CN114148048A - High-heat-dissipation aluminum-based copper-clad plate and preparation method thereof - Google Patents

High-heat-dissipation aluminum-based copper-clad plate and preparation method thereof Download PDF

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Publication number
CN114148048A
CN114148048A CN202111437705.6A CN202111437705A CN114148048A CN 114148048 A CN114148048 A CN 114148048A CN 202111437705 A CN202111437705 A CN 202111437705A CN 114148048 A CN114148048 A CN 114148048A
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heat
aluminum
clad plate
based copper
conducting filler
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詹浩
王林祥
陈明
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Jiuyao Electronic Technology Jiangsu Co ltd
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Jiuyao Electronic Technology Jiangsu Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
    • B32B15/017—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of aluminium or an aluminium alloy, another layer being formed of an alloy based on a non ferrous metal other than aluminium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
    • B32B37/1284—Application of adhesive
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • 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
    • 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
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K1/00—Printed circuits
    • H05K1/02—Details
    • H05K1/03—Use of materials for the substrate
    • H05K1/05—Insulated conductive substrates, e.g. insulated metal substrate
    • H05K1/056—Insulated conductive substrates, e.g. insulated metal substrate the metal substrate being covered by an organic insulating layer
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00—Apparatus or processes for manufacturing printed circuits
    • H05K3/02—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding
    • H05K3/022—Processes for manufacturing precursors of printed circuits, i.e. copper-clad substrates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
    • B32B2307/206—Insulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/302—Conductive
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/306—Resistant to heat
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2457/00—Electrical equipment
    • B32B2457/08—PCBs, i.e. printed circuit boards
    • 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
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives

Abstract

The invention discloses a high-heat-dissipation aluminum-based copper-clad plate and a preparation method thereof, and particularly relates to the technical field of aluminum-based copper-clad plates, which comprises the following steps: the heat-conducting paint comprises organic silicon resin, epoxy resin, dicyandiamide solution, heat-conducting filler and an organic solvent. The invention can effectively improve the high heat dispersion and high heat conductivity of the aluminum-based copper-clad plate, and can improve the peel strength of the aluminum-based copper-clad plate at low temperature; the organic silicon resin and the epoxy resin are blended and matched, so that the high and low temperature resistance, the ageing resistance and the electric insulation performance of the aluminum-based copper-clad plate can be enhanced while the bonding performance of the insulating bonding layer is ensured; meanwhile, the heat-conducting filler is used in a matched manner, so that the high-low temperature resistance and the heat-conducting property of the insulating bonding layer can be effectively improved; in the third step and the fourth step, the blending treatment effect of the base materials can be effectively enhanced, and the safety and the stability of the insulating bonding layer are enhanced; and in the sixth step, the aluminum plate layer and the copper foil layer are subjected to surface etching modification treatment, so that the peel strength of the aluminum-based copper-clad plate can be effectively enhanced.

Description

High-heat-dissipation aluminum-based copper-clad plate and preparation method thereof
Technical Field
The invention relates to the technical field of aluminum-based copper-clad plates, in particular to a high-heat-dissipation aluminum-based copper-clad plate and a preparation method thereof.
Background
The aluminum-based copper-clad plate is used as a substrate material in the manufacture of the printed circuit board, mainly plays roles of interconnection, conduction, insulation and support in the printed circuit board, and has great influence on the transmission speed, energy loss, characteristic impedance and the like of signals in the printed circuit board, and the aluminum-based copper-clad plate is a core component in the printed circuit board. The aluminum-based copper clad laminate is an aluminum substrate, which is one of raw materials, and is a plate-shaped material which is formed by using electronic glass fiber cloth or other reinforced materials, soaking resin, single resin and the like as an insulating bonding layer, covering copper foil on one surface or two surfaces of the aluminum-based copper clad laminate with copper foil and performing hot pressing, and is called a copper-clad laminate aluminum substrate, and is called the aluminum-based copper clad laminate for short.
The existing aluminum-based copper-clad plate has poor heat dissipation performance, and meanwhile, the aluminum-based copper-clad plate has poor anti-stripping performance at low temperature.
Disclosure of Invention
In order to overcome the defects in the prior art, the embodiment of the invention provides a high-heat-dissipation aluminum-based copper-clad plate and a preparation method thereof.
The high-heat-dissipation aluminum-based copper-clad plate comprises an aluminum plate layer, an insulating bonding layer and a copper foil layer, wherein the insulating bonding layer comprises the following components in percentage by weight: 29.40-31.20% of organic silicon resin, 28.40-30.60% of epoxy resin, 10.50-11.30% of dicyandiamide solution, 9.40-10.20% of heat-conducting filler and the balance of organic solvent.
