CN111154227A - High-thermal-conductivity insulating layer material, metal substrate and preparation method - Google Patents
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Abstract
The application relates to a high-thermal-conductivity insulating layer material, a metal substrate and a preparation method, wherein the preparation method comprises the following steps: performing photo/electrochemical activation treatment on the inorganic composite micro-nano filler by glow discharge plasma, then treating the inorganic composite micro-nano filler by a coupling agent, and then performing spray drying to obtain a pretreated inorganic composite micro-nano filler; dissolving the pretreated inorganic composite micro-nano filler in a solution containing epoxy resin and a curing agent to obtain a resin glue solution; curing the resin glue solution to form the high-heat-conductivity insulating layer material; the inorganic composite micro-nano filler is compound powder of heat-conducting filler and mica powder; the high-thermal-conductivity insulating layer material prepared by the invention has beneficial insulating property and thermal conductivity, can meet the requirement of heat dissipation of high-power components, and can ensure the lasting and safe operation of electrical and electronic equipment.
Description
Technical Field
The application belongs to the technical field of electronic materials, and particularly relates to a high-thermal-conductivity insulating layer material, a metal substrate and a preparation method.
Background
In recent years, in the field of electronics and electronics, microelectronic packaging technology has been rapidly developed, electronic devices have been miniaturized and miniaturized, and heat dissipation has become a significant problem as more and more components are mounted on a Printed Circuit Board (PCB). For electronic components, the reliability is reduced by 10% when the temperature is increased by 2 ℃; when the temperature is increased by 50 ℃, the service life of the component is only 1/6 originally. Therefore, in order to ensure the performance of the components, such as the lifetime, stability, and reliability, the problem of heat dissipation must be solved.
Metal substrates such as metal-based copper clad laminate carrying electronic components are widely applied to the fields of LED illumination, TV, intelligent power devices, inverters, electric motors, power supplies and the like, however, for high-power heat sources, the heat productivity of the power components is too high, so that the problems of component service life and safety are directly caused, and higher requirements are provided for the heat dissipation capacity of the metal substrates. However, the conventional metal substrate is mainly formed by coating a Polyimide (PI) or Polyester (PE) film with a copper foil, and is widely used in the fields of telecommunications and LED lighting, but since PI or PE is an insulating plastic, its heat conduction and heat dissipation performance are poor, generally 0.2W/m · K, and meanwhile, since the conventional metal substrate is insulated and heat dissipation through an insulating layer material, the method is: untreated inorganic powder such as aluminum oxide, silicon oxide, aluminum nitride, boron nitride and silicon nitride is directly added into the resin glue solution, and then curing treatment is carried out to form a high-heat-conductivity insulating layer, and the insulating layer material cannot meet the heat-conduction and heat-dissipation requirements of high-power electronic equipment such as the conventional LED, a power supply and the like, so that the application and development of the insulating layer material are limited.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the high-thermal-conductivity insulating layer material, the metal substrate and the preparation method are provided for solving the technical problem that the existing insulating layer material for the metal substrate cannot meet the thermal conduction and heat dissipation requirements of high-power electronic equipment.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of a high-thermal-conductivity insulating layer material comprises the following steps:
performing optical/electrochemical activation treatment on the inorganic composite micro-nano filler by glow discharge plasma, modifying the inorganic composite micro-nano filler by a coupling agent, and performing spray drying to obtain a pretreated inorganic composite micro-nano filler;
dissolving the pretreated inorganic composite micro-nano filler in a solution containing epoxy resin and a curing agent to obtain a resin glue solution;
curing the resin glue solution to form the high-heat-conductivity insulating layer material;
the inorganic composite micro-nano filler is compound powder of a heat-conducting filler and mica powder, the heat-conducting filler is at least one of aluminum oxide, boron nitride, aluminum nitride, silicon oxide and silicon nitride, and the mass of the mica powder is 1-5 wt% of the total mass of the inorganic composite micro-nano filler.
Preferably, the high thermal conductivity insulating layer material comprises the following components in parts by weight: 100 parts of epoxy resin, 4-8 parts of curing agent, and 700 parts of inorganic composite micro-nano filler, wherein the mass of the coupling agent is 1-5 wt% of the mass of the inorganic composite micro-nano filler.
