CN116554834A - High-heat-conductivity high-strength organic silicon pouring sealant and preparation method thereof - Google Patents

High-heat-conductivity high-strength organic silicon pouring sealant and preparation method thereof Download PDF

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CN116554834A
CN116554834A CN202310650425.6A CN202310650425A CN116554834A CN 116554834 A CN116554834 A CN 116554834A CN 202310650425 A CN202310650425 A CN 202310650425A CN 116554834 A CN116554834 A CN 116554834A
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component
parts
base material
pouring sealant
nano whisker
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CN116554834B (en
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谢荣
郑柚田
陈如琴
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Shenzhen Shengkangtai Organosilicon Material Co ltd
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Shenzhen Shengkangtai Organosilicon Material Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00—Adhesives based on 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; Adhesives based on derivatives of such polymers
    • C09J183/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08—Macromolecular additives
    • 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
    • C08K3/28—Nitrogen-containing compounds
    • C08K2003/282—Binary compounds of nitrogen with aluminium
    • 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
    • C08K3/38—Boron-containing compounds
    • C08K2003/382—Boron-containing compounds and nitrogen
    • C08K2003/385—Binary compounds of nitrogen with boron
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets
    • C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The application relates to the technical field of electronic pouring sealants, and particularly discloses a high-heat-conductivity high-strength organic silicon pouring sealant and a preparation method thereof. The organic silicon pouring sealant comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 3.5-5.5:1; the component A comprises 100-120 parts of base material, 0.2-10 parts of hydrogen-containing silicone oil and 0.002-0.01 part of crosslinking inhibitor; the component B comprises the following raw materials in parts by weight: 100-120 parts of base material and 0.1-2 parts of platinum catalyst; the base material comprises 100-120 parts of vinyl polydimethylsiloxane, 380-500 parts of inorganic heat conducting filler and 40-50 parts of modified cellulose nano whisker; the modified cellulose nanowhisker is obtained by subjecting cellulose nanowhisker to a step comprising grafting acrylamide. The organic silicon pouring sealant has the advantages of low viscosity, high strength and large heat conductivity coefficient.

Description

High-heat-conductivity high-strength organic silicon pouring sealant and preparation method thereof
Technical Field
The application relates to the technical field of electronic pouring sealants, in particular to a high-heat-conductivity high-strength organic silicon pouring sealant and a preparation method thereof.
Background
Related products in the high-tech fields such as electronic components, large-scale integrated circuit boards, LEDs and the like are gradually transformed to targets with high performance, high reliability and miniaturization, and the requirements on the electronic pouring sealant are higher as the working environment of the electronic products is harsh.
Silicone rubber (i.e., silicone) can maintain elasticity over a wide temperature range for a long period of time, has good electrical properties and chemical stability, and can be used as a preferred material for encapsulating electronic and electrical assemblies. However, at the same time, the organosilicon material has the problem of small heat conductivity, and the heat conductivity is only about 0.2W/(m.K); a large amount of heat accumulated when the filled product is in use is difficult to quickly dissipate, thereby severely affecting the reliability and lifetime of the filled product. The conventional method is to improve the heat conduction performance of the organic silicon pouring sealant in a mode of filling heat conduction materials; common thermally conductive materials such as aluminum oxide, boron nitride, silicon carbide whiskers, and the like. However, when the heat conducting material is filled, a certain problem is brought, for example, in order to achieve a better heat conducting effect, the filling amount of the heat conducting material is generally relatively large, which causes that the potting adhesive filled with a large amount of heat conducting material becomes large, and the fluidity is poor, so that the heat conducting material is difficult to be used as the potting adhesive.
Therefore, developing an organosilicon pouring sealant with higher heat conductivity and lower viscosity is the main development direction at present. For example, in the application document with publication number CN 103131381A, vinyl silicone oils with different viscosities are selected to be compounded in a specific ratio so as to reduce the viscosity of the filling glue; for another example, in the application document with publication number CN 105176484A, micro-nano-sized aluminum nitride, aluminum oxide and boron nitride are compounded in a specific ratio to prepare a low-viscosity high-heat-conductivity filling adhesive.