Further, the heat conducting filler comprises the following components in percentage by weight: 30.20-32.40% of hexagonal boron nitride micro-tablets, 9.40-11.60% of nano silicon carbide, 10.20-12.80% of nano aluminum nitride and the balance of silicon micro-powder.
Further, the insulating bonding layer comprises the following components in percentage by weight: 29.40% of silicone resin, 28.40% of epoxy resin, 10.50% of dicyandiamide solution, 9.40% of heat-conducting filler and 22.30% of organic solvent; the heat-conducting filler comprises the following components in percentage by weight: 30.20 percent of hexagonal boron nitride micro-tablets, 9.40 percent of nano silicon carbide, 10.20 percent of nano aluminum nitride and 50.20 percent of silicon micro-powder.
Further, the insulating bonding layer comprises the following components in percentage by weight: 31.20% of silicone resin, 30.60% of epoxy resin, 11.30% of dicyandiamide solution, 10.20% of heat-conducting filler and 16.70% of organic solvent; the heat-conducting filler comprises the following components in percentage by weight: 32.40% of hexagonal boron nitride micro-tablets, 11.60% of nano silicon carbide, 12.80% of nano aluminum nitride and 43.20% of silicon micro-powder.
Further, the insulating bonding layer comprises the following components in percentage by weight: 30.30% of silicone resin, 29.50% of epoxy resin, 10.90% of dicyandiamide solution, 9.80% of heat-conducting filler and 19.50% of organic solvent; the heat-conducting filler comprises the following components in percentage by weight: 31.30% of hexagonal boron nitride micro-tablets, 10.50% of nano silicon carbide, 11.50% of nano aluminum nitride and 46.70% of silicon micro-powder.
The solid content of the dicyandiamide solution is 10.6%, and the organic solvent is one or more of methanol, ethylene glycol or pyridine.
The invention also provides a preparation method of the high-heat-dissipation aluminum-based copper-clad plate, which comprises the following specific preparation steps:
the method comprises the following steps: weighing the organic silicon resin, the epoxy resin, the dicyandiamide solution, the heat-conducting filler and the organic solvent in parts by weight;
step two: adding the heat-conducting filler obtained in the step one into a steam kinetic energy mill to obtain a premixed heat-conducting filler;
step three: heating, mechanically stirring and mixing the organic silicon resin and the organic solvent in the first step by one half by weight and the premixed heat conducting filler in the second step by one half by weight for 50-60 minutes, and performing ultrasonic treatment to obtain a base material A;
step four: heating, mechanically stirring and mixing the epoxy resin and the residual organic solvent in the step four and the residual premixed heat-conducting filler in the step two for 50-60 minutes, and performing ultrasonic treatment to obtain a base material B;
step five: mechanically stirring and mixing the base material A in the third step and the base material B in the fourth step, adding the uniformly mixed base materials and the dicyandiamide solution in the first step into an emulsifying kettle, and performing high-speed emulsification and shearing treatment in the emulsifying kettle to obtain a mixed glue solution;
step six: carrying out double-sided etching treatment on the aluminum plate layer by using a plasma cleaning machine to obtain a modified aluminum plate layer; carrying out single-side etching treatment on the copper foil layer by using a plasma cleaning machine to obtain a modified copper foil layer;
step seven: coating the mixed glue solution obtained in the fifth step on the outer wall of the modified aluminum plate layer obtained in the sixth step, and drying for 3-5 minutes at 152-158 ℃ to obtain a semi-cured insulating bonding layer;
step eight: and contacting the modified surface of the modified copper foil layer in the sixth step with a semi-cured insulating adhesive layer, and then carrying out hot press molding to obtain the high-heat-dissipation aluminum-based copper-clad plate.
Further, in the second step, the steam consumption of the steam kinetic energy mill is 1300-1700 kg/h, the steam pressure is 18-26 bar, and the temperature is 290-330 ℃; the ultrasonic frequency in the third step and the fourth step is 1.6 MHz; in the fifth step, the high-speed shearing of the emulsifying kettle adopts a pipeline high-speed shearing technology, the high-speed shearing rate is 3800-4200 r/min, and the high-speed shearing time is 1-2 h; in the sixth step, the power of the radio frequency power supply of the plasma cleaning machine is 115W, the frequency of the plasma is 13.56MHz, the atmosphere is nitrogen, and the working time is 15 min; in the eighth step, hot-press forming is carried out at 200-220 ℃ under the pressure of 43-48 kg/m 2.
Further, in the second step, the steam consumption of the steam kinetic energy mill is 1300kg/h, the steam pressure is 18bar, and the temperature is 290 ℃; the ultrasonic frequency in the third step and the fourth step is 1.6 MHz; in the fifth step, the emulsification kettle adopts a pipeline high-speed shearing technology for high-speed shearing, the high-speed shearing rate is 3800r/min, and the high-speed shearing time is 1 h; in the sixth step, the power of the radio frequency power supply of the plasma cleaning machine is 115W, the frequency of the plasma is 13.56MHz, the atmosphere is nitrogen, and the working time is 15 min; in step eight, hot press forming is carried out at 200 ℃ under a pressure of 43kg/m 2.