Preferably, the heat-conducting filler is in a spherical structure with different particle sizes, the inorganic composite micro-nano filler compounded by the heat-conducting filler and mica powder has a closest packing structure, and the median particle size D50 of the heat-conducting filler is preferably 0.5-20 μm; the particle size range of the mica powder is preferably 600 meshes-5000 meshes.
Preferably, the coupling agent is a silane coupling agent and an aluminate coupling agent in a mass ratio of 1-3:1, and the step of modification treatment is preferably to add the silane coupling agent for modification treatment and then add the aluminate coupling agent for modification treatment.
Preferably, the curing agent is at least one of dicyandiamide, polyamide, dimer acid-based polyamide, 4-diaminodiphenyl sulfone, methyl tetrahydrophthalic anhydride and methyl hexahydrophthalic anhydride.
Preferably, the epoxy resin is bisphenol A type epoxy resin or bisphenol F type epoxy resin.
Preferably, the resin glue solution is fully defoamed before being cured, and the curing method is preferably to cure the resin glue solution for 2 to 6 hours at 50 to 100 ℃ and then cure the resin glue solution for 1 to 3 hours at 150 to 200 ℃.
Preferably, the preparation method of the pretreated inorganic composite micro-nano filler comprises the following steps:
1) humidifying the inorganic composite micro-nano filler;
2) placing the humidified inorganic composite micro-nano filler in a plasma generator, applying voltage to generate glow discharge plasma, and performing optical/electrochemical activation treatment on the inorganic composite micro-nano filler;
3) mixing the activated inorganic composite micro-nano filler, a coupling agent and water to prepare slurry, and then carrying out spray drying treatment on the slurry to obtain the pretreated inorganic composite micro-nano filler.
Preferably, the conditions of the photo/electrochemical activation treatment are: the discharge power is 50W-500W, the discharge voltage is 3 kV-30 kV, the temperature is 80-120 ℃, and the treatment time is 0.5-10 h.
Preferably, the humidification treatment is spray humidification treatment, the spray pressure is 2-5 MPa, the flow rate is 0.1-0.5L/min, the temperature is 80-100 ℃, and the humidification treatment time is 0.5-1 h.
Preferably, the temperature of the spray drying treatment is 100-150 ℃, and the rotating speed of the spray drying atomizing disc is 750r/min-2000 r/min.
The invention also provides the high-thermal-conductivity insulating layer material prepared by the method and a metal substrate comprising the high-thermal-conductivity insulating layer material.
The invention has the beneficial effects that:
the invention discloses a high heat conduction insulating layer material for a metal substrate, which is characterized in that composite powder of heat conduction filler and mica powder, which are sequentially subjected to plasma light/electrochemical treatment and coupling agent modification, is added into a solution of epoxy resin and a curing agent, and finally, the composite powder is cured to form an insulating layer material with excellent heat conduction performance and electrical insulating performance, furthermore, the heat conduction filler is adopted to be a spherical structure with different particle sizes, the inorganic composite micro-nano filler compounded by the heat conduction filler and the mica powder has a closest packing structure to form a heat conduction network chain so as to further improve the insulating performance and the heat conduction performance of the insulating layer material, the method has simple processing technology and good universality, the prepared high heat conduction and high insulation material can meet the heat dissipation requirement of high-power components, can ensure the durable and safe operation of electric and electronic equipment, and can enhance the heat dissipation capability and reduce the insulation thickness when being applied to the electric and electronic, miniaturization and reliability of the electric and electronic equipment can be promoted.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
Example 1
The embodiment provides a high-thermal-conductivity insulating layer material for a metal substrate and a preparation method thereof, and the preparation method comprises the following steps:
the preparation method comprises the following steps:
1) placing spherical alumina and mica powder in a drying oven, drying at 100 ℃ for 2 hours, weighing corresponding amount, and uniformly mixing to obtain inorganic composite micro-nano filler; drying the epoxy resin and the curing agent in a drying oven at 60 ℃ for 5-10 minutes to reduce the viscosity;
