CN116333675A - Single-component heat-conducting adhesive and preparation method thereof - Google Patents

Single-component heat-conducting adhesive and preparation method thereof Download PDF

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Publication number
CN116333675A
CN116333675A CN202111604253.6A CN202111604253A CN116333675A CN 116333675 A CN116333675 A CN 116333675A CN 202111604253 A CN202111604253 A CN 202111604253A CN 116333675 A CN116333675 A CN 116333675A
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heat
powder
mixing
conducting adhesive
component heat
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万炜涛
任丽
郭呈毅
王红玉
陈田安
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Shenzhen Darbond Interface Materials Co ltd
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Shenzhen Darbond Interface Materials 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
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2296—Oxides; Hydroxides of metals of zinc
    • 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

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention provides a single-component heat-conducting adhesive and a preparation method thereof, belonging to the technical field of heat-conducting adhesives. The raw materials of the single-component heat-conducting adhesive glue comprise 10-90 parts of vinyl-terminated polysiloxane A, 10-90 parts of vinyl-terminated polysiloxane B, 1200-1500 parts of modified heat-conducting insulating powder, 20-30 parts of cross-linking agent, 10-25 parts of VQM resin, 7-10 parts of chain extender, 0.0003-0.0005 part of inhibition agent and 0.0001-0.0002 part of platinum catalyst. The hardness of the adhesive obtained by the invention is obviously improved after solidification, and the adhesive has the characteristics of low thermal resistance and low viscosity.

Description

Single-component heat-conducting adhesive and preparation method thereof
Technical Field
The invention relates to the technical field of heat-conducting adhesives, in particular to a single-component heat-conducting adhesive and a preparation method thereof.
Background
At present, a first-generation semiconductor material silicon wafer is generally adopted for semiconductor components and parts, and is mainly used for electronic products such as computers and the like with large-scale integrated circuits as main technologies; the second generation semiconductor material gallium arsenide wafer and indium phosphide are mainly used for optical display, optical communication, optical storage and other electronic systems based on light emitting devices, and the third generation semiconductor material silicon carbide, gallium nitride, zinc oxide and other wide bandgap semiconductors are used for manufacturing anti-radiation, high-frequency, high-power and high-density integrated electronic devices.
At present, the thermal expansion coefficient of a chip mainly comprising a silicon wafer is about 3 ppm/DEG C, the thermal expansion coefficient of a typical copper cover nickel-plated substrate is about 18 ppm/DEG C, in the flip chip packaging process, a relatively important process parameter-temperature is included, and the thermal expansion coefficient among the chip, the thermal interface material heat-conducting glue and the packaging cover plate can be well matched with the temperature, so that the thermal interface material can achieve a good packaging effect, and the phenomena of poor coverage rate and delamination are avoided. Meanwhile, in the working state of the chip, the packaging body generates temperature change, materials with different thermal expansion coefficients deform at different rates, and the materials with different expansion coefficients can generate thermal-induced mechanical stress in the packaging assembly due to uneven distribution, so that the device is influenced, and therefore, the design of the organic thermal interface material which can be suitable for the chip packaging process and has excellent reliability is extremely important.
For selection of organic Thermal Interface Materials (TIMs) for chip packaging, thermal interface materials generally have typical thermal resistance values of 0.05 to 1.6 (cm) according to relevant literature reports 2 DEG C/W) can be expressed by the following formula,
Figure BDA0003433123990000011
(Prasher et al.,2003)。
BLT is the bonding wire thickness of TIM, K TIM For the thermal conductivity of the TIM, RC1 and RC2 are the thermal contact resistances of the contact surfaces of the TIM. The purpose of thermal design is to reduce RTIM, which can be accomplished by reducing BLT, increasing thermal conductivity, and reducing thermal contact resistance as seen by the above equation. In the practical tooling process, the TIM is required to have good diffusion characteristics, and the gap between the chip and the packaging cover plate is filled, so that the heat dissipation capacity of the device can be ensured.
