CN110922937A - Organosilicon heat-conducting encapsulating silica gel with excellent performance - Google Patents
Organosilicon heat-conducting encapsulating silica gel with excellent performance Download PDFInfo
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- CN110922937A CN110922937A CN201911135257.7A CN201911135257A CN110922937A CN 110922937 A CN110922937 A CN 110922937A CN 201911135257 A CN201911135257 A CN 201911135257A CN 110922937 A CN110922937 A CN 110922937A
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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
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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
- 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
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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
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to organic silicon heat-conducting encapsulating silica gel with excellent performance, which comprises A, B components in parts by mass: the component A comprises: 16.5-7.5 parts of methyl vinyl polysiloxane, 28-9 parts of methyl vinyl polysiloxane, 84-86 parts of heat conducting powder, 1-2 parts of adhesive, 0.3-0.4 part of color paste and 0.03-0.05 part of catalyst; and B component: 136-40 parts of methyl vinyl polysiloxane, 22.5-3.5 parts of methyl vinyl polysiloxane, 83-85 parts of heat conducting powder, 2.7-3.0 parts of cross-linking agent and 0.008-0.012 part of inhibitor. The heat-conducting encapsulating silica gel prepared by the invention has high heat conductivity, low viscosity, low oil leakage, excellent anti-settling property and good bonding property to a PCB.
Description
Technical Field
The invention relates to an organosilicon high-thermal-conductivity silica gel with excellent performance, in particular to an organosilicon thermal-conductivity pouring sealant with high proportion of thermal-conductivity filler, low viscosity, low oil permeability, excellent sedimentation resistance and good adhesion to a PCB (printed circuit board), belonging to the field of pouring sealant adhesives.
Technical Field
The application trend of solvent-free heat-conducting silica gel products in the current market is better and better, the annual usage amount of the products is greatly improved, the market competition at home and abroad is very strong, and the cost pressure is very huge. The heat-conducting silica gel with low cost has the advantages that the higher the heat conductivity coefficient is, the higher the filler proportion is, the higher the viscosity of the product is, and in order to achieve the low viscosity, a large amount of diluting silicone oil is added, so that the oil permeability of the product is poor; meanwhile, the requirement on the adhesion of the product to a PCB (printed circuit board) is higher and higher, and the adhesion is further difficult due to the existence of a plurality of soldering fluxes on the PCB.
Disclosure of Invention
The invention aims to provide the organic silicon heat-conducting encapsulating silica gel which has high heat conduction, low viscosity, low oil leakage, excellent anti-settling property and good bonding property to a PCB.
In order to solve the problems, the invention particularly provides the following technical scheme: the organic silicon heat-conducting encapsulating silica gel is a two-component heating/room temperature curing silicon-hydrogen addition type organic silica gel, and A, B components comprise the following components in parts by mass:
component A
16.5 to 7.5 parts of methyl vinyl polysiloxane
28-9 parts of methyl vinyl polysiloxane
84-86 parts of heat conducting powder
1-2 parts of adhesive
0.3-0.4 parts of color paste
0.03 to 0.05 portion of catalyst
B component
136-40 parts of methyl vinyl polysiloxane
22.5 to 3.5 parts of methyl vinyl polysiloxane
83-85 parts of heat conducting powder
2.7-3.0 parts of cross-linking agent
0.008-0.012 parts of inhibitor
On the basis of the technical scheme, the invention can be further improved as follows:
further, the methyl vinyl polysiloxane-1 is a vinyl-terminated compound with a specific structural formula shown as (1)
Wherein, 45< m <50,
further, the thermal weight loss of the methylvinyl polysiloxane-1 is less than 0.04 percent at 150 ℃ for 4 hours; the viscosity is 95 to 105mPa.s, and the vinyl content is 0.95 to 1.05 wt%.
Adopt above-mentioned further beneficial effect: the low-viscosity vinyl silicone oil plays a basic role in the purposes of high proportion of heat-conducting filler and low viscosity.
