CN112852171A - Ultra-soft high-thermal-conductivity silicone rubber composite material and preparation method thereof - Google Patents
Ultra-soft high-thermal-conductivity silicone rubber composite material and preparation method thereof Download PDFInfo
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- CN112852171A CN112852171A CN202110265587.9A CN202110265587A CN112852171A CN 112852171 A CN112852171 A CN 112852171A CN 202110265587 A CN202110265587 A CN 202110265587A CN 112852171 A CN112852171 A CN 112852171A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
Abstract
The invention discloses a super-soft high-thermal-conductivity silicone rubber composite material and a preparation method thereof, and relates to the technical field of thermal conduction materials, wherein the silicone rubber composite material comprises the following components in parts by weight: 100 parts of vinyl silicone oil; 2-4 parts of hydrogen-containing silicone oil; 900-1300 parts of spherical alumina; 1.5-3 parts of a coupling agent; 0.1-0.5 part of inhibitor; 1-2 parts of a platinum catalyst; the specific preparation method of the silicone rubber composite material comprises the following steps: s101: preparing spherical alumina; s102: mixing the raw materials; s103: rolling; s104: curing; s105: and (6) cutting. The spherical alumina in the raw materials has different particle sizes, and the spherical alumina is subjected to surface treatment by adopting the coupling agent, so that the surface compatibility of the spherical alumina is improved, the most compact filling and effective contact of the raw materials are realized, and the formation of a heat conduction network chain in a composite material system is facilitated, so that the silicone rubber composite material disclosed by the invention has excellent heat conduction performance and super-soft performance, and a better heat conduction effect.
Description
Technical Field
The invention relates to the technical field of heat conduction materials, in particular to a super-soft high-heat-conduction silicone rubber composite material and a preparation method thereof.
Background
The heat-conducting silicon rubber composite material can be used as a thermal interface material to be filled in a contact gap between a heating element and a radiator, so that air in the gap can be effectively removed, the contact thermal resistance between the heating element and the radiator is reduced, heat generated by the heating element is quickly conducted to the radiator and then dissipated, and the phenomenon that the temperature of the element is overhigh due to heat concentration is prevented.
The lower the hardness of the heat-conducting silicon rubber composite material is, the softer the material is, a layer with higher compression ratio and smaller interface thickness can be obtained in use, better fit and infiltration can be realized on a contact surface, the higher the heat conductivity coefficient of the material is, and the stronger the heat conduction capability of the interface layer is.
However, the heat-conducting silicone rubber composite material in the prior art cannot give consideration to both high heat conductivity coefficient and super-softness of the material, is not ideal in heat-conducting effect, and cannot meet the requirements of the existing market. Therefore, the person skilled in the art provides a super-soft high thermal conductive silicone rubber composite material and a preparation method thereof to solve the problems in the background art.
Disclosure of Invention
The invention aims to provide a super-soft high-heat-conductivity silicone rubber composite material and a preparation method thereof.
In order to achieve the purpose, the invention provides the following technical scheme: the super-soft high-thermal-conductivity silicone rubber composite material comprises the following components in parts by weight:
as a further scheme of the invention: the vinyl silicone oil is terminal vinyl silicone oil, wherein the vinyl content is 0.8-2.5 mol%, and the viscosity is 50-1000 mPa.
As a still further scheme of the invention: the hydrogen content in the hydrogen-containing silicone oil is 0.18 percent.
As a still further scheme of the invention: the purity of the spherical alumina is more than 99.5 percent, and the sphericity of the spherical alumina is more than or equal to 93 percent.
As a still further scheme of the invention: the spherical alumina consists of four kinds of spherical alumina with different particle sizes, namely D50: 110-130 μm, D50: 40-50 μm, D50: 10-20 μm and D50: 2-5 μm.
As a still further scheme of the invention: the adding proportion of four kinds of spherical alumina with different particle sizes of D50: 110-130 μm, D50: 40-50 μm, D50: 10-20 μm and D50: 2-5 μm in the spherical alumina is 4-7: 1-3: 1.