The organic silicon heat-conducting adhesive is an addition type heat-conducting adhesive, and has excellent high and low temperature resistance (-60-200 ℃), high adhesive strength (3.0-8.0 MPa) and excellent reliability. The thermal interface material heat-conducting adhesive has lower application thickness, generally less than 120 mu m, and the expansion coefficient is about 125 ppm/DEG C, so that the thermal interface material heat-conducting adhesive can meet the matching of the thermal expansion coefficients of other interface materials. Therefore, the heat-conducting adhesive is the best choice of organic thermal interface materials, and can meet the packaging and heat dissipation requirements of electronic components. However, related patent reports of heat conduction adhesive for chip packaging are not yet found at home. Therefore, development of a heat-conducting adhesive which has low viscosity, no defect of a cured thin layer, low thermal resistance and thinner thickness and can meet the requirement of flip chip packaging is needed to solve the problem of domestic chip packaging.
Disclosure of Invention
The invention aims to provide the heat-conducting adhesive glue which has low viscosity, low thermal resistance and thinner thickness and can meet the requirement of flip chip packaging.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a single-component heat-conducting adhesive which is prepared from the following raw materials in parts by weight:
Figure BDA0003433123990000021
the viscosity of the vinyl-terminated polysiloxane A is 5000-10000 cp, and the vinyl content is 0.045-0.072 mmol/g;
the viscosity of the vinyl-terminated polysiloxane B is 500-2000 cp, and the vinyl content is 0.14-0.18 mmol/g.
Further, the preparation method of the modified heat conduction insulating powder comprises the following steps: and mixing the modifier with absolute ethyl alcohol to obtain a mixed solution, mixing the powder to be modified with the mixed solution, and heating to obtain the modified heat-conducting insulating powder.
Further, the modifier comprises one or more of octadecyl trimethoxy silane, hexadecyl trimethoxy silane, dodecyl trimethoxy silane, gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and gamma- (2, 3-epoxypropoxy) propyl triethoxy silane.
Further, the powder to be modified comprises one or more of alumina powder with the particle size of 5-67 mu m, zinc oxide powder with the particle size of 0.5-5 mu m and hexagonal boron nitride powder with the particle size of less than or equal to 45 mu m.
Further, the crosslinking agent comprises side hydrogen silicone oil and/or MQ hydrogen resin, wherein the hydrogen content of the side hydrogen silicone oil is 7-12 mmol/g, and the hydrogen content of the MQ hydrogen resin is 8.5-10.5 mmol/g.
Further, the vinyl content of the VQM resin is 0.18-0.24 mmol/g, and the viscosity is 6000-10000 cp.
Further, the chain extender comprises hydrogen-containing silicone oil containing Si-H terminals; the inhibitor comprises alkynols and/or tetramethyl tetravinyl cyclotetrasiloxane.
The invention provides a preparation method of single-component heat-conducting adhesive, which comprises the following steps:
1) Mixing vinyl-terminated polysiloxane A, vinyl-terminated polysiloxane B, VQM resin and modified heat conducting insulating powder to obtain a first mixture;
2) And mixing the first mixture, the cross-linking agent, the chain extender, the inhibitor and the platinum catalyst to obtain the single-component heat-conducting adhesive.
Further, the conditions for obtaining the first mixture are as follows: the mixing speed is 50-70 rpm, the mixing time is 50-70 min, and the vacuum degree is less than or equal to minus 0.1MPa.
Further, in the step 2), the mixing conditions are as follows: the mixing speed is 10-20 rpm, the mixing time is 10-45 min, and the mixing temperature is 18-25 ℃.
The invention has the beneficial effects that:
the single-component heat-conducting adhesive prepared by the invention has the characteristics of ensuring high shearing force and low stress, has the thermal expansion coefficient of 102 ppm/DEG C, and can be well matched with TIM materials. And secondly, the single-component heat-conducting adhesive disclosed by the invention has low viscosity and high thixotropic property, is suitable for a high-efficiency dispensing process, and has low thermal resistance, so that the reliability of a device can be well ensured.