2) adding the dried inorganic composite micro-nano filler into an atomizing chamber with high-speed dispersion, and carrying out humidification treatment for 1h, wherein the pressure of an atomizing nozzle is 2MPa, the flow rate is 0.1L/min, and the temperature is 80 ℃;
3) on a low-temperature plasma generator treatment platform, adding voltage to the inorganic composite micro-nano filler subjected to humidification treatment to generate glow discharge plasma, and carrying out photo/electrochemical activation treatment on the humidification treatment, wherein: the discharge voltage is 3kV, the discharge power is 50W, the temperature is 80 ℃, and the discharge time is 10 h;
4) adding a silane modifier and water into the activated inorganic composite micro-nano filler, mixing and stirring the mixture for 5-10min by a stirrer, adding an aluminate coupling agent, mixing and stirring the mixture to prepare a slurry, and then sending the slurry into a spray dryer for spray drying to obtain a pretreated inorganic composite micro-nano filler; wherein: the treatment temperature is 100 ℃, and the rotation speed of an atomizing disc is 750 r/min; the mass ratio of the silane coupling agent to the aluminate coupling agent is 2: 1;
5) weighing epoxy resin, a curing agent and a solvent, mixing and fully stirring the mixture, adding the pretreated inorganic composite micro-nano filler, and fully stirring again to obtain a resin glue solution;
6) placing the resin glue solution in a KQ2200 type ultrasonic cleaner for oscillation and defoaming, and placing the resin glue solution in a planetary vacuum stirring defoaming machine for defoaming again after oscillation;
7) pouring the resin glue solution after the defoaming treatment into a mould, and putting the mould into a drying oven for heating and curing, wherein the curing treatment method comprises the following steps: curing at 70 deg.C for 4 hr, curing at 170 deg.C for 2 hr, cooling for 10 hr, and taking out.
The thermal conductivity of the insulating layer material prepared in the embodiment is 4.8W/(m.K), and the breakdown field strength is 43.45 kV/mm; wherein: the breakdown field strength is measured by using a BTF-038-50kV voltage breakdown tester, and the adopted test standard is GB/T1408.1-2006; the DRL-III thermal conductivity coefficient tester for the thermal conductivity test has the test standard of ASTM D5470-2006 and the test method of the transient plane heat source method.
Example 2
The embodiment provides a high-thermal-conductivity insulating layer material for a metal substrate and a preparation method thereof, and the preparation method comprises the following steps:
the preparation method comprises the following steps:
1) placing spherical alumina and mica powder in a drying oven, drying at 100 deg.C for 2 hr, weighing corresponding amount, mixing uniformly, and mixing inorganic composite micro-nano filler; drying the epoxy resin and the curing agent in a drying oven at 60 ℃ for 5-10 minutes to reduce the viscosity;
2) adding the dried inorganic composite micro-nano filler into an atomizing chamber with high-speed dispersion, and carrying out humidification treatment for 0.5h, wherein the pressure of an atomizing nozzle is 5MPa, the flow rate is 0.5L/min, and the temperature is 100 ℃;
3) on a low-temperature plasma generator processing platform, adding voltage to generate glow discharge plasma, and carrying out optical/electrochemical activation processing on the inorganic composite micro-nano filler, wherein: the discharge voltage is 15kV, the discharge power is 100W, the temperature is 100 ℃, and the discharge time is 5 h;
4) adding a silane modifier and water into the activated inorganic composite micro-nano filler, mixing and stirring the mixture for 5-10min by a stirrer, adding an aluminate coupling agent, mixing and stirring the mixture to prepare a slurry, and then sending the slurry into a spray dryer for spray drying to obtain a pretreated inorganic composite micro-nano filler; wherein: the treatment temperature is 150 ℃, and the rotating speed of an atomizing disc is 2000 r/min; the mass ratio of the silane coupling agent to the aluminate coupling agent is 1: 1;
5) weighing epoxy resin, a curing agent and a solvent, mixing and fully stirring the mixture, adding the pretreated inorganic composite micro-nano filler, and fully stirring again to obtain a resin glue solution;
6) placing the resin glue solution in a KQ2200 type ultrasonic cleaner for oscillation and defoaming, and placing the resin glue solution in a planetary vacuum stirring defoaming machine for defoaming again after oscillation;
7) pouring the resin glue solution after the defoaming treatment into a mould, and putting the mould into a drying oven for heating and curing, wherein the curing treatment method comprises the following steps: curing at 50 deg.C for 6 hr, curing at 200 deg.C for 1 hr, cooling for 10 hr, and taking out.