The above filling glue is more concerned about its heat conducting properties and viscosity, but for filling, its mechanical strength is also an increasingly important performance index due to its increasingly severe application conditions. Therefore, it is necessary to provide a silicone potting compound that is highly thermally conductive, high strength and low viscosity.
Disclosure of Invention
In order to improve the heat conduction performance, strength and viscosity of the traditional organic silicon filling adhesive, the application provides the organic silicon filling adhesive with high heat conduction and high strength and the preparation method thereof.
In a first aspect, the present application provides a high-thermal-conductivity and high-strength silicone pouring sealant, which adopts the following technical scheme: the high-heat-conductivity high-strength organic silicon pouring sealant comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 3.5-5.5:1;
taking the weight of the component A as a reference, the component A comprises the following raw materials in parts by weight: 100-120 parts of base material, 0.2-10 parts of hydrogen-containing silicone oil and 0.002-0.01 part of crosslinking inhibitor;
taking the weight of the component B as a reference, the component B comprises the following raw materials in parts by weight: 100-120 parts of base material and 0.1-2 parts of platinum catalyst;
taking the weight of the base material as a reference, the base material comprises the following raw materials in parts by weight: 100-120 parts of vinyl polydimethylsiloxane, 380-500 parts of inorganic heat conducting filler and 40-50 parts of modified cellulose nano whisker; the modified cellulose nano whisker is obtained by grafting cellulose nano whisker with acrylamide.
In the base material, the modified cellulose nano whiskers form a cross-linked structure when the modified cellulose nano whiskers are distributed in the base material in a crisscross manner due to the fiber structure characteristic of the modified cellulose nano whiskers; and because the cellulose nano whisker has excellent strength, the strength of the organic silicon pouring sealant can be improved under the combined action.
The cellulose nano whisker has excellent strength, heat conduction performance and electric conduction performance; however, it has been found that unmodified modified cellulose nanowhiskers and other components, such as inorganic thermally conductive fillers, do not bind well, making their excellent properties difficult to develop. After the modified cellulose nanowhisker is modified, the adsorptivity of the cellulose nanowhisker to the inorganic heat conducting filler is improved, so that the inorganic heat conducting filler can be stably loaded on the modified cellulose nanowhisker, the heat conduction has certain directivity, and finally the strength and the heat conduction of the organosilicon pouring sealant are obviously improved. In addition, the addition of the modified cellulose nano whisker can reduce the addition amount of the inorganic heat conducting filler, thereby realizing the purpose of reducing the adhesive bonding of the organic silicon potting.
Further alternatively, the vinyl polydimethylsiloxane in the base stock may be 100 parts, 105 parts, 110 parts, 115 parts, or 120 parts; the inorganic heat conductive filler may be 380 parts, 390 parts, 400 parts, 420 parts, 440 parts, 460 parts, 480 parts, or 500 parts; the modified cellulose nanowhisker may be 40 parts, 42 parts, 44 parts, 46 parts, 48 parts, or 50 parts.
Further optionally, the preparation method of the modified cellulose nanowhisker comprises the following steps:
a1, adding an initiator into a cellulose nanowhisker suspension containing the cellulose nanowhisker, uniformly mixing, heating for initiation, and then adding acrylamide for heating reaction to obtain a cellulose nanowhisker grafted acrylic acid crude product;
a2, washing the crude product of the cellulose nano whisker grafted acrylic acid with water to obtain modified cellulose nano whisker;
the weight ratio of the cellulose nano whisker to the acrylamide is 1:0.3-1.5.
By adopting the technical scheme, the inorganic heat conducting filler can be uniformly dispersed in the base material and stably loaded; therefore, the heat of the encapsulated product can be timely and rapidly evacuated, and the heat dissipation effect of the encapsulated product is remarkably improved. In addition, the strength loss of the modified cellulose nanowhisker is smaller.
Further alternatively, the weight ratio of the cellulose nanowhisker to the acrylamide may be 1:0.3, 1:0.5, 1:0.7, 1:0.9, 1:1.1, 1:1.3, or 1:1.5.
Further alternatively, the temperature for heating initiation in A1 is 60-70 ℃, and the initiation time is 5-10min; the temperature of the heating reaction is 60-70 ℃ and the reaction time is 30-90min.
