. When the heat dissipation element is connected to the heat generation element, it is generally necessary to fill the gap between the heat generation element and the heat dissipation element with a filler material and a thermally conductive material. A heat conductive silicone sheet is a commonly used heat conductive interface material.
The heat-conducting silica gel sheet in the prior art usually takes metal oxide as a filler, and has the problems of relatively common strength and adhesive force. To solve the above problems, we propose a highly adhesive heat-conductive silicone sheet and a process for producing the same.
Disclosure of Invention
In view of the deficiencies of the prior art, the present invention provides a high adhesion thermal conductive silicone rubber sheet and a manufacturing process thereof, so as to overcome the problems mentioned in the background art.
In order to achieve the purpose, the technical scheme of the invention is realized by the following technical scheme: the high-adhesion heat-conducting silica gel sheet comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 60-70 parts of vinyl-terminated polymethylvinyl siloxane, 0.5-2 parts of hydrogen-containing methyl silicone oil, 40-300 parts of modified boron carbide, 1-3 parts of methyl vinyl MQ high-viscosity silicon resin, 1-3 parts of allyl glycidyl ether and 1-2 parts of silane coupling agent; the component B comprises the following raw materials in parts by weight: 60-70 parts of vinyl-terminated polymethylvinylsiloxane, 0.5-2 parts of hydrogen-containing methyl silicone oil, 60-150 parts of modified carbon fiber and 20-150 parts of aluminum oxide.
Preferably, the hydrogen content of the hydrogen-containing methyl silicone oil is 0.5-0.7%.
Preferably, the silane coupling agent is any one of vinyl silane, amino silane and butadiene-based triethoxy silane.
Preferably, the preparation method of the modified boron carbide comprises the following steps:
s1: dispersing boron carbide and a silane coupling agent in deionized water, and stirring for 30-50min to obtain a reaction solution;
s2: and (4) centrifugally filtering and drying the reaction solution to obtain the modified boron carbide.
Preferably, the preparation method of the modified carbon fiber comprises the following steps: and (3) carrying out anodic oxidation treatment for 1-3min in ammonium bicarbonate electrolyte by taking the carbon fiber as an anode and graphite as a cathode to obtain the modified carbon fiber.
Preferably, the mass fraction of the ammonium bicarbonate electrolyte is 8-10%.
Preferably, the oxidation treatment temperature is 25-30 ℃, and the current density is 0.25-0.35A/m 2 。
The invention also provides a manufacturing process of the high-adhesion heat-conducting silica gel sheet, which specifically comprises the following steps:
(1) Putting the vinyl-terminated polymethylvinyl siloxane, hydrogen-containing methyl silicone oil, modified boron carbide, methyl vinyl MQ high-viscosity silicon resin and allyl glycidyl ether into a stirrer, and stirring at the rotating speed of 800-1500r/min for 20-25min to obtain a component A;
(2) Putting the vinyl-terminated polymethylvinylsiloxane, the hydrogen-containing methylsilicone oil, the modified carbon fiber and the alumina into a stirrer, and stirring at the rotating speed of 1200-1800r/min for 25-30min to obtain a component B;
(3) Placing 50% of the component A on a substrate, flatly paving, heating for curing and cooling to room temperature;
(4) Placing the component B on the sample cured in the step (3), flatly paving the sample, heating the sample for curing, and cooling the sample to room temperature;
(5) And (4) placing the rest 50% of the component A on the sample solidified in the step (4), flatly paving the sample, heating the sample for solidification, and cooling the sample to room temperature to obtain the high-adhesiveness heat-conducting silica gel sheet.
The invention has the beneficial effects that:
according to the invention, the modified carbon fiber is added, because the carbon fiber has a smooth surface and poor gum dipping capability, the bonding strength between the carbon fiber and a substrate piece is low, the carbon fiber is used as an anode, graphite is used as a cathode, the surface of the carbon fiber is etched and oxidized by anodic oxidation treatment in ammonium bicarbonate electrolyte, and-COOH, -OH and other groups are connected to the surface of the carbon fiber, so that the surface energy and the roughness of the carbon fiber are improved, the bonding strength between the carbon fiber and the substrate is enhanced, and the overall strength of the heat-conducting silica gel sheet is improved;
according to the invention, the component A is added, and the silane coupling agent is used for modifying boron carbide, so that the uniform dispersion of the boron carbide is facilitated; the added methyl vinyl MQ high-viscosity silicon resin and allyl glycidyl ether improve the bonding strength of the cured component A; and finally, the component A, the component B and the component A are adopted to form a composite interlayer framework, the bonding strength of the component A after curing is better, the strength of the component B after curing is better, the composite interlayer framework ensures the high adhesiveness and the overall strength of the silica gel sheet, and the practicability is good.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described below in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of protection of the present invention.