Further, the methyl vinyl polysiloxane-2 is a compound containing vinyl at a single end, and has a specific structural formula shown as (2)
Wherein, 40< n <50,
further, the thermal weight loss of the methylvinyl polysiloxane-1 is less than 0.04 percent at 150 ℃ for 4 hours; the viscosity is 45-55 mPa.s, and the vinyl content is 0.70-0.85 wt%.
Adopt above-mentioned further beneficial effect: the low-viscosity methyl vinyl polysiloxane-2 has the advantages that one side is methyl and the other side is vinyl, so that the low-viscosity methyl vinyl polysiloxane-2 plays a role of a diluent, reduces the viscosity of a product, can participate in a curing reaction, connects a molecular chain to a main body, and further eliminates the problem of product precipitation caused by introduction of the diluent.
Further, the heat conducting powder is composite spherical alumina powder with the average grain diameter of 7.5 microns, and the surface of the alumina powder is subjected to active treatment.
Further, the composite spherical alumina is compounded by spherical alumina with the grain diameter of 2-50 μm, and the composite alumina powder is treated as follows: and (3) performing surface treatment on the spherical alumina by using a coupling agent with the structural formula (5) at 150 ℃ by using a spray granulation tower, and filtering by using an electric sieve and a 30-micrometer pore size net to obtain the required compound spherical alumina powder.
Adopt above-mentioned further beneficial effect: the surface-treated aluminum oxide can be better dispersed in a system, and meanwhile, because a large number of coupling agent groups exist on the surface and ester bond groups have higher polarity, the surface-treated aluminum oxide has certain repellency to system silicone oil, so that the surface-treated aluminum oxide has certain suspension property and good anti-settling property, and meanwhile, the adhesive force of the colloid to a base material is also effectively improved.
Further, the cross-linking agent is methyl hydrogen-containing polysiloxane, the hydrogen content is 0.30-0.40 wt%, and the viscosity is 30-60 mPa.s. The cross-linking agent contains hydrogen at side, and has a specific structural formula shown in (3)
Wherein 10< a <14, 12< b < 16.
Further, the structural formula of the adhesive is shown as (4):
wherein, K1＝6～8，K2＝3～5；
Advantageous effects of the use of the above further adhesive: molecules contain various polar groups, so that the bonding effect (various metals and plastics) on various base materials can be effectively improved, and the bonding effect on PCB materials is particularly obvious; a small amount of C ═ C double bonds can participate in the hydrosilylation reaction of the matrix, so that the introduction of useless molecular structures is avoided, the oil permeability is reduced, and the later stability and the aging performance of the adhesive are ensured; small amounts of carbonyl groups also contribute to improved adhesion of the colloid to the substrate surface.
Further, the inhibitor is vinyl double-end.
The beneficial effects of the previous step are as follows: the vinyl double-end socket is not easy to volatilize, plays a great role in the storage and use stability of the product, contains two vinyl groups, can participate in the reaction when reaching the curing condition, is connected to the main body structure, also avoids the problem of generating bubbles in the curing process caused by a volatile inhibitor, further eliminates the existence of useless substances after curing, and enhances the stability of the product.
Further, the catalyst should be selected from the platinum group of catalysts, preferably poisoning-resistant platinum-vinylsiloxane complexes, with a platinum content of 5000 ppm.
Adopt above-mentioned further beneficial effect: effectively reduces the poisoning phenomenon in the glue curing process.
Furthermore, the color paste is prepared by premixing vinyl silicone oil and dye, and is bright red.
Detailed Description
The processes and principles of the present invention are described in detail below with reference to specific embodiments, which are provided for further illustration of the invention and are not intended to limit the scope of the invention.
This glue solidification strip: curing at 80 ℃ for 30min or at room temperature for 24 h.
