CN114290769B - Metal plate, insulated metal plate and preparation method and application of insulated metal plate - Google Patents
Metal plate, insulated metal plate and preparation method and application of insulated metal plate Download PDFInfo
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Abstract
The invention belongs to the technical field of LEDs, and discloses a metal plate, an insulating metal plate, a preparation method and application thereof. The preparation method of the metal plate comprises the following steps: coating a resin composition on the surface of a metal substrate to form a cured film; coating an oxidant on the surface of the cured film to form an oxide layer with polar functional groups; and coating a catalyst on the surface of the cured film to form a catalyst layer. The insulating metal plate includes the metal plate, a heat conductive composite film, and a metal foil. The metal plate in the insulating metal plate and the heat conduction insulating film have higher bonding strength through the synergistic effect of the curing film, the oxidation layer and the catalyst layer, and the insulating metal plate still maintains better bonding strength after being placed at high temperature for a long time, thus being suitable for being used in a high-heat environment; the preparation method of the metal plate is simple and is easy to realize industrialization.
Description
Technical Field
The invention belongs to the technical field of LEDs, and relates to a metal plate, an insulating metal plate, a preparation method and application thereof.
Background
The LED module has a substrate on which an LED light emitting element is provided, and typically, the substrate is a ceramic substrate or a metal substrate. Since a large amount of heat is generated when the LED light emitting element is operated, the substrate needs to have good heat conduction and heat dissipation capabilities.
The common substrate sequentially comprises a metal substrate, a heat conduction insulating layer and a copper foil layer; the heat conducting insulating layer has the dual functions of heat dissipation and insulation, and is generally prepared by adding high-heat conducting ceramic powder into epoxy resin and a condensate thereof and performing high-temperature lamination and curing; the quality of the press-fit affects the bonding strength between the thermally conductive insulating layer and the metal substrate.
At present, the bonding strength between the heat conduction insulating layer and the metal substrate is generally improved in the industry by coating a coupling agent on the surface of the substrate or performing anodic oxidation treatment; but the bonding strength still does not meet the application requirements in a long-term heating environment.
Accordingly, it is desirable to provide an insulated metal sheet comprising a metal sheet and an insulating composite film which can maintain a high bonding strength under normal and high temperature environments.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems in the prior art described above. Therefore, the invention provides a metal plate, an insulating metal plate, a preparation method and application thereof, and the metal plate and the insulating composite film in the insulating metal plate prepared by the metal plate can keep higher bonding strength in normal temperature and high temperature environments.
In order to achieve the above object, a first aspect of the present invention provides a method for producing a metal plate.
The preparation method of the metal plate comprises the following steps: coating a resin composition on the surface of a metal substrate to form a cured film; coating an oxidant on the surface of the cured film to form an oxide layer with polar functional groups; and coating a catalyst on the surface of the cured film to form a catalyst layer.
According to some embodiments of the invention, the polar functional group is at least one of a hydroxyl group, a carbonyl group, or a carboxyl group.
According to some embodiments of the invention, the oxidizing agent is permanganate. Preferably, the permanganate is potassium permanganate.
According to some embodiments of the invention, the concentration of potassium permanganate is 3% -10%. Preferably, the concentration of potassium permanganate is 5%.
According to some embodiments of the invention, the catalyst is used to promote covalent bond formation of the polar functional group with the amino group.
According to some embodiments of the invention, the catalyst is 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride.
According to some embodiments of the invention, the metal substrate is a copper substrate, an aluminum substrate, or a stainless steel substrate.
According to some embodiments of the invention, the resin composition includes an epoxy resin and a curing agent; the epoxy resin is phenolic epoxy resin or dicyclopentadiene epoxy resin.
According to some embodiments of the invention, the epoxy resin is a phenolic epoxy resin; preferably, the phenolic epoxy resin is o-cresol novolac epoxy resin.
According to some embodiments of the invention, the curing agent is at least one of a resin-based curing agent, an anhydride-based curing agent, or an amine-based curing agent.
According to some embodiments of the invention, the curing agent is an amine curing agent; preferably, the amine curing agent is dicyandiamide.
According to some embodiments of the invention, the resin composition further comprises an imidazole-based catalyst or an organophosphorus catalyst.
According to some embodiments of the invention, the imidazole-based catalyst is dimethylimidazole.