Further, in the second step, the steam consumption of the steam kinetic energy mill is 1500kg/h, the steam pressure is 22bar, and the temperature is 310 ℃; the ultrasonic frequency in the third step and the fourth step is 1.6 MHz; in the fifth step, the emulsification kettle adopts a pipeline high-speed shearing technology for high-speed shearing, the high-speed shearing rate is 4000r/min, and the high-speed shearing time is 1.5 h; in the sixth step, the power of the radio frequency power supply of the plasma cleaning machine is 115W, the frequency of the plasma is 13.56MHz, the atmosphere is nitrogen, and the working time is 15 min; in step eight, hot press forming is carried out at 210 ℃ and the pressure is 45kg/m 2.
The invention has the technical effects and advantages that:
1. the high-heat-dissipation aluminum-based copper-clad plate prepared by adopting the raw material formula can effectively improve the high heat-dissipation performance and the high heat-conducting performance of the aluminum-based copper-clad plate, and can improve the peel strength of the aluminum-based copper-clad plate at low temperature; the organic silicon resin and the epoxy resin are blended and matched, so that the high and low temperature resistance, the ageing resistance and the electric insulation performance of the aluminum-based copper-clad plate can be enhanced while the bonding performance of the insulating bonding layer is ensured; the hexagonal boron nitride micro-sheets are uniformly compounded and blended into the insulating bonding layer, so that the heat resistance and the insulating heat dissipation performance of the insulating bonding layer can be effectively enhanced, and the high heat dissipation performance of the aluminum-based copper-clad plate is further enhanced; the nano silicon carbide is uniformly compounded into the insulating bonding layer, so that the heat conduction performance and the heat dissipation performance of the insulating bonding layer can be effectively enhanced, and the high heat dissipation performance of the aluminum-based copper-clad plate is further improved; the nanometer aluminum nitride is uniformly compounded into the insulating bonding layer, so that the heat conducting performance and the high and low temperature resistance of the insulating bonding layer can be effectively enhanced, the high heat dissipation performance and the high and low temperature resistance of the aluminum-based copper-clad plate are further improved, and the use performance of the aluminum-based copper-clad plate at low temperature is ensured; the silicon micropowder is used as a functional filler to be applied to an insulating bonding layer of the aluminum-based copper-clad plate, so that the cost can be reduced, and the mechanical property and the temperature resistance of the aluminum-based copper-clad plate can be improved; meanwhile, the hexagonal boron nitride micro-sheet, the nano silicon carbide, the nano aluminum nitride and the silicon micro-powder are used in a matching way, so that the high and low temperature resistance and the heat conduction performance of the insulating bonding layer can be effectively improved;
2. in the process of preparing the high-heat-dissipation aluminum-based copper-clad plate, the crushed particle size of the heat-conducting filler can be effectively enhanced in the second step, and the mixing uniformity of the heat-conducting filler is improved; in the third step, the blending treatment effect of the base material A can be effectively enhanced, and the uniform mixing degree of the heat-conducting filler and the organic silicon resin can be effectively enhanced, so that the safety and the stability of the insulating bonding layer are enhanced; in the fourth step, the blending treatment effect of the base material B can be effectively enhanced, the blending uniformity of the heat-conducting filler and the epoxy resin can be effectively enhanced, and the safety and the stability of the insulating bonding layer are further enhanced; carrying out surface etching modification treatment on the aluminum plate layer and the copper foil layer by using a plasma cleaning machine in the sixth step; in the seventh step, the bonding stability of the semi-cured insulating bonding layer and the modified aluminum plate layer is better, so that the peeling strength of the aluminum-based copper-clad plate is higher; and in the eighth step, the bonding stability of the modified copper foil layer and the semi-cured insulating bonding layer is better, and the peel strength resistance of the aluminum-based copper-clad plate is further enhanced.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the invention provides a high-heat-dissipation aluminum-based copper-clad plate which comprises an aluminum plate layer, an insulating bonding layer and a copper foil layer, wherein the insulating bonding layer comprises the following components in percentage by weight: 31.20% of silicone resin, 30.60% of epoxy resin, 11.30% of dicyandiamide solution, 10.20% of heat-conducting filler and 16.70% of organic solvent; the heat-conducting filler comprises the following components in percentage by weight: 32.40% of hexagonal boron nitride micro-tablets, 11.60% of nano silicon carbide, 12.80% of nano aluminum nitride and 43.20% of silicon micro-powder;