Detailed Description
The invention provides a single-component heat-conducting adhesive which is prepared from the following raw materials in parts by weight:
Figure BDA0003433123990000041
the viscosity of the vinyl-terminated polysiloxane A is 5000-10000 cp, and the vinyl content is 0.045-0.072 mmol/g;
the viscosity of the vinyl-terminated polysiloxane B is 500-2000 cp, and the vinyl content is 0.14-0.18 mmol/g.
In the invention, the addition amount of the vinyl-terminated polysiloxane A is 10 to 90 parts by weight, preferably 20 to 80 parts by weight, and more preferably 30 to 60 parts by weight; the viscosity of the vinyl-terminated polysiloxane A is preferably 6000-9000 cp, and the vinyl content is preferably 0.050-0.060 mmol/g.
In the present invention, the vinyl-terminated polysiloxane B is added in an amount of 10 to 90 parts by weight, preferably 20 to 80 parts by weight, and more preferably 30 to 60 parts by weight; the viscosity of the vinyl-terminated polysiloxane B is preferably 600-1800 cp, and the vinyl content is preferably 0.15-0.17 mmol/g.
In the invention, the modified heat-conducting insulating powder is added in an amount of 1200 to 1500 parts by weight, preferably 1300 to 1400 parts by weight, and more preferably 1350 parts by weight.
In the invention, the preparation method of the modified heat conduction insulating powder comprises the following steps: and mixing the modifier with absolute ethyl alcohol to obtain a mixed solution, mixing the powder to be modified with the mixed solution, and heating to obtain the modified heat-conducting insulating powder.
In the invention, the preparation method of the modified heat conduction insulating powder preferably comprises the following steps: mixing modifier and absolute ethyl alcohol to obtain a mixed solution, spraying the mixed solution onto powder to be modified by adopting a dry modification and pneumatic spraying mode, rapidly mixing at the rotating speed of 1000-2000 rpm, and drying the modified powder at the temperature of 50-80 ℃ for later use.
In the present invention, the modifier comprises one or more of octadecyl trimethoxysilane, hexadecyl trimethoxysilane, dodecyl trimethoxysilane, gamma- (2, 3-glycidoxy) propyl trimethoxysilane and gamma- (2, 3-glycidoxy) propyl triethoxysilane, preferably octadecyl trimethoxysilane, hexadecyl trimethoxysilane and dodecyl trimethoxysilane.
In the present invention, the powder to be modified contains one or more of alumina powder having a particle diameter of 5 to 67 μm, zinc oxide powder having a particle diameter of 0.5 to 5 μm, and hexagonal boron nitride powder having a particle diameter of 45 μm or less, preferably alumina powder having a particle diameter of 5 to 67 μm and/or zinc oxide powder having a particle diameter of 0.5 to 5 μm.
In the present invention, the particle diameter of the alumina powder is preferably 10 to 50. Mu.m, more preferably 20 to 40. Mu.m; the particle diameter of the zinc oxide powder is preferably 1 to 3. Mu.m, more preferably 2. Mu.m; the particle size of the hexagonal boron nitride powder is preferably less than or equal to 40 mu m.
In the invention, the mass volume ratio of the modifier to be modified to the powder to be modified to the absolute ethyl alcohol is 9-15 g: 900-1200 g:100mL, preferably 10-11 g: 1000-1100 g:100mL.
In the present invention, the powder to be modified is further dried at 50 to 80℃for 2 to 4 hours, preferably at 80℃for 3 hours, before modification.
In the present invention, the heating temperature is 80 to 120 ℃, preferably 120 ℃.