According to some embodiments of the invention, the resin composition further comprises a silane coupling agent; preferably, the silane coupling agent has at least one of an amino functional group, a thiol functional group, or a vinyl functional group.
According to some embodiments of the invention, the silane coupling agent is gamma-aminopropyl triethoxysilane.
According to some embodiments of the invention, the resin composition further comprises a toughening agent; the toughening agent is at least one of carboxyl-terminated nitrile rubber, hydroxyl-terminated nitrile rubber, polysulfide rubber or polyurethane rubber. Preferably, the toughening agent is carboxyl terminated nitrile rubber.
According to some embodiments of the invention, the resin composition further comprises an antioxidant; preferably, the antioxidant is at least one of antioxidant BHT, antioxidant 1010 or antioxidant 168.
According to some embodiments of the invention, the antioxidant is antioxidant BHT.
According to some embodiments of the present invention, the resin composition includes, in parts by weight, 1 to 5 parts of an epoxy resin, 0.2 to 3.0 parts of a curing agent, 0.01 to 0.3 parts of a catalyst, 0.01 to 1.5 parts of a silane coupling agent, 0.1 to 5.0 parts of a toughening agent, and 0.01 to 0.1 parts of an antioxidant.
According to some embodiments of the invention, the resin composition further comprises a solvent; the solvent is at least one of acetone, butanone, N-dimethylformamide or N-methylpyrrolidone.
According to some embodiments of the invention, the solvent is N, N-dimethylformamide.
According to some embodiments of the present invention, the resin composition includes, in parts by weight, 1 to 5 parts of an epoxy resin, 0.2 to 3.0 parts of a curing agent, 0.01 to 0.3 parts of a catalyst, 0.01 to 1.5 parts of a silane coupling agent, 0.1 to 5.0 parts of a toughening agent, 0.01 to 0.1 parts of an antioxidant, and 86.0 to 98.0 parts of a solvent.
According to some embodiments of the invention, the method for manufacturing the metal plate comprises: coating a resin composition on the surface of a metal substrate, and baking at 50-200 ℃ to form a cured film; coating an oxidant on the surface of the cured film, maintaining for 5-10min, cleaning, and drying to form an oxide layer with polar functional groups; and coating a catalyst on the surface of the cured film, and drying to form a catalyst layer.
A second aspect of the present invention provides a metal plate produced by the above-described production method.
According to some embodiments of the invention, the metal plate comprises a metal substrate, a cured film, an oxide layer, and a catalyst layer connected in sequence; the cured film is made of a resin composition; the oxide layer is prepared from an oxidant and has polar functional groups; the catalyst layer is made of a catalyst.
According to some embodiments of the invention, the metal substrate is a copper substrate, an aluminum substrate, or a stainless steel substrate.
According to some embodiments of the invention, the cured film has a thickness of 0.01-10 μm.
According to some embodiments of the invention, the cured film has a thickness of 1 μm.
A third aspect of the present invention provides an insulating metal plate including a metal plate, a heat conductive insulating film, and a metal foil; the metal plate is the metal plate.
According to some embodiments of the invention, the metal plate, the heat conductive insulating film, and the metal foil are sequentially stacked and connected, with the heat conductive insulating film facing the cured film of the metal plate.
According to some embodiments of the invention, the thermally conductive insulating film has amino functional groups on its surface.
According to some embodiments of the invention, the thermally conductive insulating film is in an uncured state.
According to some embodiments of the invention, the preparation raw material components of the heat-conducting insulating film comprise E51 type epoxy resin, dicyandiamide, dimethyl imidazole, gamma-aminopropyl triethoxy silicon, spherical aluminum oxide, antioxidant BHT, carboxyl terminated nitrile rubber, glycerol triglycidyl ether and polyvinyl butyral.
According to some embodiments of the invention, the preparation raw material components of the heat-conducting insulating film comprise, by weight, 8-10 parts of E51 type epoxy resin, 2.5-4 parts of dicyandiamide, 0.05-0.15 part of dimethyl imidazole, 0.4-0.6 part of gamma-aminopropyl triethoxysilane, 70-85 parts of spherical aluminum oxide, 0.4-0.6 part of antioxidant BHT, 1-3 parts of carboxyl-terminated nitrile rubber, 3-4 parts of glycerol triglycidyl ether and 1-2 parts of polyvinyl butyral.