Example 1
The high-adhesion heat-conducting silica gel sheet comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 60 parts of vinyl-terminated polymethylvinyl siloxane, 0.5 part of hydrogen-containing methyl silicone oil, 40 parts of modified boron carbide, 1 part of methyl vinyl MQ high-viscosity silicon resin, 1 part of allyl glycidyl ether and 1 part of silane coupling agent; the component B comprises the following raw materials in parts by weight: 60 parts of vinyl-terminated polymethylvinylsiloxane, 0.5 part of hydrogen-containing methyl silicone oil, 60 parts of modified carbon fiber and 20 parts of aluminum oxide.
The hydrogen content of the hydrogen-containing methyl silicone oil is 0.5 percent; the silane coupling agent is vinyl silane.
The preparation method of the modified boron carbide comprises the following steps: s1, dispersing boron carbide and a silane coupling agent in deionized water, and stirring for 30min to obtain a reaction solution; s2, carrying out centrifugal filtration and drying on the reaction liquid to obtain the modified boron carbide.
The preparation method of the modified carbon fiber comprises the following steps: carrying out anodic oxidation treatment for 1min in ammonium bicarbonate electrolyte by taking carbon fiber as an anode and graphite as a cathode to obtain modified carbon fiber; the mass fraction of the ammonium bicarbonate electrolyte is 8 percent; the oxidation treatment temperature was 25 ℃ and the current density was 0.25A/m 2 。
The manufacturing process of the high-adhesion heat-conducting silica gel sheet comprises the following steps:
(1) Putting the vinyl-terminated polymethylvinyl siloxane, hydrogen-containing methyl silicone oil, modified boron carbide, methyl vinyl MQ high-viscosity silicon resin and allyl glycidyl ether into a stirrer, and stirring at the rotating speed of 800r/min for 20min to obtain a component A;
(2) Putting the vinyl-terminated polymethylvinylsiloxane, the hydrogen-containing methylsilicone oil, the modified carbon fiber and the alumina into a stirrer, and stirring at the rotating speed of 1200r/min for 25min to obtain a component B;
(3) Placing 50% of the component A on a substrate, flatly paving, heating for curing and cooling to room temperature;
(4) Placing the component B on the sample cured in the step (3), flatly paving the sample, heating the sample for curing, and cooling the sample to room temperature;
(5) And (4) placing the rest 50% of the component A on the sample solidified in the step (4), flatly paving the sample, heating the sample for solidification, and cooling the sample to room temperature to obtain the high-adhesiveness heat-conducting silica gel sheet.
Example 2
The high-adhesion heat-conducting silica gel sheet comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 65 parts of vinyl-terminated polymethylvinyl siloxane, 1 part of hydrogen-containing methyl silicone oil, 100 parts of modified boron carbide, 2 parts of methyl vinyl MQ high-viscosity silicon resin, 2 parts of allyl glycidyl ether and 1.5 parts of silane coupling agent; the component B comprises the following raw materials in parts by weight: 60 parts of vinyl-terminated polymethylvinylsiloxane, 1 part of hydrogen-containing methyl silicone oil, 100 parts of modified carbon fiber and 60 parts of aluminum oxide.
The hydrogen content of the hydrogen-containing methyl silicone oil is 0.6 percent; the silane coupling agent is aminosilane.
The preparation method of the modified boron carbide comprises the following steps: s1, dispersing boron carbide and a silane coupling agent in deionized water, and stirring for 40min to obtain a reaction solution; s2, carrying out centrifugal filtration and drying on the reaction liquid to obtain the modified boron carbide.
The preparation method of the modified carbon fiber comprises the following steps: carrying out anodic oxidation treatment for 1.5min in ammonium bicarbonate electrolyte by taking carbon fiber as an anode and graphite as a cathode to obtain modified carbon fiber; the mass fraction of the ammonium bicarbonate electrolyte is 9 percent; the oxidation treatment temperature was 28 ℃ and the current density was 0.25A/m 2 。
The manufacturing process of the high-adhesion heat-conducting silica gel sheet comprises the following steps:
(1) Putting the vinyl-terminated polymethylvinyl siloxane, hydrogen-containing methyl silicone oil, modified boron carbide, methyl vinyl MQ high-viscosity silicon resin and allyl glycidyl ether into a stirrer, and stirring at the rotating speed of 1000r/min for 22min to obtain a component A;
(2) Putting the vinyl-terminated polymethylvinylsiloxane, the hydrogen-containing methylsilicone oil, the modified carbon fiber and the alumina into a stirrer, and stirring at the rotating speed of 1200r/min for 25min to obtain a component B;
(3) Placing 50% of the component A on a substrate, flatly paving, heating for curing and cooling to room temperature;
(4) Placing the component B on the sample cured in the step (3), flatly paving the sample, heating the sample for curing, and cooling the sample to room temperature;
(5) And (5) placing the rest 50% of the component A on the sample solidified in the step (4), flatly paving, heating for solidification, and cooling to room temperature to obtain the high-adhesion heat-conducting silica gel sheet.