The thermal conductivity of the insulating layer material prepared in this example was 4.2W/(m.K), the breakdown field strength was 39.11kV/mm, and the test method was the same as in example 1.
Example 3
The embodiment provides a high-thermal-conductivity insulating layer material for a metal substrate and a preparation method thereof, and the preparation method comprises the following steps:
the preparation method comprises the following steps:
1) placing spherical alumina and mica powder in a drying oven, drying at 100 deg.C for 2 hr, weighing corresponding amount, mixing uniformly, and mixing inorganic composite micro-nano filler; drying the epoxy resin and the curing agent in a drying oven at 60 ℃ for 5-10 minutes to reduce the viscosity;
2) adding the dried inorganic composite micro-nano filler into an atomizing chamber with high-speed dispersion, and carrying out humidification treatment for 0.5h, wherein the pressure of an atomizing nozzle is 5MPa, the flow rate is 0.5L/min, and the temperature is 100 ℃;
3) on the inorganic composite micro-nano filler of humidification processing on low temperature plasma generator processing platform, add voltage and produce glow discharge plasma, carry out photoelectrochemical activation processing to inorganic composite micro-nano filler cooking, wherein: the discharge voltage is 30kV, the discharge power is 500W, the temperature is 120 ℃, and the discharge time is 0.5 h;
4) adding a silane modifier and water into the activated inorganic composite micro-nano filler, mixing and stirring the mixture for 5-10min by a stirrer, adding an aluminate coupling agent, mixing and stirring the mixture to prepare a slurry, and then sending the slurry into a spray dryer for spray drying to obtain a pretreated inorganic composite micro-nano filler; wherein: the treatment temperature is 120 ℃, and the rotating speed of an atomizing disc is 1000 r/min; the mass ratio of the silane coupling agent to the aluminate coupling agent is 3: 1;
5) weighing epoxy resin, a curing agent and a solvent, mixing and fully stirring the mixture, adding the pretreated inorganic composite micro-nano filler, and fully stirring again to obtain a resin glue solution;
6) placing the resin glue solution in a KQ2200 type ultrasonic cleaner for oscillation and defoaming, and placing the resin glue solution in a planetary vacuum stirring defoaming machine for defoaming again after oscillation;
7) pouring the resin glue solution after the defoaming treatment into a mould, and putting the mould into a drying oven for heating and curing, wherein the curing treatment method comprises the following steps: curing at 100 deg.C for 2 hr, curing at 150 deg.C for 3 hr, cooling for 10 hr, and taking out.
The thermal conductivity of the insulating layer material prepared in this example was 5.5W/(m.K), the breakdown field strength was 38.15kV/mm, and the test method was the same as in example 1.
In light of the foregoing description of the preferred embodiments according to the present application, it is to be understood that various changes and modifications may be made without departing from the spirit and scope of the invention. The technical scope of the present application is not limited to the contents of the specification, and must be determined according to the scope of the claims.
Claims (10)
1. The preparation method of the high-thermal-conductivity insulating layer material is characterized by comprising the following steps of:
performing optical/electrochemical activation treatment on the inorganic composite micro-nano filler by glow discharge plasma, modifying the inorganic composite micro-nano filler by a coupling agent, and performing spray drying to obtain a pretreated inorganic composite micro-nano filler;
dissolving the pretreated inorganic composite micro-nano filler in a solution containing epoxy resin and a curing agent to obtain a resin glue solution;
curing the resin glue solution to form the high-heat-conductivity insulating layer material;
the inorganic composite micro-nano filler is compound powder of a heat-conducting filler and mica powder, the heat-conducting filler is at least one of aluminum oxide, boron nitride, aluminum nitride, silicon oxide and silicon nitride, and the mass of the mica powder is 1-5 wt% of the total mass of the inorganic composite micro-nano filler.