According to some embodiments of the invention, the thermally conductive insulating film comprises, in parts by weight, 9 parts of an E51 type epoxy resin, 3 parts of dicyandiamide, 0.1 part of dimethylimidazole, 0.5 part of gamma-aminopropyl triethoxysilane, 80 parts of spherical aluminum oxide, 0.5 part of antioxidant BHT, 2 parts of carboxyl terminated nitrile rubber, 3.4 parts of glycerol triglycidyl ether, and 1.5 parts of polyvinyl butyral.
According to some embodiments of the invention, the metal foil is aluminum foil or copper foil.
According to some embodiments of the invention, the copper foil is an electrolytic copper foil.
According to some embodiments of the invention, the metal foil has a thickness of 50-100 μm. Preferably, the metal foil is 70 μm.
According to some embodiments of the invention, the metal substrate has a thickness of 0.3-5mm.
According to some embodiments of the invention, the thermally conductive and insulating film has a thickness of 50-500 μm.
According to some embodiments of the invention, the thermal conductivity of the thermally conductive and insulating film is 1.0-12.0W/mK.
According to some embodiments of the invention, the thermally conductive insulating film has an insulation withstand voltage greater than 2000V.
A fourth aspect of the present invention provides a method for producing the above insulated metal sheet.
The preparation method comprises the following steps: and sequentially laminating the metal plate, the heat-conducting insulating film and the metal foil, and pressing to obtain the insulating metal plate.
According to some embodiments of the invention, the pressing is performed at 110-210 ℃ and 50-130 MPa.
According to some embodiments of the invention, the pressing comprises: pressing at 110-125deg.C and 50-70MPa for 50-80min; then pressing at 140-180deg.C and 75-100MPa for 70-100min; and then pressing for 100-130min at 190-210 ℃ and 105-130 MPa.
According to some embodiments of the invention, the pressing comprises: pressing at 120deg.C under 60MPa for 60min; then pressing for 90min at 160 ℃ and 80 MPa; then pressing for 120min at 200 ℃ and 120 MPa.
A fifth aspect of the present invention provides the use of the above-described insulated metal sheet in the manufacture of an electronic device.
According to some embodiments of the invention, the electronic device is an LED module.
According to some embodiments of the invention, the electronic device is a high heat generating device.
Therefore, the beneficial effects of the invention include:
1. according to the metal plate, through the synergistic effect of the curing film, the oxide layer and the catalyst layer, the metal plate and the heat conduction insulating film in the insulating metal plate prepared by using the metal plate have higher bonding strength, and the metal plate still maintains higher bonding strength after being placed at high temperature for a long time and is suitable for being used in a high-heat environment;
2. the preparation method of the metal plate is simple and is easy to realize industrialization.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described below.
Example 1
The embodiment provides a metal plate, and the preparation method of the metal plate comprises the following steps:
(1) Coating a resin composition on the surface of a metal substrate to form a cured film;
the resin composition comprises, by weight, 4.5 parts of an o-cresol novolac epoxy resin, 2.0 parts of dicyandiamide, 0.1 part of dimethyl imidazole, 0.5 part of gamma-aminopropyl triethoxysilane, 2.0 parts of carboxyl terminated nitrile rubber, 0.1 part of an antioxidant BHT and 90.8 parts of N, N-dimethylformamide.
The thickness of the cured film was 1. Mu.m.
The metal substrate is a 5052 series aluminum plate with the thickness of 1.5mm;
specifically, sequentially adding o-cresol novolac epoxy resin, dicyandiamide, dimethyl imidazole, gamma-aminopropyl triethoxysilane, carboxyl-terminated nitrile rubber and 2, 6-di-tert-butyl-p-cresol into N, N-dimethylformamide, and uniformly stirring to obtain the resin composition; then coating the resin composition on the surface of the metal substrate; and (5) placing the metal substrate in a tunnel furnace, baking at 150 ℃ for 25min, and further forming a cured film on the surface of the metal substrate.
(2) Coating 5% potassium permanganate solution on the surface of the cured film, keeping for 8 minutes, cleaning with clear water, and drying at 80 ℃ to form an oxide layer with polar functional groups;
an oxide layer having carboxyl groups is formed on the surface of the cured film by coating potassium permanganate.
(3) The surface of the cured film was coated with 0.02% of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride aqueous solution, and then dried at 80℃to form a catalyst layer.
A catalyst layer is formed on the surface of the cured film by coating 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride. The catalyst can trigger the carboxyl group and the amino group on the surface of the cured film to react in the pressing process to form a covalent bond, so that the bonding strength between the cured film and the insulating composite film with the amino group is improved.