In the present invention, the crosslinking agent is added in an amount of 20 to 30 parts by weight, preferably 25 parts by weight. In the present invention, the crosslinking agent comprises a side hydrogen silicone oil and/or an MQ hydrogen resin, the side hydrogen silicone oil having a hydrogen content of 7 to 12mmol/g, preferably 8 to 10mmol/g; the hydrogen content of the MQ hydrogen-containing resin is 8.5-10.5 mmol/g, preferably 9-10 mmol/g.
In the present invention, the VQM resin is added in an amount of 10 to 25 parts by weight, preferably 15 to 20 parts by weight, and more preferably 18 parts by weight. In the invention, the vinyl content of the VQM resin is 0.18-0.24 mmol/g, and the viscosity is 6000-10000 cp; preferably, the vinyl content of the VQM resin is 0.20 to 0.22mmol/g and the viscosity is 7000 to 9000cp.
In the invention, the addition amount of the chain extender is 7-10 parts by weight, preferably 8-9 parts by weight; the chain extender comprises a hydrogen-containing silicone oil containing Si-H terminals, preferably a hydrogen-containing silicone oil having a hydrogen content of 0.16 to 0.18mmol/g.
In the present invention, the inhibitor is added in an amount of 0.0003 to 0.0005 parts by weight, preferably 0.0004 parts by weight; the inhibitor comprises alkynols and/or tetramethyl tetravinyl cyclotetrasiloxane, preferably tetramethyl tetravinyl cyclotetrasiloxane.
In the present invention, the platinum catalyst is added in an amount of 0.0001 to 0.0002 parts by weight, preferably 0.0001 parts by weight.
The invention provides a preparation method of single-component heat-conducting adhesive, which comprises the following steps:
1) Mixing vinyl-terminated polysiloxane A, vinyl-terminated polysiloxane B, VQM resin and modified heat conducting insulating powder to obtain a first mixture;
2) And mixing the first mixture, the cross-linking agent, the chain extender, the inhibitor and the platinum catalyst to obtain the single-component heat-conducting adhesive.
In the invention, the conditions for obtaining the first mixture are as follows: the mixing speed is 50-70 rpm, the mixing time is 50-70 min, and the vacuum degree is less than or equal to minus 0.1MPa; preferably, the mixing speed is 55-65 rpm, the mixing time is 55-65 min, and the vacuum degree is-0.1 MPa; further preferably, the mixing speed is 60rpm, the mixing time is 60min, and the vacuum degree is-0.10 MPa.
In the present invention, in the step 2), the mixing conditions are as follows: the mixing speed is 10-20 rpm, the mixing time is 10-45 min, and the mixing temperature is 18-25 ℃; preferably, the mixing speed is 12-18 rpm, the mixing time is 20-35 min, and the mixing temperature is 20-24 ℃; further preferably, the speed of mixing is 15rpm, the time of mixing is 25 minutes, and the temperature of mixing is 22 ℃.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
The preparation method of the heat-conducting adhesive comprises the following steps:
1) Modification treatment of heat conduction insulating powder: 1000g of alumina powder with the particle size of 5 mu m, 10 mu m and 20 mu m and zinc oxide powder with the particle size of 1 mu m (the mass ratio of the four is 4.5:4.5:6.6:1) are weighed and dried for 3 hours at 100 ℃, 11g of hexadecyl trimethoxy silane and 100mL of absolute ethyl alcohol are weighed and mixed uniformly, then a high-speed heating mixer is adopted for powder modification at 120 ℃, a continuous spraying mode linked with the powder feeding speed is adopted to improve the coating rate of the powder, and finally the powder is dried for standby.
2) 10g of vinyl silicone oil with viscosity of 10000cp, 90g of vinyl silicone oil with viscosity of 2000cp, 15g of VQM resin with viscosity of 10000cp and 1500g of modified heat-conducting insulating powder in the step 1) are weighed, and stirred for 60min under the conditions that the rotating speed is 60rpm and the vacuum degree is-0.1 MPa.