the solid content of the dicyandiamide solution is 10.6%, and the organic solvent is methanol and glycol according to the weight part ratio: 1: 2;
the invention also provides a preparation method of the high-heat-dissipation aluminum-based copper-clad plate, which comprises the following specific preparation steps:
the method comprises the following steps: weighing the organic silicon resin, the epoxy resin, the dicyandiamide solution, the heat-conducting filler and the organic solvent in parts by weight;
step two: adding the heat-conducting filler obtained in the step one into a steam kinetic energy mill to obtain a premixed heat-conducting filler;
step three: heating, mechanically stirring and mixing the organic silicon resin and the organic solvent in the first step by one half by weight and the premixed heat conducting filler in the second step by one half by weight for 50 minutes, and performing ultrasonic treatment to obtain a base material A;
step four: heating, mechanically stirring and mixing the epoxy resin and the residual organic solvent in the step four and the residual premixed heat-conducting filler in the step two for 50 minutes, and simultaneously performing ultrasonic treatment to obtain a base material B;
step five: mechanically stirring and mixing the base material A in the third step and the base material B in the fourth step, adding the uniformly mixed base materials and the dicyandiamide solution in the first step into an emulsifying kettle, and performing high-speed emulsification and shearing treatment in the emulsifying kettle to obtain a mixed glue solution;
step six: carrying out double-sided etching treatment on the aluminum plate layer by using a plasma cleaning machine to obtain a modified aluminum plate layer; carrying out single-side etching treatment on the copper foil layer by using a plasma cleaning machine to obtain a modified copper foil layer;
step seven: coating the mixed glue solution obtained in the fifth step on the outer wall of the modified aluminum plate layer obtained in the sixth step, and drying for 3 minutes at 152 ℃ to obtain a semi-cured insulating bonding layer;
step eight: and contacting the modified surface of the modified copper foil layer in the sixth step with a semi-cured insulating adhesive layer, and then carrying out hot press molding to obtain the high-heat-dissipation aluminum-based copper-clad plate.
In the second step, the steam consumption of the steam kinetic energy mill is 1300kg/h, the steam pressure is 18bar, and the temperature is 290 ℃; the ultrasonic frequency in the third step and the fourth step is 1.6 MHz; in the fifth step, the emulsification kettle adopts a pipeline high-speed shearing technology for high-speed shearing, the high-speed shearing rate is 3800r/min, and the high-speed shearing time is 1 h; in the sixth step, the power of the radio frequency power supply of the plasma cleaning machine is 115W, the frequency of the plasma is 13.56MHz, the atmosphere is nitrogen, and the working time is 15 min; in step eight, hot press forming is carried out at 200 ℃ under a pressure of 43kg/m 2.
Example 2:
different from the embodiment 1, the insulating bonding layer comprises the following components in percentage by weight: 31.20% of silicone resin, 30.60% of epoxy resin, 11.30% of dicyandiamide solution, 10.20% of heat-conducting filler and 16.70% of organic solvent; the heat-conducting filler comprises the following components in percentage by weight: 32.40% of hexagonal boron nitride micro-tablets, 11.60% of nano silicon carbide, 12.80% of nano aluminum nitride and 43.20% of silicon micro-powder.
Example 3:
different from the embodiments 1-2, the insulating bonding layer comprises the following components in percentage by weight: 30.30% of silicone resin, 29.50% of epoxy resin, 10.90% of dicyandiamide solution, 9.80% of heat-conducting filler and 19.50% of organic solvent; the heat-conducting filler comprises the following components in percentage by weight: 31.30% of hexagonal boron nitride micro-tablets, 10.50% of nano silicon carbide, 11.50% of nano aluminum nitride and 46.70% of silicon micro-powder.