The embodiment also provides an insulated metal plate, and the preparation method of the insulated metal plate comprises the following steps:
(1) Sequentially stacking the metal plate, the heat-conducting insulating film and the electrolytic copper foil provided by the embodiment, so that the curing film in the metal plate faces one surface of the heat-conducting insulating film; placing in a hot press, and pressing at 120deg.C and 60MPa for 60min;
the thickness of the electrolytic copper foil was 70. Mu.m.
The heat conducting insulating film is an uncured heat conducting insulating film, the thickness is 100 mu m, and the heat conducting coefficient is 2.0W/mK. The heat-conducting insulating film comprises, by weight, 9 parts of E51 epoxy resin, 3 parts of dicyandiamide, 0.1 part of dimethyl imidazole, 0.5 part of gamma-aminopropyl triethoxy silicon, 80 parts of spherical aluminum oxide, 0.5 part of antioxidant BHT, 2 parts of carboxyl-terminated nitrile rubber, 3.4 parts of glycerol triglycidyl ether and 1.5 parts of polyvinyl butyral.
In the lamination process, carboxyl groups on the surface of the cured film can react with amino groups on the surface of the heat-conducting insulating film under the catalysis of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to form covalent bonds, so that the bonding strength between the metal plate and the heat-conducting insulating film is improved.
(2) Pressing at 160deg.C and 80MPa for 90min;
(3) Pressing at 200deg.C and 120MPa for 120min, and taking out to obtain the insulating metal plate.
Comparative example 1
The comparative example provides an insulated metal plate, which is prepared by the following steps:
(1) Sequentially stacking a metal plate, a heat-conducting insulating film and an electrolytic copper foil, so that a cured film in the metal plate faces one surface of the heat-conducting insulating film; placing in a hot press, and pressing at 120deg.C and 60MPa for 60min;
the metal plate was a 5052 series of aluminum plates 1.5mm thick.
The thickness of the electrolytic copper foil was 70. Mu.m.
The heat conducting insulating film is an uncured heat conducting insulating film, the thickness is 100 mu m, and the heat conducting coefficient is 2.0W/mK. The heat-conducting insulating film comprises, by weight, 9 parts of E51 epoxy resin, 3 parts of dicyandiamide, 0.1 part of dimethyl imidazole, 0.5 part of gamma-aminopropyl triethoxy silicon, 80 parts of spherical aluminum oxide, 0.5 part of antioxidant BHT, 2 parts of carboxyl-terminated nitrile rubber, 3.4 parts of glycerol triglycidyl ether and 1.5 parts of polyvinyl butyral.
(2) Pressing at 160deg.C and 80MPa for 90min;
(3) Pressing at 200deg.C and 120MPa for 120min, and taking out to obtain the insulating metal plate.
Comparative example 2
The comparative example provides a metal plate, which is prepared by the following steps:
(1) Coating a resin composition on the surface of a metal substrate to form a cured film;
the resin composition comprises, by weight, 4.5 parts of an o-cresol novolac epoxy resin, 2.0 parts of dicyandiamide, 0.1 part of dimethyl imidazole, 0.5 part of gamma-aminopropyl triethoxysilane, 2.0 parts of carboxyl terminated nitrile rubber, 0.1 part of an antioxidant BHT and 90.8 parts of N, N-dimethylformamide. The thickness of the cured film was 1. Mu.m.
The metal substrate was a 5052 series of aluminum plates 1.5mm thick.
Specifically, sequentially adding o-cresol novolac epoxy resin, dicyandiamide, dimethyl imidazole, gamma-aminopropyl triethoxysilane, carboxyl-terminated nitrile rubber and 2, 6-di-tert-butyl-p-cresol into N, N-dimethylformamide, and uniformly stirring to obtain the resin composition; then coating the resin composition on the surface of the metal substrate; and (5) placing the metal substrate in a tunnel furnace, baking at 150 ℃ for 25min, and further forming a cured film on the surface of the metal substrate.
(2) And (3) coating 5% potassium permanganate solution on the surface of the cured film, keeping for 8 minutes, cleaning with clear water, and drying at 80 ℃ to form an oxide layer.