As a still further scheme of the invention: the coupling agent is a long-chain alkyl silane coupling agent.
As a still further scheme of the invention: the coupling agent is any one or a mixture of several of n-decyltrimethoxysilane, dodecyl trimethoxy silane, dodecyl triethoxy silane and hexadecyl trimethoxy silane.
A preparation method of a super-soft high-thermal-conductivity silicone rubber composite material comprises the following steps:
s101: preparing spherical alumina: putting four spherical aluminas with different particle diameters of D50: 110-130 μm, D50: 40-50 μm, D50: 10-20 μm and D50: 2-5 μm into a high-speed stirrer according to the proportion requirement, stirring and mixing for 2-5 min, then adding a coupling agent, stirring and mixing for 2-5 min, taking out the mixed materials after uniform stirring, putting the mixed materials into a drying box, and drying for 3-5 h at 80-100 ℃ to obtain dry modified compound spherical alumina;
s102: mixing raw materials: sequentially adding vinyl silicone oil, hydrogen-containing silicone oil, an inhibitor, a platinum catalyst and the dry-modified compound spherical alumina into a stirring tank according to the weight part ratio, putting the stirring tank into a centrifugal vacuum defoaming mixer for mixing raw materials, simultaneously vacuumizing the stirring tank in the mixing process, wherein the vacuum degree is-99 to-90 kPa, and obtaining a uniformly mixed sizing material after the mixing is finished;
s103: rolling: placing the rubber material between two layers of release films, and performing calendaring molding to obtain a sample wafer with a certain thickness;
s104: and (3) curing: curing and molding the sample wafer at the temperature of 80-120 ℃ for 20-40 min to obtain a cured finished product;
s105: cutting: cutting the cured finished product into required shape and size according to actual requirements to obtain the composite material product.
As a still further scheme of the invention: the mixing process in the S102 is carried out for three times, and the mixing is carried out for 20-30S at 500-1000 RPM, then for 10-20S at 1500-2500 RPM, and finally for 80-100S at 800-1200 RPM.
Compared with the prior art, the invention has the beneficial effects that: the invention discloses a super-soft high-heat-conductivity silicone rubber composite material and a preparation method thereof, wherein spherical alumina with different particle sizes is combined according to a certain proportion in raw materials, so that the most compact filling and effective contact of the raw materials are realized, the formation of a heat-conducting network chain in a composite material system is facilitated, and the spherical alumina is subjected to surface treatment by using a coupling agent, so that the surface compatibility of the spherical alumina is improved, and the defects are reduced, so that the silicone rubber composite material has excellent heat-conducting property and super-soft property, has a good heat-conducting effect, and solves the problems that the high-heat-conducting property and the super-soft property of the material cannot be considered in the prior art, and the heat-conducting effect is not ideal; the preparation method is simple, convenient to operate, low in cost, easy to produce and suitable for large-scale popularization.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the embodiment of the present invention, the first and second substrates,
example 1
The super-soft high-thermal-conductivity silicone rubber composite material comprises the following components in parts by weight:
further, the vinyl silicone oil is a terminal vinyl silicone oil having a vinyl group content of 2.0 mol% and a viscosity of 100 mPas.
Still further, the hydrogen content in the hydrogen-containing silicone oil is 0.18%.
Furthermore, the purity of the spherical alumina is more than 99.5 percent, and the sphericity of the spherical alumina is more than or equal to 93 percent.
Still further, the spherical alumina is composed of four spherical aluminas with different particle sizes of D50:120 μm, D50:40 μm, D50:10 μm and D50:5 μm.
Furthermore, the adding proportion of four spherical alumina with different grain diameters of D50:120 μm, D50:40 μm, D50:10 μm and D50:5 μm in the spherical alumina is 6:2:1: 1.
Still further, the coupling agent is n-decyltrimethoxysilane.