Example 1
The component A comprises: 7.0g of methylvinylpolysiloxane-1 of the formula (1) having a viscosity of 100mPa.s (where m is 48, the vinyl content is 1.0% by weight) were weighed in this order; 8.5g of methylvinylpolysiloxane-2 of formula (2) having a viscosity of 50mpa.s (where n is 45 and the vinyl content is 0.80% by weight); 85g of heat conducting powder; 1.5g of an adhesive of formula (4) (wherein K1＝7，K24); 0.35g of color paste; 5000ppm of catalyst 0.04 g; adding into a double-planet mixing kettle, and mixing uniformly under a vacuum state to obtain a component A;
and B component: 38g of methylvinylpolysiloxane-1 of the formula (1) having a viscosity of 100mpa.s (where m is 48, the vinyl content is 1.0% by weight) were weighed out in succession; 3.0g of methylvinylpolysiloxane-2 of formula (2) having a viscosity of 50mpa.s (where n is 45 and the vinyl content is 0.80% by weight); 84g of heat conducting powder; 2.85g of a crosslinker of formula (3) having a viscosity of 45mpa.s (where a is 12, b is 14, hydrogen content 0.35 wt%); 0.01g of inhibitor. Adding into a double-planet mixing kettle, and mixing uniformly under a vacuum state to obtain the component B.
Example 2
The component A comprises: 6.5g of methylvinylpolysiloxane-1 of the formula (1) having a viscosity of 100mPa.s (where m is 48, the vinyl content is 1.0% by weight) were weighed in this order; 9g of methylvinylpolysiloxane-2 of the formula (2) having a viscosity of 50mpa.s (where n is 45 and the vinyl content is 0.80% by weight); heat conductive powder 84g; 1.0g of an adhesive of formula (4) (wherein K1＝6，K25); 0.30g of color paste; 5000ppm of catalyst 0.05 g; adding into a double-planet mixing kettle, and mixing uniformly under a vacuum state to obtain a component A;
and B component: 36g of methylvinylpolysiloxane-1 of the formula (1) having a viscosity of 100mpa.s (where m is 48, the vinyl content is 1.0% by weight) were weighed in this order; 3.5g of methylvinylpolysiloxane-2 of formula (2) having a viscosity of 50mpa.s (where n is 45 and the vinyl content is 0.80% by weight); 85g of heat conducting powder; 2.70g of a crosslinker of formula (3) having a viscosity of 45mpa.s (where a is 12, b is 14, hydrogen content 0.35 wt%); 0.012g of inhibitor. Adding into a double-planet mixing kettle, and mixing uniformly under a vacuum state to obtain the component B.
Example 3
The component A comprises: 7.5g of methylvinylpolysiloxane-1 of the formula (1) having a viscosity of 95mPa.s (where m is 45 and the vinyl content is 1.05% by weight) were weighed in this order; 8g of methylvinylpolysiloxane-2 of formula (2) having a viscosity of 55mpa.s (where n is 50 and the vinyl content is 0.70% by weight); 86g of heat conducting powder; 2.0g of an adhesive of formula (4) (wherein K1＝8，K23); 0.0.4g of color paste; 5000ppm of catalyst 0.03 g; adding into a double-planet mixing kettle, and mixing uniformly under a vacuum state to obtain a component A;
and B component: 40g of methylvinylpolysiloxane-1 of the formula (1) having a viscosity of 105mPa.s (where m is 50, the vinyl content is 0.95% by weight) were weighed in this order; 3.0g of methylvinylpolysiloxane-2 of formula (2) having a viscosity of 45mpa.s (where n is 40 and the vinyl content is 0.85% by weight); 83g of heat conducting powder; 2.70g of a crosslinker of formula (3) having a viscosity of 45mpa.s (where a is 10, b is 16, hydrogen content 0.40 wt%); 0.008g of inhibitor. Adding into a double-planet mixing kettle, and mixing uniformly under a vacuum state to obtain the component B.
Comparative example 1
The component A comprises: 7.0g of methylvinylpolysiloxane-1 of the formula (1) having a viscosity of 100mPa.s (where m is 48, the vinyl content is 1.0% by weight) were weighed in this order; 8.5g of methylvinylpolysiloxane-2 of formula (2) having a viscosity of 50mpa.s (where n is 45 and the vinyl content is 0.80% by weight); 85g of heat conducting powder; 1.5g of KH-570 coupling agent; 0.35g of color paste; 5000ppm of catalyst 0.04 g; adding into a double-planet mixing kettle, and mixing uniformly under a vacuum state to obtain the component A.