Taking the high-heat-dissipation aluminum-based copper-clad plate prepared in the above examples 1-3, as well as the high-heat-dissipation aluminum-based copper-clad plate of the first control group, the high-heat-dissipation aluminum-based copper-clad plate of the second control group, the high-heat-dissipation aluminum-based copper-clad plate of the third control group, the high-heat-dissipation aluminum-based copper-clad plate of the fourth control group and the high-heat-dissipation aluminum-based copper-clad plate of the fifth control group, respectively, the high-heat-dissipation aluminum-based copper-clad plate of the first control group has no hexagonal boron nitride micro-patches compared with the examples, the high-heat-dissipation aluminum-based copper-clad plate of the second control group has no nano silicon carbide compared with the examples, the high-heat-dissipation aluminum-based copper-clad plate of the third control group has no nano aluminum nitride compared with the examples, the high-heat-dissipation aluminum-based copper-clad plate of the fourth control group has no silicon micro-powder compared with the examples, the high-heat-dissipation aluminum-based copper-clad plate of the fifth control group prepared in the three examples and the high-heat-dissipation aluminum-based copper-clad plates of the five control groups are respectively, every 30 samples are taken as a group, and the test results are shown in the table one:
table one:
Figure RE-292019DEST_PATH_IMAGE002
as can be seen from Table I, the raw material ratio of the insulating bonding layer in the high-heat-dissipation aluminum-based copper-clad plate is as follows: comprises the following components in percentage by weight: 30.30% of silicone resin, 29.50% of epoxy resin, 10.90% of dicyandiamide solution, 9.80% of heat-conducting filler and 19.50% of organic solvent; the heat-conducting filler comprises the following components in percentage by weight: 31.30% of hexagonal boron nitride microchip, 10.50% of nano silicon carbide, 11.50% of nano aluminum nitride and 46.70% of silicon micropowder, the high heat dissipation performance and the high heat conduction performance of the aluminum-based copper-clad plate can be effectively improved, and meanwhile, the peel strength of the aluminum-based copper-clad plate at low temperature can be improved; therefore, the embodiment 3 is a preferred embodiment of the invention, the organic silicon resin in the formula is thermosetting polyorganosiloxane with a highly cross-linked structure, and has excellent heat resistance, cold resistance, weather resistance, electrical insulation and hydrophobic performance, and the organic silicon resin and the epoxy resin are blended and matched, so that the high and low temperature resistance, the aging resistance and the electrical insulation performance of the aluminum-based copper-clad plate can be enhanced while the adhesive performance of the insulating adhesive layer is ensured; dicyandiamide solution in the formula is taken as a curing agent to enhance the curing performance of epoxy resin and organic silicon resin; the hexagonal boron nitride micro-sheets in the heat-conducting filler have high heat resistance, high heat conductivity coefficient, low thermal expansion coefficient and high-temperature insulation performance, and the hexagonal boron nitride micro-sheets are uniformly compounded and blended into the insulating bonding layer, so that the heat resistance and the insulating heat dissipation performance of the insulating bonding layer can be effectively enhanced, and further the high heat dissipation performance of the aluminum-based copper-clad plate is enhanced; the nano silicon carbide in the heat-conducting filler has stable chemical properties and high heat conductivity coefficient, and is uniformly compounded into the insulating bonding layer, so that the heat-conducting property and the heat dissipation performance of the insulating bonding layer can be effectively enhanced, and the high heat dissipation performance of the aluminum-based copper-clad plate is further improved; the nano aluminum nitride in the heat-conducting filler has good heat conductivity, good electrical insulation and wider electrical insulation service temperature, can be used under the conditions of low temperature and high temperature at the same time, and is uniformly compounded into the insulating adhesive layer, so that the heat-conducting property and the high-low temperature resistance of the insulating adhesive layer can be effectively enhanced, the high heat-radiating property and the high-low temperature resistance of the aluminum-based copper-clad plate are further improved, and the service performance of the aluminum-based copper-clad plate at low temperature is ensured; the silicon powder in the heat-conducting filler has high electrical insulation, high thermal stability, acid and alkali resistance and wear resistance, and can be used as a functional filler to be applied to an insulation bonding layer of an aluminum-based copper-clad plate, so that the cost can be reduced, and the mechanical property and the temperature resistance of the aluminum-based copper-clad plate can be improved; meanwhile, the hexagonal boron nitride micro-sheet, the nano silicon carbide, the nano aluminum nitride and the silicon micro-powder are used in a matching way, so that the high and low temperature resistance and the heat conduction performance of the insulating bonding layer can be effectively improved.
Example 4:
the invention provides a high-heat-dissipation aluminum-based copper-clad plate which comprises an aluminum plate layer, an insulating bonding layer and a copper foil layer, and the aluminum-based copper-clad plate comprises the following components in percentage by weight: 30.30% of silicone resin, 29.50% of epoxy resin, 10.90% of dicyandiamide solution, 9.80% of heat-conducting filler and 19.50% of organic solvent; the heat-conducting filler comprises the following components in percentage by weight: 31.30% of hexagonal boron nitride micro-tablets, 10.50% of nano silicon carbide, 11.50% of nano aluminum nitride and 46.70% of silicon micro-powder;
the solid content of the dicyandiamide solution is 10.6%, and the organic solvent is methanol and glycol according to the weight part ratio: 1: 2;
the invention also provides a preparation method of the high-heat-dissipation aluminum-based copper-clad plate, which comprises the following specific preparation steps:
the method comprises the following steps: weighing the organic silicon resin, the epoxy resin, the dicyandiamide solution, the heat-conducting filler and the organic solvent in parts by weight;
step two: adding the heat-conducting filler obtained in the step one into a steam kinetic energy mill to obtain a premixed heat-conducting filler;
step three: heating, mechanically stirring and mixing the organic silicon resin and the organic solvent in the first step by one half by weight and the premixed heat conducting filler in the second step by one half by weight for 50 minutes, and performing ultrasonic treatment to obtain a base material A;
step four: heating, mechanically stirring and mixing the epoxy resin and the residual organic solvent in the step four and the residual premixed heat-conducting filler in the step two for 50 minutes, and simultaneously performing ultrasonic treatment to obtain a base material B;
step five: mechanically stirring and mixing the base material A in the third step and the base material B in the fourth step, adding the uniformly mixed base materials and the dicyandiamide solution in the first step into an emulsifying kettle, and performing high-speed emulsification and shearing treatment in the emulsifying kettle to obtain a mixed glue solution;
step six: carrying out double-sided etching treatment on the aluminum plate layer by using a plasma cleaning machine to obtain a modified aluminum plate layer; carrying out single-side etching treatment on the copper foil layer by using a plasma cleaning machine to obtain a modified copper foil layer;
step seven: coating the mixed glue solution obtained in the fifth step on the outer wall of the modified aluminum plate layer obtained in the sixth step, and drying for 3 minutes at 152 ℃ to obtain a semi-cured insulating bonding layer;
step eight: and contacting the modified surface of the modified copper foil layer in the sixth step with a semi-cured insulating adhesive layer, and then carrying out hot press molding to obtain the high-heat-dissipation aluminum-based copper-clad plate.