A preparation method of a super-soft high-thermal-conductivity silicone rubber composite material comprises the following steps:
s101: preparing spherical alumina: putting four spherical aluminas with different grain diameters of D50:120 μm, D50:40 μm, D50:10 μm and D50:5 μm into a high-speed stirrer according to the proportion requirement, stirring and mixing for 2min, then adding a coupling agent, stirring and mixing for 5min, taking out the mixed materials after uniform stirring, putting the mixed materials into a drying box, and drying for 3h at 100 ℃ to obtain dry modified compound spherical alumina;
s102: mixing raw materials: sequentially adding vinyl silicone oil, hydrogen-containing silicone oil, an inhibitor, a platinum catalyst and the dry-modified compound spherical alumina into a stirring tank according to the weight part ratio requirement, then putting the stirring tank into a centrifugal vacuum defoaming mixer to mix the raw materials, mixing the raw materials for three times, firstly mixing the raw materials for 30s at 500RPM, then mixing the raw materials for 20s at 2000RPM, finally mixing the raw materials for 80s at 1200RPM, simultaneously vacuumizing the mixing process, and controlling the vacuum degree to be-99 kPa to obtain a uniformly mixed sizing material after the mixing is finished;
s103: rolling: placing the rubber material between two layers of release films, and performing calendaring molding to obtain a sample wafer with a certain thickness;
s104: and (3) curing: curing and molding the sample wafer at 120 ℃ for 20min to obtain a cured finished product;
s105: cutting: cutting the cured finished product into required shape and size according to actual requirements to obtain the composite material product.
Example 2
The super-soft high-thermal-conductivity silicone rubber composite material comprises the following components in parts by weight:
further, the vinyl silicone oil is a terminal vinyl silicone oil having a vinyl group content of 1.8 mol% and a viscosity of 500 mPas.
Still further, the hydrogen content in the hydrogen-containing silicone oil is 0.18%.
Furthermore, the purity of the spherical alumina is more than 99.5 percent, and the sphericity of the spherical alumina is more than or equal to 93 percent.
Still further, the spherical alumina is composed of four spherical aluminas with different particle sizes of D50:115 μm, D50:45 μm, D50:10 μm and D50:2 μm.
Still further, the adding ratio of four spherical alumina with different particle sizes of D50:115 μm, D50:45 μm, D50:10 μm and D50:2 μm in the spherical alumina is 4:3:2: 1.
Still further, the coupling agent is hexadecyl trimethoxy silane.
A preparation method of a super-soft high-thermal-conductivity silicone rubber composite material comprises the following steps:
s101: preparing spherical alumina: putting four spherical aluminas with different grain diameters of D50:115 μm, D50:45 μm, D50:10 μm and D50:2 μm into a high-speed stirrer according to the proportion requirement, stirring and mixing for 3min, then adding a coupling agent, stirring and mixing for 4min, taking out the mixed materials after uniform stirring, putting the mixed materials into a drying box, and drying for 4h at 90 ℃ to obtain dry modified compound spherical alumina;
s102: mixing raw materials: sequentially adding vinyl silicone oil, hydrogen-containing silicone oil, an inhibitor, a platinum catalyst and the dry-modified compound spherical alumina into a stirring tank according to the weight part ratio requirement, then putting the stirring tank into a centrifugal vacuum defoaming mixer to mix the raw materials, mixing the raw materials for three times, firstly mixing the raw materials for 20s at 800RPM, then mixing the raw materials for 10s at 2500RPM, finally mixing the raw materials for 100s at 1000RPM, simultaneously vacuumizing the mixing process, wherein the vacuum degree is-95 kPa, and obtaining a uniformly mixed sizing material after the mixing is finished;
s103: rolling: placing the rubber material between two layers of release films, and performing calendaring molding to obtain a sample wafer with a certain thickness;
s104: and (3) curing: curing and molding the sample wafer at 100 ℃ for 30min to obtain a cured finished product;
s105: cutting: cutting the cured finished product into required shape and size according to actual requirements to obtain the composite material product.