Further alternatively, the initiator comprises 5-8wt% of the cellulose nanowhisker.
Optionally, the width of the nanocellulose whisker is 5-50nm, and the length is 50-500nm.
Optionally, the base material is prepared by a method comprising the following steps:
mixing vinyl polydimethylsiloxane, inorganic heat conducting filler and modified cellulose nano whisker according to the proportion, vacuum mixing for 45-80min at the temperature of 80-90 ℃, cooling and crushing to obtain the base material.
By adopting the technical scheme, the raw materials in the base material can be fully and uniformly mixed, and the effective load of the inorganic heat conducting filler on the modified cellulose nano whisker is realized.
Optionally, the inorganic heat conductive filler is selected from any one of spherical alumina, a mixture of spherical alumina and aluminum nitride, and a mixture of spherical alumina and boron nitride.
By adopting the technical scheme, the selection of the inorganic heat conduction filler is further optimized, so that the heat conduction effect of the organic silicon pouring sealant is further improved.
Further alternatively, the mixture of spherical alumina and aluminum nitride is obtained by mixing spherical alumina and aluminum nitride in a weight ratio of 8-15:1; the mixture of spherical alumina and boron nitride is obtained by mixing spherical alumina and boron nitride in a weight ratio of 5-8:1. Further alternatively, the weight ratio of spherical alumina to aluminum nitride may be 8:1, 10:1, 12:1, 13:1, or 15:1; the weight ratio of spherical alumina to boron nitride may be 5:1, 6:1, 7:1, or 8:1.
Further alternatively, the spherical alumina has a particle size of 10 to 50 μm, the aluminum nitride has a particle size of 0.6 to 0.8 μm, and the boron nitride has a particle size of 0.1 to 5 μm.
Alternatively, the platinum catalyst is chloroplatinic acid or a chloroplatinic acid complex having a platinum content of 100 to 5000 ppm.
Optionally, the hydrogen content of the hydrogen-containing silicone oil is 0.3-1.8wt%.
Optionally, the vinyl polydimethylsiloxane is terminated vinyl polydimethylsiloxane, the vinyl content of the vinyl polydimethylsiloxane is 0.3-0.5wt%, and the viscosity at 25 ℃ is 450-550 mPa.s.
In a second aspect, the present application provides a preparation method of the above-mentioned silicone pouring sealant, which adopts the following technical scheme: the preparation method of the organic silicon pouring sealant comprises the following steps:
s1, preparing a component A: uniformly mixing the formula amount of base material, hydrogen-containing silicone oil and crosslinking inhibitor to obtain the component A;
and (3) preparing a component B: uniformly mixing the formula amount of base material and a platinum catalyst to obtain the component B;
and S2, uniformly mixing the component A and the component B according to a proportion, and carrying out vacuum defoaming to obtain the organosilicon pouring sealant.
By adopting the technical scheme, the organic silicon pouring sealant with high strength, excellent thermal conductivity and low viscosity is prepared.
In summary, the present application has the following beneficial effects:
1. when the base material is prepared, modified cellulose nano whisker is added; the modified cellulose nano whiskers form a cross-linked structure when distributed in a crisscross manner in the base material, and meanwhile, inorganic heat conducting filler is stably loaded; because the cellulose nano whisker and the inorganic heat conducting filler have excellent strength, the strength and the heat conducting property of the organic silicon pouring sealant can be obviously improved under the comprehensive action; meanwhile, the addition of the modified cellulose nano whisker reduces the use amount of the inorganic heat conducting filler, so that the viscosity of the organic silicon pouring sealant is obviously reduced.
2. In this application, it is preferred to modify the cellulose nanowhiskers with acrylamide to give them an excellent ability to load inorganic thermally conductive fillers.
Detailed Description
The present application is described in further detail below with reference to examples.
The cellulose nanowhisker suspension is purchased from Northc nanotechnology, inc. of Suzhou, wherein the cellulose nanowhisker content is 2wt%, the cellulose nanowhisker has a diameter of 10-50nm, a length of 100-500nm, and an aspect ratio of 1-100. The vinyl-terminated polydimethylsiloxane has a CAS number of 68083-19-2, a vinyl content of 0.37-0.43 wt.% and a viscosity of 500 mPa.s at 25 ℃. The particle size of the spherical alumina is 10-50 mu m, the particle size of the aluminum nitride is 0.6-0.8 mu m, and the particle size of the boron nitride is 0.1-5 mu m. The CAS number of the hydrogen-containing silicone oil is 63148-57-2, and the hydrogen content is 1.6wt%.