Example 3
The high-adhesion heat-conducting silica gel sheet comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 65 parts of vinyl-terminated polymethylvinyl siloxane, 1 part of hydrogen-containing methyl silicone oil, 100 parts of modified boron carbide, 2 parts of methyl vinyl MQ high-viscosity silicon resin, 2 parts of allyl glycidyl ether and 1.5 parts of silane coupling agent; the component B comprises the following raw materials in parts by weight: 60 parts of vinyl-terminated polymethylvinylsiloxane, 1 part of hydrogen-containing methyl silicone oil, 100 parts of modified carbon fiber and 60 parts of aluminum oxide.
The hydrogen content of the hydrogen-containing methyl silicone oil is 0.6 percent; the silane coupling agent is butadiene-based triethoxysilane.
The preparation method of the modified boron carbide comprises the following steps: s1, dispersing boron carbide and a silane coupling agent in deionized water, and stirring for 35min to obtain a reaction solution; s2, carrying out centrifugal filtration and drying on the reaction liquid to obtain the modified boron carbide.
The preparation method of the modified carbon fiber comprises the following steps: carrying out anodic oxidation treatment for 1-3min in ammonium bicarbonate electrolyte by taking carbon fiber as an anode and graphite as a cathode to obtain modified carbon fiber; the mass fraction of the ammonium bicarbonate electrolyte is 10 percent; the oxidation treatment temperature was 30 ℃ and the current density was 0.3A/m 2 。
The manufacturing process of the high-adhesion heat-conducting silica gel sheet comprises the following steps:
(1) Putting the vinyl-terminated polymethylvinyl siloxane, hydrogen-containing methyl silicone oil, modified boron carbide, methyl vinyl MQ high-viscosity silicon resin and allyl glycidyl ether into a stirrer, and stirring at the rotating speed of 1200r/min for 20min to obtain a component A;
(2) Putting the vinyl-terminated polymethylvinylsiloxane, the hydrogen-containing methylsilicone oil, the modified carbon fiber and the alumina into a stirrer, and stirring for 30min at the rotating speed of 1600r/min to obtain a component B;
(3) Placing 50% of the component A on a substrate, flatly paving, heating for curing and cooling to room temperature;
(4) Placing the component B on the sample solidified in the step (3), flatly paving, heating for solidification and cooling to room temperature;
(5) And (4) placing the rest 50% of the component A on the sample solidified in the step (4), flatly paving the sample, heating the sample for solidification, and cooling the sample to room temperature to obtain the high-adhesiveness heat-conducting silica gel sheet.
Example 4
The high-adhesion heat-conducting silica gel sheet comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 70 parts of vinyl-terminated polymethylvinyl siloxane, 2 parts of hydrogen-containing methyl silicone oil, 150 parts of modified boron carbide, 3 parts of methyl vinyl MQ high-viscosity silicon resin, 3 parts of allyl glycidyl ether and 2 parts of silane coupling agent; the component B comprises the following raw materials in parts by weight: 70 parts of vinyl-terminated polymethylvinylsiloxane, 2 parts of hydrogen-containing methyl silicone oil, 120 parts of modified carbon fiber and 30 parts of aluminum oxide.
The hydrogen content of the hydrogen-containing methyl silicone oil is 0.7 percent; the silane coupling agent is vinyl silane.
The preparation method of the modified boron carbide comprises the following steps: s1, dispersing boron carbide and a silane coupling agent in deionized water, and stirring for 50min to obtain a reaction solution; s2, carrying out centrifugal filtration and drying on the reaction liquid to obtain the modified boron carbide.