Example 3
The super-soft high-thermal-conductivity silicone rubber composite material comprises the following components in parts by weight:
further, the vinyl silicone oil is a terminal vinyl silicone oil, wherein the vinyl content is 0.8 mol%, and the viscosity is 1000mPa · s.
Still further, the hydrogen content in the hydrogen-containing silicone oil is 0.18%.
Furthermore, the purity of the spherical alumina is more than 99.5 percent, and the sphericity of the spherical alumina is more than or equal to 93 percent.
Still further, the spherical alumina is composed of four spherical aluminas with different particle sizes of D50:130 μm, D50:50 μm, D50:20 μm and D50:5 μm.
Still further, the adding ratio of four spherical alumina with different particle sizes of D50:130 μm, D50:50 μm, D50:20 μm and D50:5 μm in the spherical alumina is 7:1:1: 1.
Still further, the coupling agent is dodecyl trimethoxy silane.
A preparation method of a super-soft high-thermal-conductivity silicone rubber composite material comprises the following steps:
s101: preparing spherical alumina: putting four spherical aluminas with different grain diameters of D50:130 μm, D50:50 μm, D50:20 μm and D50:5 μm into a high-speed stirrer according to the proportion requirement, stirring and mixing for 3min, then adding a coupling agent, stirring and mixing for 4min, taking out the mixed materials after uniform stirring, putting the mixed materials into a drying box, and drying for 5h at 80 ℃ to obtain dry modified compound spherical alumina;
s102: mixing raw materials: sequentially adding vinyl silicone oil, hydrogen-containing silicone oil, an inhibitor, a platinum catalyst and the dry-modified compound spherical alumina into a stirring tank according to the weight part ratio requirement, then putting the stirring tank into a centrifugal vacuum defoaming mixer to mix the raw materials, mixing the raw materials for three times, firstly mixing the raw materials for 20s at 1000RPM, then mixing the raw materials for 20s at 1500RPM, finally mixing the raw materials for 100s at 800RPM, simultaneously vacuumizing the mixing process, wherein the vacuum degree is-90 kPa, and obtaining a uniformly mixed sizing material after the mixing is finished;
s103: rolling: placing the rubber material between two layers of release films, and performing calendaring molding to obtain a sample wafer with a certain thickness;
s104: and (3) curing: curing and molding the sample wafer at 110 ℃ for 25min to obtain a cured finished product;
s105: cutting: cutting the cured finished product into required shape and size according to actual requirements to obtain the composite material product.
Examples of the experiments
The experimental method comprises the following steps: the silicone rubber composites prepared in example 1, example 2 and example 3 above were tested for thermal conductivity with reference to ASTM D5470; testing elongation at break with reference to GB/T528; hardness was tested by reference to ASTM D2240.
The experimental results are as follows: the specific test results are detailed in table 1 below.
TABLE 1 Performance test results for each product
| Item | Example 1 | Example 2 | Example 3 |
| Coefficient of thermal conductivity (W/m. K) | 2.81 | 3.04 | 3.61 |
| Elongation at Break (%) | 90.2 | 84.6 | 68.9 |
| Hardness (Shore00) | 14 | 17 | 20 |
Therefore, the ultra-soft high-thermal-conductivity silicone rubber composite materials prepared by the formulas and the preparation methods of the embodiment 1, the embodiment 2 and the embodiment 3 have the thermal conductivity coefficient of more than 2.8W/mK, the hardness Shore00 of less than or equal to 20, the elongation at break of more than 68, excellent thermal conductivity and ultra-soft performance, and the material has high elongation at break, and is beneficial to uncovering and repairing the material from a release film.