Base stock preparation example
Base preparation example 1
The raw materials for preparing the base material are as follows: 100g of vinyl-terminated polydimethylsiloxane, 380g of spherical alumina and 40g of modified cellulose nano whisker.
The preparation raw materials of the modified cellulose nano whisker are as follows: a suspension of cellulose nanowhiskers (cellulose nanowhisker content of 2 wt%) of potassium persulfate as an initiator, 5wt% of cellulose nanowhiskers, and acrylamide in a weight ratio of cellulose nanowhiskers of 0.3:1.
The preparation method of the modified cellulose nano whisker comprises the following steps: a1, adding an initiator potassium persulfate into the cellulose nano whisker suspension according to the proportion, and initiating for 10min after heating to 60 ℃; then adding the acrylamide with the proportion, and reacting for 90min at the temperature of 60 ℃ to obtain the cellulose nano whisker grafted acrylic acid crude product.
A2, washing the crude product of the cellulose nano whisker grafted acrylic acid with water, centrifuging, and drying to obtain the modified cellulose nano whisker.
The preparation method of the base material comprises the following steps: mixing vinyl-terminated polydimethylsiloxane, spherical alumina and modified cellulose nano whisker according to the proportion, mixing for 80min at 80 ℃ under vacuum (the vacuum degree is 0.06 MPa), cooling, grinding and crushing to obtain the base material.
Base stock preparation example 2
The raw materials for preparing the base material are as follows: 110g of vinyl-terminated polydimethylsiloxane, 400g of spherical alumina, 35g of aluminum nitride and 45g of modified cellulose nano whisker.
The preparation raw materials of the modified cellulose nano whisker are as follows: a suspension of cellulose nanowhiskers (cellulose nanowhisker content of 2 wt%) of potassium persulfate as an initiator, which is 6.5wt% of cellulose nanowhiskers, and acrylamide in a weight ratio of cellulose nanowhiskers of 0.8:1.
The preparation method of the modified cellulose nano whisker comprises the following steps: a1, adding an initiator potassium persulfate into the cellulose nano whisker suspension according to the proportion, heating to 65 ℃ and initiating for 8min; then adding the acrylamide with the proportion, and reacting for 60min at the temperature of 65 ℃ to obtain the cellulose nano whisker grafted acrylic acid crude product.
A2, washing the crude product of the cellulose nano whisker grafted acrylic acid with water, centrifuging, and drying to obtain the modified cellulose nano whisker.
The preparation method of the base material comprises the following steps: mixing vinyl-terminated polydimethylsiloxane, spherical alumina, aluminum nitride and modified cellulose nano whisker according to the proportion, mixing for 65min at the temperature of 85 ℃ in vacuum (the vacuum degree is 0.08 MPa), cooling, grinding and crushing to obtain the base material.
Base stock preparation example 3
The raw materials for preparing the base material are as follows: 120g of vinyl-terminated polydimethylsiloxane, 437g of spherical alumina, 63g of boron nitride and 50g of modified cellulose nano whisker.
The preparation raw materials of the modified cellulose nano whisker are as follows: a suspension of cellulose nanowhiskers (cellulose nanowhisker content of 2 wt%) of potassium persulfate as an initiator, which is 8wt% of the cellulose nanowhiskers, and acrylamide in a weight ratio of cellulose nanowhiskers of 1.5:1.
The preparation method of the modified cellulose nano whisker comprises the following steps: a1, adding an initiator potassium persulfate into the cellulose nano whisker suspension according to the proportion, and initiating for 5min after heating to 70 ℃; then adding the acrylamide with the proportion, and reacting for 30min at the temperature of 70 ℃ to obtain the cellulose nano whisker grafted acrylic acid crude product.
A2, washing the crude product of the cellulose nano whisker grafted acrylic acid with water, centrifuging, and drying to obtain the modified cellulose nano whisker.