3) Then adding 30g of cross-linking agent, 9g of chain extender and 0.0003g of inhibitor in turn, continuously stirring for 30min under the cooling circulation water at 20 ℃, finally adding 0.0001g of platinum catalyst, and stirring for 15min at 15 rpm. Wherein the cross-linking agent is side hydrogen-containing silicone oil with the hydrogen content of 10mmol/g, the chain extender is hydrogen-containing silicone oil with the hydrogen content of 0.18mmol/g, and the inhibitor is tetramethyl tetravinyl cyclotetrasiloxane.
Example 2
The preparation method of the heat-conducting adhesive comprises the following steps:
1) 1000g of alumina powder with the particle size of 5 mu m, 10 mu m and 20 mu m and zinc oxide powder with the particle size of 1 mu m (the mass ratio of the four is 4.5:4.5:6.6:1) are weighed and dried for 3 hours at 100 ℃, 11g of hexadecyl trimethoxy silane and 100mL of absolute ethyl alcohol are weighed and mixed uniformly, then a high-speed heating mixer is adopted for powder modification at 120 ℃, a continuous spraying mode linked with the powder feeding speed is adopted to improve the coating rate of the powder, and finally the powder is dried for standby.
2) 90g of vinyl silicone oil with viscosity of 10000cp, 10g of vinyl silicone oil with viscosity of 2000cp, 25g of VQM resin with viscosity of 10000cp and 1200g of modified heat-conducting insulating powder in the step 1) are weighed, and stirred for 60min under the conditions that the rotating speed is 60rpm and the vacuum degree is minus 0.1MPa.
3) Then 20g of cross-linking agent, 7g of chain extender and 0.0003g of inhibitor are added in sequence, stirring is continued under cooling circulation water at 18 ℃ for 30min, finally 0.0001g of platinum catalyst is added, and stirring is carried out at 15rpm for 15min. Wherein the cross-linking agent is MQ hydrogen-containing resin with hydrogen content of 8.5mmol/g, the chain extender is terminal hydrogen-containing silicone oil with hydrogen content of 0.16mmol/g, and the inhibitor is tetramethyl tetravinyl cyclotetrasiloxane.
Example 3
The preparation method of the heat-conducting adhesive comprises the following steps:
1) Modification treatment of heat conduction insulating powder: 1000g of alumina powder with the particle size of 5 mu m, 10 mu m and 20 mu m (the mass ratio of the three is 1:1.2:1.7) is weighed and dried for 3 hours at the temperature of 100 ℃, 11g of hexadecyl trimethoxy silane and 100mL of absolute ethyl alcohol are weighed and mixed uniformly, then a high-speed heating mixer is adopted to carry out powder modification at the temperature of 120 ℃, a continuous spraying mode linked with the feeding speed of the powder is adopted to improve the coating rate of the powder, and finally the powder is dried for later use.
2) 80g of vinyl silicone oil with the viscosity of 5000cp, 20g of vinyl silicone oil with the viscosity of 500cp, 15g of VQM resin with the viscosity of 10000cp and 1500g of modified heat-conducting insulating powder in the step 1) are weighed, and stirred for 60min under the conditions of the rotating speed of 60rpm and the vacuum degree of-0.1 MPa.
3) Then 23g of cross-linking agent, 9g of chain extender and 0.0004g of alkynol inhibitor are added in turn, stirring is continued under cooling circulation water at 22 ℃ for 30min, finally 0.0001g of platinum catalyst is added, and stirring is carried out at 15rpm for 15min. Wherein the cross-linking agent is MQ hydrogen-containing resin with the hydrogen content of 10mmol/g, and the chain extender is terminal hydrogen-containing silicone oil with the hydrogen content of 0.16 mmol/g.