The comparative example also provides an insulated metal sheet, which is prepared by:
(1) The metal plate, the heat-conducting insulating film and the electrolytic copper foil provided in this comparative example were laminated in this order, so that the cured film in the metal plate faced one side of the heat-conducting insulating film; placing in a hot press, and pressing at 120deg.C and 60MPa for 60min;
the thickness of the electrolytic copper foil was 70. Mu.m.
The heat conducting insulating film is an uncured heat conducting insulating film, the thickness is 100 mu m, and the heat conducting coefficient is 2.0W/mK. The heat-conducting insulating film comprises, by weight, 9 parts of E51 epoxy resin, 3 parts of dicyandiamide, 0.1 part of dimethyl imidazole, 0.5 part of gamma-aminopropyl triethoxy silicon, 80 parts of spherical aluminum oxide, 0.5 part of antioxidant BHT, 2 parts of carboxyl-terminated nitrile rubber, 3.4 parts of glycerol triglycidyl ether and 1.5 parts of polyvinyl butyral.
(2) Pressing at 160deg.C and 80MPa for 90min;
(3) Pressing at 200deg.C and 120MPa for 120min; and then taking out to obtain the insulated metal plate.
Comparative example 3
The comparative example provides a metal plate, which is prepared by the following steps: and coating the resin composition on the surface of the metal substrate to form a cured film, thereby obtaining the metal plate.
The resin composition comprises, by weight, 4.5 parts of an o-cresol novolac epoxy resin, 2.0 parts of dicyandiamide, 0.1 part of dimethyl imidazole, 0.5 part of gamma-aminopropyl triethoxysilane, 2.0 parts of carboxyl terminated nitrile rubber, 0.1 part of an antioxidant BHT and 90.8 parts of N, N-dimethylformamide. The thickness of the cured film was 1. Mu.m.
The metal substrate was a 5052 series of aluminum plates 1.5mm thick.
Specifically, sequentially adding o-cresol novolac epoxy resin, dicyandiamide, dimethyl imidazole, gamma-aminopropyl triethoxysilane, carboxyl-terminated nitrile rubber and 2, 6-di-tert-butyl-p-cresol into N, N-dimethylformamide, and uniformly stirring to obtain the resin composition; then coating the resin composition on the surface of the metal substrate; and (5) placing the metal substrate in a tunnel furnace, baking at 150 ℃ for 25min, and further forming a cured film on the surface of the metal substrate.
The comparative example also provides an insulated metal sheet, which is prepared by:
(1) The metal plate, the heat-conducting insulating film and the electrolytic copper foil provided in this comparative example were laminated in this order, so that the cured film in the metal plate faced one side of the heat-conducting insulating film; placing in a hot press, and pressing at 120deg.C and 60MPa for 60min;
the thickness of the electrolytic copper foil was 70. Mu.m.
The heat conducting insulating film is an uncured heat conducting insulating film, the thickness is 100 mu m, and the heat conducting coefficient is 2.0W/mK. The heat-conducting insulating film comprises, by weight, 9 parts of E51 epoxy resin, 3 parts of dicyandiamide, 0.1 part of dimethyl imidazole, 0.5 part of gamma-aminopropyl triethoxy silicon, 80 parts of spherical aluminum oxide, 0.5 part of antioxidant BHT, 2 parts of carboxyl-terminated nitrile rubber, 3.4 parts of glycerol triglycidyl ether and 1.5 parts of polyvinyl butyral.
(2) Pressing at 160deg.C and 80MPa for 90min;
(3) Pressing at 200deg.C and 120MPa for 120min, and taking out to obtain the insulating metal plate.
Comparative example 4
The comparative example provides a metal plate, which is prepared by the following steps:
(1) Coating a resin composition on the surface of a metal substrate to form a cured film;
the resin composition comprises, by weight, 4.5 parts of an o-cresol novolac epoxy resin, 2.0 parts of dicyandiamide, 0.1 part of dimethyl imidazole, 0.5 part of gamma-aminopropyl triethoxysilane, 2.0 parts of carboxyl terminated nitrile rubber, 0.1 part of an antioxidant BHT and 90.8 parts of N, N-dimethylformamide. The thickness of the cured film was 1. Mu.m.
The metal substrate was a 5052 series of aluminum plates 1.5mm thick.