2. The preparation method of the high thermal conductivity insulating layer material according to claim 1, wherein the high thermal conductivity insulating layer material comprises the following components in parts by weight: 100 parts of epoxy resin, 4-8 parts of curing agent, and 700 parts of inorganic composite micro-nano filler, wherein the mass of the coupling agent is 1-5 wt% of the mass of the inorganic composite micro-nano filler.
3. The preparation method of the high thermal conductivity insulating layer material according to claim 1 or 2, wherein the thermal conductive filler is a spherical structure with different particle sizes, the inorganic composite micro-nano filler compounded by the thermal conductive filler and mica powder has a closest packing structure, and the median particle size D50 of the thermal conductive filler is preferably 0.5 μm to 20 μm; the particle size range of the mica powder is preferably 600 meshes-5000 meshes.
4. The preparation method of the high thermal conductivity insulating layer material according to any one of claims 1 to 3, wherein the coupling agent is a silane coupling agent and an aluminate coupling agent in a mass ratio of 1-3:1, and the modifying treatment is preferably carried out by adding the silane coupling agent for modification and then adding the aluminate coupling agent for modification.
5. The method for preparing a material of an insulating layer with high thermal conductivity according to any one of claims 1 to 4, wherein the curing agent is at least one of dicyandiamide, polyamide, dimer acid-based polyamide, 4-diaminodiphenyl sulfone, methyl tetrahydrophthalic anhydride and methyl hexahydrophthalic anhydride.
6. The preparation method of the material for the high thermal conductive insulating layer according to any one of claims 1 to 5, wherein the resin glue solution is fully defoamed before being cured, and preferably, the curing treatment method comprises curing at 50 ℃ to 100 ℃ for 2 to 6 hours, and then curing at 150 ℃ to 200 ℃ for 1 to 3 hours.
7. The preparation method of the high thermal conductivity insulating layer material according to any one of claims 1 to 6, wherein the preparation method of the pretreated inorganic composite micro-nano filler comprises the following steps:
1) humidifying the inorganic composite micro-nano filler;
2) placing the humidified inorganic composite micro-nano filler in a plasma generator, applying voltage to generate glow discharge plasma, and performing optical/electrochemical activation treatment on the inorganic composite micro-nano filler;
3) mixing the activated inorganic composite micro-nano filler, a coupling agent and water to prepare slurry, and then carrying out spray drying treatment on the slurry to obtain the pretreated inorganic composite micro-nano filler.
8. The method for preparing the high thermal conductivity insulating layer material according to claim 7, wherein the conditions of the photo/electrochemical activation treatment are as follows: the discharge power is 50W-500W, the discharge voltage is 3 kV-30 kV, the temperature is 80-120 ℃, and the treatment time is 0.5-10 h; the humidification treatment is preferably spray humidification treatment, and the conditions of the spray humidification treatment are preferably as follows: the spraying pressure is 2-5 MPa, the flow is 0.1-0.5L/min, the temperature is 80-100 ℃, and the humidifying treatment time is 0.5-1 h; the conditions of the spray drying treatment are preferably: the temperature is 100-150 ℃, and the rotating speed of the spray drying atomizing disc is 750r/min-2000 r/min.
9. A high thermal conductive insulating layer material prepared by the method of any one of claims 1 to 8.
10. A metal substrate comprising the high thermal conductive insulating layer material of claim 9.
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| CN201911370127.1A CN111154227A (en) | 2019-12-26 | 2019-12-26 | High-thermal-conductivity insulating layer material, metal substrate and preparation method |
| PCT/CN2020/110976 WO2021128895A1 (en) | 2019-12-26 | 2020-08-25 | High-thermal-conductivity insulating layer material, metal substrate, and preparation method |
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| CN116364816A (en) * | 2023-05-31 | 2023-06-30 | 南昌凯捷半导体科技有限公司 | Thermoelectric separation AlGaInP LED chip and manufacturing method |
| CN116364816B (en) * | 2023-05-31 | 2023-08-25 | 南昌凯捷半导体科技有限公司 | Thermoelectric separation AlGaInP LED chip and manufacturing method |
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