Example 4
The preparation method of the heat-conducting adhesive comprises the following steps:
1) Modification treatment of heat conduction insulating powder: 1000g of alumina powder with the particle size of 5 mu m and 10 mu m and the alumina powder with the particle size of 2 mu m (the mass ratio of the alumina powder to the alumina powder is 3:9.1:1) are weighed, the alumina powder is dried for 3 hours at 100 ℃, the body is dried for 3 hours at 100 ℃, 11g of hexadecyl trimethoxy silane and 100mL of absolute ethyl alcohol are weighed and uniformly mixed, then a high-speed heating mixer is adopted for powder modification at 120 ℃, a continuous spraying mode linked with the feeding speed of the powder is adopted, the coating rate of the powder is improved, and finally the powder is dried for later use.
2) 90g of vinyl silicone oil with the viscosity of 5000cp, 10g of vinyl silicone oil with the viscosity of 2000cp, 20g of VQM resin with the viscosity of 10000cp and 1500g of modified heat-conducting insulating powder in the step 1) are weighed, and stirred for 60min under the conditions of the rotating speed of 60rpm and the vacuum degree of-0.1 MPa.
3) Then, 23g of a crosslinking agent, 9g of a chain extender and 0.0003g of an inhibitor are sequentially added, stirring is continued under cooling circulation water at 25 ℃ for 30min, and finally, 0.0001g of a platinum catalyst is added, and stirring is carried out at 15rpm for 15min. Wherein the cross-linking agent is side hydrogen-containing silicone oil with the hydrogen content of 12mmol/g, the chain extender is terminal hydrogen-containing silicone oil with the hydrogen content of 0.16mmol/g, and the inhibitor is alkynol.
Example 5
The preparation method of the heat-conducting adhesive comprises the following steps:
1) Modification treatment of heat conduction insulating powder: 1000g of alumina powder with the particle size of 5 mu m, 10 mu m and 20 mu m (the mass ratio of the three is 1:1.2:1.7) is weighed and dried for 3 hours at the temperature of 100 ℃, 10g of hexadecyl trimethoxy silane and 100mL of absolute ethyl alcohol are weighed and mixed uniformly, then a high-speed heating mixer is adopted for powder modification at the temperature of 120 ℃, a continuous spraying mode linked with the feeding speed of the powder is adopted to improve the coating rate of the powder, and finally the powder is dried for later use.
2) 40g of vinyl silicone oil with viscosity of 10000cp, 20g of vinyl silicone oil with viscosity of 2000cp, 40g of VQM resin with viscosity of 6000cp and 1300g of modified heat-conducting insulating powder in the step 1) are weighed, and stirred for 60min under the conditions of rotating speed of 60rpm and vacuum degree of-0.1 MPa.
3) Then 25g of cross-linking agent, 7g of chain extender and 0.0004g of tetramethyl tetravinyl cyclotetrasiloxane inhibitor are added in sequence, stirring is continued for 30min under cooling circulation water at 18 ℃, finally 0.0001g of platinum catalyst is added, and stirring is carried out for 15min at 15 rpm. Wherein the cross-linking agent is MQ hydrogen-containing resin with hydrogen content of 10.5mmol/g, and the chain extender is terminal hydrogen-containing silicone oil with hydrogen content of 0.18mmol/g.
The heat conductive adhesive obtained in examples 1 to 5 was cured at 150℃for 60 minutes, the heat conductivity of the heat conductive adhesive was measured using ASTM D5470-06, the hardness of the heat conductive adhesive was measured using Shore A durometer, and the adhesive strength of the heat conductive adhesive was measured using ASTM D3528. The thermally conductive adhesive was tested for elongation and tensile strength using ASTM D412-16. The viscosity of the heat-conducting adhesive is tested by a Hark rheometer, and the thermal impedance of the heat-conducting adhesive is tested by a Rayleigh collar LW-9387 thermal resistance meter. The thickness (BLT) of the thin layer after curing at a certain pressure and area was measured using a profiler and the results are shown in table 1 below.