In the second step, the steam consumption of the steam kinetic energy mill is 1300kg/h, the steam pressure is 18bar, and the temperature is 290 ℃; the ultrasonic frequency in the third step and the fourth step is 1.6 MHz; in the fifth step, the emulsification kettle adopts a pipeline high-speed shearing technology for high-speed shearing, the high-speed shearing rate is 3800r/min, and the high-speed shearing time is 1 h; in the sixth step, the power of the radio frequency power supply of the plasma cleaning machine is 115W, the frequency of the plasma is 13.56MHz, the atmosphere is nitrogen, and the working time is 15 min; in step eight, hot press forming is carried out at 200 ℃ under a pressure of 43kg/m 2.
Example 5:
different from the embodiment 4, in the second step, the steam consumption of the steam kinetic energy mill is 1300kg/h, the steam pressure is 18bar, and the temperature is 290 ℃; the ultrasonic frequency in the third step and the fourth step is 1.6 MHz; stirring and mixing for 60 minutes in the third step, stirring and mixing for 60 minutes in the fourth step, drying for 5 minutes at 158 ℃ in the seventh step, and shearing at high speed of 3800r/min and 1h in the fifth step by adopting a pipeline high-speed shearing technology; in the sixth step, the power of the radio frequency power supply of the plasma cleaning machine is 115W, the frequency of the plasma is 13.56MHz, the atmosphere is nitrogen, and the working time is 15 min; in step eight, hot press forming is carried out at 200 ℃ under a pressure of 43kg/m 2.
Example 6:
different from the embodiments 4-5, in the second step, the steam consumption of the steam kinetic energy mill is 1500kg/h, the steam pressure is 22bar, and the temperature is 310 ℃; the ultrasonic frequency in the third step and the fourth step is 1.6 MHz; stirring and mixing for 55 minutes in the third step, stirring and mixing for 55 minutes in the fourth step, and drying for 4 minutes at 155 ℃ in the seventh step; in the fifth step, the emulsification kettle adopts a pipeline high-speed shearing technology for high-speed shearing, the high-speed shearing rate is 4000r/min, and the high-speed shearing time is 1.5 h; in the sixth step, the power of the radio frequency power supply of the plasma cleaning machine is 115W, the frequency of the plasma is 13.56MHz, the atmosphere is nitrogen, and the working time is 15 min; in step eight, hot press forming is carried out at 210 ℃ and the pressure is 45kg/m 2.