The preparation method of the modified carbon fiber comprises the following steps: carrying out anodic oxidation treatment for 3min in ammonium bicarbonate electrolyte by taking carbon fiber as an anode and graphite as a cathode to obtain modified carbon fiber; the mass fraction of the ammonium bicarbonate electrolyte is 10 percent; the oxidation treatment temperature was 30 ℃ and the current density was 0.35A/m 2 。
The manufacturing process of the high-adhesion heat-conducting silica gel sheet comprises the following steps:
(1) Putting the vinyl-terminated polymethylvinyl siloxane, hydrogen-containing methyl silicone oil, modified boron carbide, methyl vinyl MQ high-viscosity silicon resin and allyl glycidyl ether into a stirrer, and stirring at the rotating speed of 1500r/min for 25min to obtain a component A;
(2) Putting the vinyl-terminated polymethylvinylsiloxane, the hydrogen-containing methylsilicone oil, the modified carbon fiber and the alumina into a stirrer, and stirring at the rotating speed of 1800r/min for 30min to obtain a component B;
(3) Placing 50% of the component A on a substrate, flatly paving, heating for curing and cooling to room temperature;
(4) Placing the component B on the sample cured in the step (3), flatly paving the sample, heating the sample for curing, and cooling the sample to room temperature;
(5) And (4) placing the rest 50% of the component A on the sample solidified in the step (4), flatly paving the sample, heating the sample for solidification, and cooling the sample to room temperature to obtain the high-adhesiveness heat-conducting silica gel sheet.
Performance detection
The test method comprises the following steps: the high adhesion thermally conductive silicone sheets of examples 1-4 were tested separately, wherein the tensile strength: the method is carried out according to the GB/T529-2008 standard; coefficient of thermal conductivity: reference is made to ASTM-D5470; initial tack ball number: the initial viscosity of the rubber composition is measured by a CNY-1 initial viscosity tester. Specific detection results are shown in table 1.
TABLE 1 Performance test
As can be seen from the above table, the high adhesion heat conductive silicone sheet of the present invention has good adhesion and strength.
It should be noted that, in this document, relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrases "comprising a," "8230," "8230," or "comprising" does not exclude the presence of additional like elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (4)
1. The high-adhesion heat-conducting silica gel sheet is characterized by comprising a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 60-70 parts of vinyl-terminated polymethylvinyl siloxane, 0.5-2 parts of hydrogen-containing methyl silicone oil, 40-300 parts of modified boron carbide, 1-3 parts of methyl vinyl MQ high-viscosity silicon resin, 1-3 parts of allyl glycidyl ether and 1-2 parts of silane coupling agent; the component B comprises the following raw materials in parts by weight: 60-70 parts of vinyl-terminated polymethylvinylsiloxane, 0.5-2 parts of hydrogen-containing methyl silicone oil, 60-150 parts of modified carbon fiber and 20-150 parts of aluminum oxide;
the preparation method of the modified carbon fiber comprises the following steps: carrying out anodic oxidation treatment for 1-3min in ammonium bicarbonate electrolyte by taking carbon fiber as an anode and graphite as a cathode to obtain modified carbon fiber;
the mass fraction of the ammonium bicarbonate electrolyte is 8-10%; the oxidation treatment temperature is 25-30 DEG CThe current density is 0.25-0.35A/m 2 ；
The manufacturing process of the high-adhesion heat-conducting silica gel sheet comprises the following steps:
(1) Putting the vinyl-terminated polymethylvinyl siloxane, hydrogen-containing methyl silicone oil, modified boron carbide, methyl vinyl MQ high-viscosity silicon resin and allyl glycidyl ether into a stirrer, and stirring at the rotating speed of 800-1500r/min for 20-25min to obtain a component A;
(2) Putting the vinyl-terminated polymethylvinylsiloxane, the hydrogen-containing methylsilicone oil, the modified carbon fiber and the alumina into a stirrer, and stirring at the rotating speed of 1200-1800r/min for 25-30min to obtain a component B;
(3) Placing 50% of the component A on a substrate, flatly paving, heating for curing and cooling to room temperature;
(4) Placing the component B on the sample solidified in the step (3), flatly paving, heating for solidification and cooling to room temperature;
(5) And (5) placing the rest 50% of the component A on the sample solidified in the step (4), flatly paving, heating for solidification, and cooling to room temperature to obtain the high-adhesion heat-conducting silica gel sheet.
2. The high-adhesion heat-conducting silicone sheet according to claim 1, wherein the hydrogen content of the hydrogen-containing methyl silicone oil is 0.5-0.7%.
3. The high-adhesion heat-conductive silicone sheet according to claim 1, wherein the silane coupling agent is any one of vinyl silane, amino silane, and butadienyl triethoxysilane.
4. The high-adhesion heat-conducting silica gel sheet according to claim 1, wherein the modified boron carbide is prepared by the following steps:
s1: dispersing boron carbide and a silane coupling agent in deionized water, and stirring for 30-50min to obtain a reaction solution;
s2: and carrying out centrifugal filtration and drying on the reaction solution to obtain the modified boron carbide.
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