The preparation method of the base material comprises the following steps: mixing vinyl-terminated polydimethylsiloxane, spherical alumina, boron nitride and modified cellulose nano whisker according to the proportion, vacuum mixing at 90 ℃ for 45min (the vacuum degree is 0.1 MPa), cooling, grinding and crushing to obtain the base material.
Base stock preparation example 4
The difference from preparation example 2 is that the raw materials for preparing the base material are: 110g of vinyl-terminated polydimethylsiloxane, 400g of spherical alumina and 35g of aluminum nitride.
The preparation method of the base material comprises the following steps: mixing vinyl-terminated polydimethylsiloxane with spherical alumina and aluminum nitride according to the proportion, vacuum-mixing at 85 ℃ for 65min (vacuum degree is 0.08 MPa), cooling, grinding and crushing to obtain the base material.
Base stock preparation example 5
The difference from preparation example 2 is the different amounts of modified cellulose nanowhiskers; the raw materials for preparing the base material specifically comprise: 110g of vinyl-terminated polydimethylsiloxane, 400g of spherical alumina, 35g of aluminum nitride and 35g of modified cellulose nano whisker. The procedure of preparation 2 is otherwise followed.
Base stock preparation example 6
The difference from preparation example 2 is the different amounts of modified cellulose nanowhiskers; the raw materials for preparing the base material specifically comprise: 110g of vinyl-terminated polydimethylsiloxane, 400g of spherical alumina, 35g of aluminum nitride and 40g of modified cellulose nano whisker. The procedure of preparation 2 is otherwise followed.
Base stock preparation example 7
The difference from preparation example 2 is the different amounts of modified cellulose nanowhiskers; the raw materials for preparing the base material specifically comprise: 110g of vinyl-terminated polydimethylsiloxane, 400g of spherical alumina, 35g of aluminum nitride and 50g of modified cellulose nano whisker. The procedure of preparation 2 is otherwise followed.
Base stock preparation example 8
The difference from preparation example 2 is the different amounts of modified cellulose nanowhiskers; the raw materials for preparing the base material specifically comprise: 110g of vinyl-terminated polydimethylsiloxane, 400g of spherical alumina, 35g of aluminum nitride and 55g of modified cellulose nano whisker. The procedure of preparation 2 is otherwise followed.
Base stock preparation example 9
The difference from preparation example 2 is that the modified cellulose nanowhisker is replaced by an equal weight of cellulose nanowhisker in the preparation raw material; the raw materials for preparing the base material specifically comprise: 110g of vinyl-terminated polydimethylsiloxane, 400g of spherical alumina, 35g of aluminum nitride and 45g of cellulose nano whisker. The cellulose nano whisker is obtained by filtering and dewatering a cellulose nano whisker suspension and then drying; the selection of the cellulose nanowhisker suspension was the same as in preparation example 2. Other raw materials and preparation methods are the same as in preparation example 2.
Base stock preparation example 10
The difference from preparation example 2 is that the raw materials for preparing the base material are: 110g of vinyl-terminated polydimethylsiloxane, 644g of spherical alumina and 56g of aluminum nitride.
The preparation method of the base material comprises the following steps: mixing vinyl-terminated polydimethylsiloxane, spherical alumina and aluminum nitride according to the proportion, vacuum-mixing at 85 ℃ for 65min (vacuum degree is 0.08 MPa), cooling, grinding and crushing to obtain the base material.
Base stock preparation 11
The difference from preparation example 2 is that the raw materials for preparing the base material are: 110g of vinyl-terminated polydimethylsiloxane, 435g of spherical alumina and 45g of modified cellulose nanowhisker. The procedure of preparation 2 is otherwise followed.
Base stock preparation example 12
The difference from preparation example 2 is that the raw materials for preparing the base material are: 110g of vinyl-terminated polydimethylsiloxane, 380g of spherical alumina, 55g of boron nitride and 45g of modified cellulose nano whisker. The procedure of preparation 2 is otherwise followed.
Examples
Example 1
A high-heat-conductivity high-strength organic silicon pouring sealant comprises a component A and a component B.