The high-heat-dissipation aluminum-based copper-clad plate prepared in the above examples 4-6, the high-heat-dissipation aluminum-based copper-clad plate of the sixth control group, the high-heat-dissipation aluminum-based copper-clad plate of the seventh control group, the high-heat-dissipation aluminum-based copper-clad plate of the eighth control group and the high-heat-dissipation aluminum-based copper-clad plate of the ninth control group are taken respectively, compared with the embodiment, the high heat dissipation aluminum-based copper-clad plate of the comparison group six has no operation in the step two, and the high heat dissipation aluminum-based copper-clad plate of the comparison group seven has no operation in the step three, the high-heat-dissipation aluminum-based copper-clad plate of the contrast group eight is compared with the embodiment and has no operation in the fourth step, the high-heat-dissipation aluminum-based copper-clad plate of the contrast group nine is compared with the embodiment and has no operation in the sixth step, the high-heat-dissipation aluminum-based copper-clad plate prepared in the three embodiments and the high-heat-dissipation aluminum-based copper-clad plates of the four contrast groups are respectively tested in seven groups, every 30 samples are taken as one group, the test is carried out, and the test result is shown in the table two:
table two:
Figure RE-943580DEST_PATH_IMAGE004
as can be seen from table two, example 6 is a preferred embodiment of the present invention; in the second step, the heat-conducting filler is processed in a steam kinetic energy mill, so that the crushing particle size of the heat-conducting filler can be effectively enhanced, and the mixing uniformity of the heat-conducting filler is improved; in the third step, the organic silicon resin, part of the organic solvent and the premixed heat-conducting filler are subjected to mixed ultrasonic treatment, so that the blending treatment effect of the base material A can be effectively enhanced, the uniform mixing degree of the heat-conducting filler and the organic silicon resin can be effectively enhanced, the mixing effect of the base material A is further improved, and the safety and the stability of the insulating bonding layer are enhanced; in the fourth step, the epoxy resin, the residual organic solvent and the heat-conducting filler are subjected to mixing ultrasonic treatment, so that the blending treatment effect of the base material B can be effectively enhanced, the blending uniformity of the heat-conducting filler and the epoxy resin can be effectively enhanced, the mixing effect of the base material B is further improved, and the safety and the stability of the insulating bonding layer are further enhanced; hatching and shearing the base material A and the base material B in the fifth step to obtain mixed glue solution; carrying out surface etching modification treatment on the aluminum plate layer and the copper foil layer by using a plasma cleaning machine in the sixth step; in the seventh step, the mixed glue solution is coated on the modified aluminum plate layer and is cured, so that the combination stability of the semi-cured insulating bonding layer and the modified aluminum plate layer is better, and the anti-peeling strength of the aluminum-based copper-clad plate is higher; and step eight, hot-pressing and compounding the modified copper foil layer outside the semi-cured insulating bonding layer, so that the bonding stability of the modified copper foil layer and the semi-cured insulating bonding layer is better, and the peel strength resistance of the aluminum-based copper-clad plate is further enhanced.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A high heat dissipation aluminium base copper-clad plate which characterized in that: the aluminum-clad laminate comprises an aluminum plate layer, an insulating bonding layer and a copper foil layer, wherein the insulating bonding layer comprises the following components in percentage by weight: 29.40-31.20% of organic silicon resin, 28.40-30.60% of epoxy resin, 10.50-11.30% of dicyandiamide solution, 9.40-10.20% of heat-conducting filler and the balance of organic solvent.
2. The high-heat-dissipation aluminum-based copper-clad plate according to claim 1, characterized in that: the heat-conducting filler comprises the following components in percentage by weight: 30.20-32.40% of hexagonal boron nitride micro-tablets, 9.40-11.60% of nano silicon carbide, 10.20-12.80% of nano aluminum nitride and the balance of silicon micro-powder.
3. The high-heat-dissipation aluminum-based copper-clad plate according to claim 2, characterized in that: the insulating bonding layer comprises the following components in percentage by weight: 29.40% of silicone resin, 28.40% of epoxy resin, 10.50% of dicyandiamide solution, 9.40% of heat-conducting filler and 22.30% of organic solvent; the heat-conducting filler comprises the following components in percentage by weight: 30.20 percent of hexagonal boron nitride micro-tablets, 9.40 percent of nano silicon carbide, 10.20 percent of nano aluminum nitride and 50.20 percent of silicon micro-powder.
4. The high-heat-dissipation aluminum-based copper-clad plate according to claim 2, characterized in that: the insulating bonding layer comprises the following components in percentage by weight: 31.20% of silicone resin, 30.60% of epoxy resin, 11.30% of dicyandiamide solution, 10.20% of heat-conducting filler and 16.70% of organic solvent; the heat-conducting filler comprises the following components in percentage by weight: 32.40% of hexagonal boron nitride micro-tablets, 11.60% of nano silicon carbide, 12.80% of nano aluminum nitride and 43.20% of silicon micro-powder.
5. The high-heat-dissipation aluminum-based copper-clad plate according to claim 2, characterized in that: the insulating bonding layer comprises the following components in percentage by weight: 30.30% of silicone resin, 29.50% of epoxy resin, 10.90% of dicyandiamide solution, 9.80% of heat-conducting filler and 19.50% of organic solvent; the heat-conducting filler comprises the following components in percentage by weight: 31.30% of hexagonal boron nitride micro-tablets, 10.50% of nano silicon carbide, 11.50% of nano aluminum nitride and 46.70% of silicon micro-powder.
6. The high-heat-dissipation aluminum-based copper-clad plate according to claim 1, characterized in that: the solid content of the dicyandiamide solution is 10.6%, and the organic solvent is one or more of methanol, ethylene glycol or pyridine.