Table 1 table of performance test of heat conductive adhesive obtained in examples 1 to 5
Figure BDA0003433123990000091
Figure BDA0003433123990000101
As can be seen from the above examples, the present invention provides a single-component heat-conducting adhesive and a method for preparing the same. The performance test of the cured heat-conducting adhesive is carried out to obtain the heat-conducting adhesive with the heat conductivity coefficient of 1.68W/mK and the heat resistance as low as 0.046℃ in 2 and/W. The single-component heat-conducting adhesive has low viscosity and high thixotropic property, is suitable for a high-efficiency dispensing process, and has low thermal resistance and can well ensure the reliability of devices.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.

Claims (10)

1. The single-component heat-conducting adhesive is characterized by being prepared from the following raw materials in parts by weight:
Figure FDA0003433123980000011
the viscosity of the vinyl-terminated polysiloxane A is 5000-10000 cp, and the vinyl content is 0.045-0.072 mmol/g;
the viscosity of the vinyl-terminated polysiloxane B is 500-2000 cp, and the vinyl content is 0.14-0.18 mmol/g.
2. The single-component heat-conducting adhesive glue according to claim 1, wherein the preparation method of the modified heat-conducting insulating powder is as follows: and mixing the modifier with absolute ethyl alcohol to obtain a mixed solution, mixing the powder to be modified with the mixed solution, and heating to obtain the modified heat-conducting insulating powder.
3. The single-component heat-conducting adhesive according to claim 2, wherein the modifier comprises one or more of octadecyl trimethoxysilane, hexadecyl trimethoxysilane, dodecyl trimethoxysilane, gamma- (2, 3-glycidoxy) propyl trimethoxysilane and gamma- (2, 3-glycidoxy) propyl triethoxysilane.
4. The single-component heat-conducting adhesive glue according to claim 2, wherein the powder to be modified comprises one or more of alumina powder with a particle size of 5-67 μm, zinc oxide powder with a particle size of 0.5-5 μm and hexagonal boron nitride powder with a particle size of less than or equal to 45 μm.
5. The single-component heat-conducting adhesive according to any one of claims 1 to 4, wherein the crosslinking agent comprises a side hydrogen silicone oil and/or an MQ hydrogen resin, the hydrogen content of the side hydrogen silicone oil is 7 to 12mmol/g, and the hydrogen content of the MQ hydrogen resin is 8.5 to 10.5mmol/g.
6. The single-component heat-conducting adhesive according to claim 5, wherein the VQM resin has a vinyl content of 0.18-0.24 mmol/g and a viscosity of 6000-10000 cp.
7. The one-component heat conductive adhesive paste according to claim 1 or 2 or 3 or 4 or 6, wherein the chain extender comprises a Si-H terminated hydrogen containing silicone oil; the inhibitor comprises alkynols and/or tetramethyl tetravinyl cyclotetrasiloxane.
8. The method for preparing the single-component heat-conducting adhesive according to any one of claims 1 to 7, which is characterized by comprising the following steps:
1) Mixing vinyl-terminated polysiloxane A, vinyl-terminated polysiloxane B, VQM resin and modified heat conducting insulating powder to obtain a first mixture;
2) And mixing the first mixture, the cross-linking agent, the chain extender, the inhibitor and the platinum catalyst to obtain the single-component heat-conducting adhesive.
9. The method for preparing the single-component heat-conducting adhesive according to claim 8, wherein the conditions for obtaining the first mixture are as follows: the mixing speed is 50-70 rpm, the mixing time is 50-70 min, and the vacuum degree is less than or equal to minus 0.1MPa.
10. The method for preparing a single-component heat-conducting adhesive according to claim 9, wherein in the step 2), the mixing conditions are as follows: the mixing speed is 10-20 rpm, the mixing time is 10-45 min, and the mixing temperature is 18-25 ℃.
CN202111604253.6A 2021-12-24 2021-12-24 Single-component heat-conducting adhesive and preparation method thereof Pending CN116333675A (en)

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Application Number Priority Date Filing Date Title
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Publication Number Publication Date
CN116333675A true CN116333675A (en) 2023-06-27

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