The raw materials for preparing the component A are as follows: 100g of base material, 0.2g of hydrogen-containing silicone oil and 0.002g of crosslinking inhibitor phenylacetylene; the raw materials for preparing the component B are as follows: 100g of base material and 0.1g of chloroplatinic acid with the platinum content of 5000 ppm. Wherein, the base materials of the component A and the component B are prepared by base material preparation example 1.
The preparation method of the high-heat-conductivity high-strength organic silicon pouring sealant comprises the following steps: s1, preparing a component A: mixing and stirring the formula amount of base material, hydrogen-containing silicone oil and phenylacetylene for 10min, and obtaining the component A after uniform mixing; and (3) preparing a component B: mixing the base material with the formula amount and chloroplatinic acid for 10min, and obtaining the component B after uniform mixing. S2, uniformly mixing the component A and the component B according to the weight ratio of 3.5:1, and defoaming for 5 minutes under vacuum (the vacuum degree is 0.06 MPa) to obtain the organic silicon pouring sealant.
Example 2
A high-heat-conductivity high-strength organic silicon pouring sealant comprises a component A and a component B.
The raw materials for preparing the component A are as follows: 110g of base material, 5g of hydrogen-containing silicone oil and 0.006g of crosslinking inhibitor phenylacetylene; the raw materials for preparing the component B are as follows: 110g of base material and 0.8g of chloroplatinic acid with the platinum content of 1000 ppm. Wherein, the base materials of the component A and the component B are prepared by base material preparation example 2.
The preparation method of the high-heat-conductivity high-strength organic silicon pouring sealant comprises the following steps: s1, preparing a component A: mixing and stirring the formula amount of base material, hydrogen-containing silicone oil and phenylacetylene for 20min, and obtaining the component A after uniform mixing; and (3) preparing a component B: mixing and stirring the base material with the formula amount and chloroplatinic acid for 20min, and obtaining the component B after uniform mixing. S2, uniformly mixing the component A and the component B according to the weight ratio of 4:1, and defoaming for 8min under vacuum (the vacuum degree is 0.08 MPa) to obtain the organosilicon pouring sealant.
Example 3
A high-heat-conductivity high-strength organic silicon pouring sealant comprises a component A and a component B.
The raw materials for preparing the component A are as follows: 120g of base material, 10g of hydrogen-containing silicone oil and 0.01g of crosslinking inhibitor phenylacetylene; the raw materials for preparing the component B are as follows: 120g of base material and 2.0g of chloroplatinic acid with the platinum content of 100 ppm. Wherein, the base materials of the A component and the B component are prepared by base material preparation example 3.
The preparation method of the high-heat-conductivity high-strength organic silicon pouring sealant comprises the following steps: s1, preparing a component A: mixing and stirring the formula amount of base material, hydrogen-containing silicone oil and phenylacetylene for 30min, and obtaining the component A after uniform mixing; and (3) preparing a component B: mixing and stirring the base material with the formula amount and chloroplatinic acid for 30min, and obtaining the component B after uniform mixing. S2, uniformly mixing the component A and the component B according to the weight ratio of 5.5:1, and defoaming for 10 minutes under vacuum (the vacuum degree is 0.1 MPa) to obtain the organic silicon pouring sealant.
Examples 4 to 7
Examples 4-7 differ from example 2 in that the sources of the binders for the A and B components are different, see in particular Table 1; otherwise, the same as in example 2 is carried out.
Table 1 selection of binders in different embodiments
Description of the embodiments Example 2 Example 4 Example 5 Example 6 Example 7
Base stock source of component A Preparation example 2 Preparation example 6 Preparation example 7 PREPARATION EXAMPLE 11 Preparation example 12
Base stock source of component B Preparation example 2 Preparation example 6 Preparation example 7 PREPARATION EXAMPLE 11 Preparation example 12
Comparative examples 1 to 5
Comparative examples 1-5 differ from example 2 in that the sources of the binders for the A and B components are different, see in particular Table 2; otherwise, the same as in example 2 is carried out.