And B component: 38g of methylvinylpolysiloxane-1 of the formula (1) having a viscosity of 100mpa.s (where m is 48, the vinyl content is 1.0% by weight) were weighed out in succession; 3.0g of methylvinylpolysiloxane-2 of formula (2) having a viscosity of 50mpa.s (where n is 45 and the vinyl content is 0.80% by weight); 84g of heat conducting powder; 2.85g of a crosslinker of formula (3) having a viscosity of 45mpa.s (where a is 12, b is 14, hydrogen content 0.35 wt%); 0.01g of inhibitor. Adding into a double-planet mixing kettle, and mixing uniformly under a vacuum state to obtain the component B.
The adhesive is a novel adhesive developed by itself, comparing the composition of comparative example 1 with the composition of example 1.
Comparative example 2
The component A comprises: 6.5g of methylvinylpolysiloxane-1 of the formula (1) having a viscosity of 100mPa.s (where m is 48, the vinyl content is 1.0% by weight) were weighed in this order; 9g of dimethicone having a viscosity of 50 mPa.s; 84g of heat conducting powder; 1.0g of an adhesive of formula (4) (wherein K1＝6，K25); 0.30g of color paste; 5000ppm of catalyst 0.05 g; adding into a double-planet mixing kettle, and mixing uniformly under a vacuum state to obtain the component A.
And B component: 36g of methylvinylpolysiloxane-1 of the formula (1) having a viscosity of 100mpa.s (where m is 48, the vinyl content is 1.0% by weight) were weighed in this order; 3.5g of dimethicone with a viscosity of 50 mPa.s; 85g of heat conducting powder; 2.70g of a crosslinker of formula (3) having a viscosity of 45mpa.s (where a is 12, b is 14, hydrogen content 0.35 wt%); 0.012g of inhibitor. Adding into a double-planet mixing kettle, and mixing uniformly under a vacuum state to obtain the component B.
The composition of comparative example 2 is comparable to the composition of example 2, with the dimethicone diluent of the comparative example being free of reactive groups.
Comparative example 3
The component A comprises: successively weighing methylethyl ether with the viscosity of 95mPa.s as shown in the structural formula (1)7.5g of alkenylpolysiloxane-1 (wherein m is 45, and the vinyl content is 1.05 wt%); 8g of methylvinylpolysiloxane-2 of formula (2) having a viscosity of 55mpa.s (where n is 50 and the vinyl content is 0.70% by weight); 86g of heat conductive powder (treated with KH-570); 2.0g of an adhesive of formula (4) (wherein K1＝8，K23); 0.0.4g of color paste; 5000ppm of catalyst 0.03 g; adding into a double-planet mixing kettle, and mixing uniformly under a vacuum state to obtain the component A.
And B component: 40g of methylvinylpolysiloxane-1 of the formula (1) having a viscosity of 105mPa.s (where m is 50, the vinyl content is 0.95% by weight) were weighed in this order; 3.0g of methylvinylpolysiloxane-2 of formula (2) having a viscosity of 45mpa.s (where n is 40 and the vinyl content is 0.85% by weight); 83g of heat conductive powder (KH-570 was used for treating composite spherical alumina); 2.70g of a crosslinker of formula (3) having a viscosity of 45mpa.s (where a is 10, b is 16, hydrogen content 0.40 wt%); 0.008g of inhibitor. Adding into a double-planet mixing kettle, and mixing uniformly under a vacuum state to obtain the component B.
The composition of comparative example 3 is different from that of example 3 in the treatment agent used for the heat conductive powder of comparative example, and other raw materials, processes and the like are completely the same.
Oil permeability standard:
1. die cutting or jig curing three sample pieces with phi 30mm x 3 (+ -0.1) mm.