7. The preparation method of the high heat dissipation aluminum-based copper-clad plate according to any one of claims 1 to 6, characterized in that: the preparation method comprises the following specific steps:
the method comprises the following steps: weighing the organic silicon resin, the epoxy resin, the dicyandiamide solution, the heat-conducting filler and the organic solvent in parts by weight;
step two: adding the heat-conducting filler obtained in the step one into a steam kinetic energy mill to obtain a premixed heat-conducting filler;
step three: heating, mechanically stirring and mixing the organic silicon resin and the organic solvent in the first step by one half by weight and the premixed heat conducting filler in the second step by one half by weight for 50-60 minutes, and performing ultrasonic treatment to obtain a base material A;
step four: heating, mechanically stirring and mixing the epoxy resin and the residual organic solvent in the step four and the residual premixed heat-conducting filler in the step two for 50-60 minutes, and performing ultrasonic treatment to obtain a base material B;
step five: mechanically stirring and mixing the base material A in the third step and the base material B in the fourth step, adding the uniformly mixed base materials and the dicyandiamide solution in the first step into an emulsifying kettle, and performing high-speed emulsification and shearing treatment in the emulsifying kettle to obtain a mixed glue solution;
step six: carrying out double-sided etching treatment on the aluminum plate layer by using a plasma cleaning machine to obtain a modified aluminum plate layer; carrying out single-side etching treatment on the copper foil layer by using a plasma cleaning machine to obtain a modified copper foil layer;
step seven: coating the mixed glue solution obtained in the fifth step on the outer wall of the modified aluminum plate layer obtained in the sixth step, and drying for 3-5 minutes at 152-158 ℃ to obtain a semi-cured insulating bonding layer;
step eight: and contacting the modified surface of the modified copper foil layer in the sixth step with a semi-cured insulating adhesive layer, and then carrying out hot press molding to obtain the high-heat-dissipation aluminum-based copper-clad plate.
8. The preparation method of the high-heat-dissipation aluminum-based copper-clad plate according to claim 7, characterized in that: in the second step, the steam consumption of the steam kinetic energy mill is 1300-1700 kg/h, the steam pressure is 18-26 bar, and the temperature is 290-330 ℃; the ultrasonic frequency in the third step and the fourth step is 1.6 MHz; in the fifth step, the high-speed shearing of the emulsifying kettle adopts a pipeline high-speed shearing technology, the high-speed shearing rate is 3800-4200 r/min, and the high-speed shearing time is 1-2 h; in the sixth step, the power of the radio frequency power supply of the plasma cleaning machine is 115W, the frequency of the plasma is 13.56MHz, the atmosphere is nitrogen, and the working time is 15 min; in the eighth step, hot-press forming is carried out at 200-220 ℃ under the pressure of 43-48 kg/m 2.
9. The preparation method of the high-heat-dissipation aluminum-based copper-clad plate according to claim 8, characterized in that: in the second step, the steam consumption of the steam kinetic energy mill is 1300kg/h, the steam pressure is 18bar, and the temperature is 290 ℃; the ultrasonic frequency in the third step and the fourth step is 1.6 MHz; in the fifth step, the emulsification kettle adopts a pipeline high-speed shearing technology for high-speed shearing, the high-speed shearing rate is 3800r/min, and the high-speed shearing time is 1 h; in the sixth step, the power of the radio frequency power supply of the plasma cleaning machine is 115W, the frequency of the plasma is 13.56MHz, the atmosphere is nitrogen, and the working time is 15 min; in step eight, hot press forming is carried out at 200 ℃ under a pressure of 43kg/m 2.
10. The preparation method of the high-heat-dissipation aluminum-based copper-clad plate according to claim 8, characterized in that: in the second step, the steam consumption of the steam kinetic energy mill is 1500kg/h, the steam pressure is 22bar, and the temperature is 310 ℃; the ultrasonic frequency in the third step and the fourth step is 1.6 MHz; in the fifth step, the emulsification kettle adopts a pipeline high-speed shearing technology for high-speed shearing, the high-speed shearing rate is 4000r/min, and the high-speed shearing time is 1.5 h; in the sixth step, the power of the radio frequency power supply of the plasma cleaning machine is 115W, the frequency of the plasma is 13.56MHz, the atmosphere is nitrogen, and the working time is 15 min; in step eight, hot press forming is carried out at 210 ℃ and the pressure is 45kg/m 2.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114654829A (en) * 2022-04-09 2022-06-24 江西鑫远基电子科技有限公司 Aluminum-based copper-clad plate with high breakdown voltage and production process thereof
CN114953629A (en) * 2022-04-20 2022-08-30 江西鑫远基电子科技有限公司 High-heat-dissipation aluminum-based copper-clad plate and production process thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114654829A (en) * 2022-04-09 2022-06-24 江西鑫远基电子科技有限公司 Aluminum-based copper-clad plate with high breakdown voltage and production process thereof
CN114654829B (en) * 2022-04-09 2023-11-17 江西鑫远基电子科技有限公司 Aluminum-based copper-clad plate with high breakdown voltage and production process thereof
CN114953629A (en) * 2022-04-20 2022-08-30 江西鑫远基电子科技有限公司 High-heat-dissipation aluminum-based copper-clad plate and production process thereof

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