Table 2 selection of binders in different embodiments
Description of the embodiments Comparative example 1 Comparative example 2 Comparative example 3 Comparative example 4 Comparative example 5
Base stock source of component A Preparation example 4 Preparation example 5 Preparation example 8 Preparation example 9 Preparation example 10
Base stock source of component B Preparation example 4 Preparation example 5 Preparation example 8 Preparation example 9 Preparation example 10
Performance test
1. The relevant performance of all the prepared organic silicon pouring sealants is detected by referring to relevant regulations of T/FSI 043-2019 'organic silicon pouring sealant with high heat conductivity for electronic appliances', and the specific results are shown in Table 3.
TABLE 3 viscosity, tensile Strength, thermal conductivity of organosilicon casting glue
From the data results of examples 1-7 in Table 3, the organosilicon pouring sealant prepared by the application has the advantages of low viscosity, high tensile strength and large heat conductivity.
By comparing example 2 with comparative example 1, when preparing the organosilicon pouring sealant, the addition of the modified cellulose nanowhisker to the base material thereof can effectively improve the heat conductivity coefficient, viscosity and tensile strength of the organosilicon pouring sealant: the fiber structure of the modified cellulose nano whisker forms a penetrating network structure in the base material, and the excellent mechanical property of the modified cellulose nano whisker is combined, so that the tensile strength of the organic silicon pouring sealant can be improved; in addition, the modified cellulose nano whisker has larger load capacity and higher load stability on the inorganic heat-conducting filler, so that the inorganic heat-conducting filler with heat-conducting capacity and the modified cellulose nano whisker are loaded together, and the inorganic heat-conducting filler and the modified cellulose nano whisker have synergistic effect, so that the heat conductivity coefficient of the organosilicon pouring sealant can be obviously increased; after inorganic heat conducting filler is loaded on the modified cellulose nano whisker, the viscosity of the organosilicon pouring sealant is also reduced. And further combining the results of comparative example 4, it is shown that, because of the fiber characteristics of the cellulose nanowhiskers, the mechanical properties of the silicone potting adhesive can still be improved by adding the unmodified cellulose nanowhiskers, but the loading capacity of the unmodified cellulose nanowhiskers on the inorganic heat conducting filler is significantly reduced, so that the heat conducting and heat radiating processes of the unmodified cellulose nanowhiskers and the inorganic heat conducting filler are relatively carried out independently, and therefore, the aim of significantly improving the heat conducting property of the unmodified cellulose nanowhiskers is difficult to achieve. In comparative example 5, the heat conduction performance of the silicone potting adhesive was improved by increasing the addition amount of the inorganic heat conduction filler after no modified cellulose nanowhisker was added, so that the heat conduction coefficient thereof was 2.33W/(m·k), but the viscosity of the prepared silicone potting adhesive was too high to perform potting because the addition amount of the inorganic heat conduction material was too large.
While examples 2, 4-5 and comparative examples 2-3 illustrate that the modified cellulose nanowhiskers have an effect on the tensile strength, thermal conductivity and viscosity of the silicone potting adhesive when the base material of the silicone potting adhesive is prepared. The method comprises the following steps: in the base material, the addition amount of the modified cellulose nano whisker is recommended to be set in the range of 40-50 parts, and when the addition amount is too large (comparative example 3), the influence on the elongation at break of the organosilicon pouring sealant is small, but the heat conductivity coefficient and the tensile strength of the organosilicon pouring sealant are both greatly and negatively influenced; when the addition amount is too large (comparative example 2), the elongation at break, the heat conductivity coefficient, the tensile strength and the viscosity of the organosilicon pouring sealant are greatly negatively influenced.
2. The relevant performance of the prepared partial organosilicon pouring sealant is detected by referring to relevant regulations of T/FSI 043-2019 'addition type organosilicon pouring sealant with high heat conductivity for electronic appliances', and the specific results are shown in Table 4.
Table 4 shore hardness and flame retardant rating of silicone potting adhesive
From the results in table 4, the organosilicon pouring sealant prepared by the application has certain hardness and excellent flame retardant property.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.