2. An electronic balance (precision +/-0.1 mg) is used for weighing and recording the weight.
3. After the sample is weighed, white filter paper is placed on one surface, and a PE film is placed on the other surface. The glass is placed between two pieces of toughened glass and is locked by four screws, and the product compression ratio is adjusted by controlling the distance between the upper glass and the lower glass. The compressibility was 25%, 3 (+ -0.1) mm was compressed to 2.25 (+ -0.1) mm. Putting the fixing device into an environment box with 85 ℃ and 85% humidity for 1000h, and taking out.
4. After the sample passes through a double 85 environment for 1000 hours, the silicone oil seeps out and is adsorbed by the filter paper to form an approximately circular oil halo. Measuring the weight of the sample before and after baking to obtain the oil leakage amount of the sample; the average value of two diameters in the vertical direction of the oil halo is taken as the oil penetration diameter.
5. formula:
weight loss (g) is the amount of oil leakage (weight before experiment-weight after experiment)
Oil permeability [% ] or oil permeability ÷ experimental golden sample weight × 100
6. The average oil permeability of three sample pieces was taken.
The results of the performance parameter tests of examples 1-3 and comparative examples 1-2 are given in the following table:
the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the scope of the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention are included in the scope of the present invention.
Claims (5)
1. An organic silicon heat-conducting encapsulating silica gel with excellent performance is characterized in that A, B components comprise the following components in parts by mass:
component A
16.5 to 7.5 parts of methyl vinyl polysiloxane
28-9 parts of methyl vinyl polysiloxane
84-86 parts of heat conducting powder
1-2 parts of adhesive
0.3-0.4 parts of color paste
0.03 to 0.05 portion of catalyst
B component
136-40 parts of methyl vinyl polysiloxane
22.5 to 3.5 parts of methyl vinyl polysiloxane
83-85 parts of heat conducting powder
2.7-3.0 parts of cross-linking agent
0.008-0.012 parts of inhibitor
The methyl vinyl polysiloxane-1 is a vinyl-terminated compound with a specific structural formula (1)
Wherein 45< m < 50;
the methyl vinyl polysiloxane-2 is a compound containing vinyl at a single end and has a specific structural formula shown as (2)
Wherein 40< n < 50.
2. The silicone heat-conducting potting silica gel of claim 1, wherein the cross-linking agent is methyl hydrogen-containing polysiloxane having the structural formula (3)
Wherein 10< a <14, 12< b < 16.
3. The silicone heat-conducting potting silicone as claimed in claim 1, wherein the structural formula of the adhesive is as shown in (4):
wherein, K1＝6～8，K2＝3～5。
4. The silicone heat-conducting encapsulating silica gel as claimed in claim 1, wherein the heat-conducting powder is a composite spherical alumina powder with an average particle size of 7.5 μm, the composite spherical alumina is compounded by spherical alumina with a particle size of 2 μm to 50 μm, and the compounded alumina powder is treated as follows: using a spray granulation tower, carrying out surface treatment on spherical alumina by using a coupling agent with the structural formula shown in the formula (5) at 150 ℃, and simultaneously filtering by using an electric sieve and a 30-micrometer pore size net to prepare the required compound spherical alumina powder;
5. the silicone heat-conducting potting silica gel of claim 1, wherein the inhibitor is a vinyl double head, the catalyst is an anti-poisoning platinum-vinylsiloxane complex, and the platinum content is 5000 ppm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114213979A (en) * | 2021-11-10 | 2022-03-22 | 中科检测技术服务(重庆)有限公司 | Electronic material glue solution and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114213979A (en) * | 2021-11-10 | 2022-03-22 | 中科检测技术服务(重庆)有限公司 | Electronic material glue solution and preparation method thereof |
| CN114213979B (en) * | 2021-11-10 | 2023-09-05 | 中科检测技术服务(重庆)有限公司 | Electronic material glue solution and preparation method thereof |
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| CN110922937B (en) | 2021-12-07 |
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