In conclusion, the raw materials are combined according to a certain proportion by spherical alumina with different particle sizes, so that the most compact filling and effective contact of the raw materials are realized, the formation of a heat conduction network chain in a composite material system is facilitated, and the spherical alumina is subjected to surface treatment by using a coupling agent, so that the surface compatibility of the spherical alumina is improved, the defects are reduced, the silicon rubber composite material has excellent heat conduction performance and super-soft performance, and the heat conduction effect is better; the preparation method is simple, convenient to operate, low in cost, easy to produce and suitable for large-scale popularization.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. The super-soft high-thermal-conductivity silicone rubber composite material is characterized in that: the silicone rubber composite material comprises the following components in parts by weight:
2. the ultra-soft high-thermal-conductivity silicone rubber composite material as claimed in claim 1, wherein: the vinyl silicone oil is terminal vinyl silicone oil, wherein the vinyl content is 0.8-2.5 mol%, and the viscosity is 50-1000 mPa.
3. The ultra-soft high-thermal-conductivity silicone rubber composite material as claimed in claim 1, wherein: the hydrogen content in the hydrogen-containing silicone oil is 0.18 percent.
4. The ultra-soft high-thermal-conductivity silicone rubber composite material as claimed in claim 1, wherein: the purity of the spherical alumina is more than 99.5 percent, and the sphericity of the spherical alumina is more than or equal to 93 percent.
5. The ultra-soft high thermal conductivity silicone rubber composite material according to claim 4, wherein: the spherical alumina consists of four kinds of spherical alumina with different particle sizes, namely D50: 110-130 μm, D50: 40-50 μm, D50: 10-20 μm and D50: 2-5 μm.
6. The ultra-soft high thermal conductivity silicone rubber composite material according to claim 5, wherein: the adding proportion of four kinds of spherical alumina with different particle sizes of D50: 110-130 μm, D50: 40-50 μm, D50: 10-20 μm and D50: 2-5 μm in the spherical alumina is 4-7: 1-3: 1.
7. The ultra-soft high-thermal-conductivity silicone rubber composite material as claimed in claim 1, wherein: the coupling agent is a long-chain alkyl silane coupling agent.
8. The ultra-soft high thermal conductivity silicone rubber composite material according to claim 7, wherein: the coupling agent is any one or a mixture of several of n-decyltrimethoxysilane, dodecyl trimethoxy silane, dodecyl triethoxy silane and hexadecyl trimethoxy silane.
9. The preparation method of the ultra-soft high-thermal-conductivity silicone rubber composite material according to any one of claims 1 to 8, characterized by comprising the following steps: the specific preparation method of the silicone rubber composite material comprises the following steps:
s101: preparing spherical alumina: putting four spherical aluminas with different particle diameters of D50: 110-130 μm, D50: 40-50 μm, D50: 10-20 μm and D50: 2-5 μm into a high-speed stirrer according to the proportion requirement, stirring and mixing for 2-5 min, then adding a coupling agent, stirring and mixing for 2-5 min, taking out the mixed materials after uniform stirring, putting the mixed materials into a drying box, and drying for 3-5 h at 80-100 ℃ to obtain dry modified compound spherical alumina;
s102: mixing raw materials: sequentially adding vinyl silicone oil, hydrogen-containing silicone oil, an inhibitor, a platinum catalyst and the dry-modified compound spherical alumina into a stirring tank according to the weight part ratio, putting the stirring tank into a centrifugal vacuum defoaming mixer for mixing raw materials, simultaneously vacuumizing the stirring tank in the mixing process, wherein the vacuum degree is-99 to-90 kPa, and obtaining a uniformly mixed sizing material after the mixing is finished;
s103: rolling: placing the rubber material between two layers of release films, and performing calendaring molding to obtain a sample wafer with a certain thickness;
s104: and (3) curing: curing and molding the sample wafer at the temperature of 80-120 ℃ for 20-40 min to obtain a cured finished product;
s105: cutting: cutting the cured finished product into required shape and size according to actual requirements to obtain the composite material product.
10. The preparation method of the ultra-soft high-thermal-conductivity silicone rubber composite material according to claim 9, characterized by comprising the following steps: the mixing process in the S102 is carried out for three times, and the mixing is carried out for 20-30S at 500-1000 RPM, then for 10-20S at 1500-2500 RPM, and finally for 80-100S at 800-1200 RPM.
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