Claims (10)

1. The high-heat-conductivity high-strength organic silicon pouring sealant is characterized by comprising a component A and a component B, wherein the mass ratio of the component A to the component B is 3.5-5.5:1;
taking the weight of the component A as a reference, the component A comprises the following raw materials in parts by weight: 100-120 parts of base material, 0.2-10 parts of hydrogen-containing silicone oil and 0.002-0.01 part of crosslinking inhibitor;
taking the weight of the component B as a reference, the component B comprises the following raw materials in parts by weight: 100-120 parts of base material and 0.1-2 parts of platinum catalyst;
taking the weight of the base material as a reference, the base material comprises the following raw materials in parts by weight: 100-120 parts of vinyl polydimethylsiloxane, 380-500 parts of inorganic heat conducting filler and 40-50 parts of modified cellulose nano whisker; the modified cellulose nano whisker is obtained by grafting cellulose nano whisker with acrylamide.
2. The silicone potting adhesive of claim 1, wherein the preparation method of the modified cellulose nanowhisker comprises the following steps:
a1, adding an initiator into a cellulose nanowhisker suspension containing the cellulose nanowhisker, uniformly mixing, heating for initiation, and then adding acrylamide for heating reaction to obtain a cellulose nanowhisker grafted acrylic acid crude product;
a2, washing the crude product of the cellulose nano whisker grafted acrylic acid with water to obtain modified cellulose nano whisker;
the weight ratio of the cellulose nano whisker to the acrylamide is 1:0.3-1.5.
3. The organic silicon pouring sealant according to claim 2, wherein the temperature for heating initiation in A1 is 60-70 ℃ and the initiation time is 5-10min; the temperature of the heating reaction is 60-70 ℃ and the reaction time is 30-90min.
4. The silicone potting adhesive of claim 1, wherein the nanocellulose whiskers have a width of 5-50nm and a length of 50-500nm.
5. The organic silicon pouring sealant according to claim 1, wherein the base material is prepared by a method comprising the following steps:
mixing vinyl polydimethylsiloxane, inorganic heat conducting filler and modified cellulose nano whisker according to the proportion, vacuum mixing for 45-80min at the temperature of 80-90 ℃, cooling and crushing to obtain the base material.
6. The silicone potting adhesive of claim 1, wherein the inorganic thermally conductive filler is selected from any one of spherical alumina, a mixture of spherical alumina and aluminum nitride, a mixture of spherical alumina and boron nitride.
7. The silicone potting adhesive of claim 6, wherein the spherical alumina has a particle size of 10 to 50 μm, the aluminum nitride has a particle size of 0.6 to 0.8 μm, and the boron nitride has a particle size of 0.1 to 5 μm.
8. The silicone potting adhesive of claim 1, wherein the platinum catalyst is chloroplatinic acid having a platinum content of 100 to 5000 ppm.
9. The silicone potting adhesive according to claim 1, wherein the hydrogen content of the hydrogen-containing silicone oil is 0.3 to 1.8wt%.
10. A method for preparing the organic silicon pouring sealant according to any one of claims 1 to 9, which is characterized by comprising the following steps:
s1, preparing a component A: uniformly mixing the formula amount of base material, hydrogen-containing silicone oil and crosslinking inhibitor to obtain the component A;
and (3) preparing a component B: uniformly mixing the formula amount of base material and a platinum catalyst to obtain the component B;
and S2, uniformly mixing the component A and the component B according to a proportion, and carrying out vacuum defoaming to obtain the organosilicon pouring sealant.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102337033A (en) * 2011-08-18 2012-02-01 华南理工大学 Additive high-thermal-conductivity organic silicon electronic pouring sealant and preparation method thereof
WO2019194032A1 (en) * 2018-04-06 2019-10-10 星光Pmc株式会社 Resin composition for solid molding material, method for producing same, and solid molded article
CN113201151A (en) * 2021-04-25 2021-08-03 浙江农林大学 High-strength high-toughness composite hydrogel crosslinked by trifunctional hyperbranched polysiloxane and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102337033A (en) * 2011-08-18 2012-02-01 华南理工大学 Additive high-thermal-conductivity organic silicon electronic pouring sealant and preparation method thereof
WO2019194032A1 (en) * 2018-04-06 2019-10-10 星光Pmc株式会社 Resin composition for solid molding material, method for producing same, and solid molded article
CN113201151A (en) * 2021-04-25 2021-08-03 浙江农林大学 High-strength high-toughness composite hydrogel crosslinked by trifunctional hyperbranched polysiloxane and preparation method thereof

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