Specifically, sequentially adding o-cresol novolac epoxy resin, dicyandiamide, dimethyl imidazole, gamma-aminopropyl triethoxysilane, carboxyl-terminated nitrile rubber and 2, 6-di-tert-butyl-p-cresol into N, N-dimethylformamide, and uniformly stirring to obtain the resin composition; then coating the resin composition on the surface of the metal substrate; and (5) placing the metal substrate in a tunnel furnace, baking at 150 ℃ for 25min, and further forming a cured film on the surface of the metal substrate.
(2) Coating 0.02% of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride aqueous solution on the surface of the cured film, and then drying at 80 ℃ to form a catalyst layer;
(3) And (3) coating 5% potassium permanganate solution on the surface of the cured film, keeping for 8 minutes, cleaning with clear water, and drying at 80 ℃ to form an oxide layer.
The comparative example also provides an insulated metal sheet, which is prepared by:
(1) The metal plate, the heat-conducting insulating film and the electrolytic copper foil provided in this comparative example were laminated in this order, so that the cured film in the metal plate faced one side of the heat-conducting insulating film; placing in a hot press, and pressing at 120deg.C and 60MPa for 60min;
the thickness of the electrolytic copper foil was 70. Mu.m.
The heat conducting insulating film is an uncured heat conducting insulating film, the thickness is 100 mu m, and the heat conducting coefficient is 2.0W/mK. The heat-conducting insulating film comprises, by weight, 9 parts of E51 epoxy resin, 3 parts of dicyandiamide, 0.1 part of dimethyl imidazole, 0.5 part of gamma-aminopropyl triethoxy silicon, 80 parts of spherical aluminum oxide, 0.5 part of antioxidant BHT, 2 parts of carboxyl-terminated nitrile rubber, 3.4 parts of glycerol triglycidyl ether and 1.5 parts of polyvinyl butyral.
(2) Pressing at 160deg.C and 80MPa for 90min;
(3) Pressing at 200deg.C and 120MPa for 120min, and taking out to obtain the insulating metal plate.
Comparative example 5
The comparative example provides a metal plate, which is prepared by the following steps:
(1) Coating a resin composition on the surface of a metal substrate to form a cured film;
the resin composition comprises, by weight, 4.5 parts of an o-cresol novolac epoxy resin, 2.0 parts of dicyandiamide, 0.1 part of dimethyl imidazole, 0.5 part of gamma-aminopropyl triethoxysilane, 2.0 parts of carboxyl terminated nitrile rubber, 0.1 part of an antioxidant BHT and 90.8 parts of N, N-dimethylformamide. The thickness of the cured film was 1. Mu.m.
The metal substrate was a 5052 series of aluminum plates 1.5mm thick.
Specifically, sequentially adding o-cresol novolac epoxy resin, dicyandiamide, dimethyl imidazole, gamma-aminopropyl triethoxysilane, carboxyl-terminated nitrile rubber and 2, 6-di-tert-butyl-p-cresol into N, N-dimethylformamide, and uniformly stirring to obtain the resin composition; then coating the resin composition on the surface of the metal substrate; and (5) placing the metal substrate in a tunnel furnace, baking at 150 ℃ for 25min, and further forming a cured film on the surface of the metal substrate.
(2) The surface of the cured film was coated with 0.02% of an aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, and the film was dried at 80℃to form a catalyst layer.
The comparative example also provides an insulated metal sheet, which is prepared by:
(1) The metal plate, the heat-conducting insulating film and the electrolytic copper foil provided in this comparative example were laminated in this order, so that the cured film in the metal plate faced one side of the heat-conducting insulating film; placing in a hot press, and pressing at 120deg.C and 60MPa for 60min;
the thickness of the electrolytic copper foil was 70. Mu.m.
The heat conducting insulating film is an uncured heat conducting insulating film, the thickness is 100 mu m, and the heat conducting coefficient is 2.0W/mK. The heat-conducting insulating film comprises, by weight, 9 parts of E51 epoxy resin, 3 parts of dicyandiamide, 0.1 part of dimethyl imidazole, 0.5 part of gamma-aminopropyl triethoxy silicon, 80 parts of spherical aluminum oxide, 0.5 part of antioxidant BHT, 2 parts of carboxyl-terminated nitrile rubber, 3.4 parts of glycerol triglycidyl ether and 1.5 parts of polyvinyl butyral.
(2) Pressing at 160deg.C and 80MPa for 90min;
(3) Pressing at 200deg.C and 120MPa for 120min, and taking out to obtain the insulating metal plate.
Performance testing
1. Tensile Strength test
Sample: the insulated metal sheets provided in example 1 and comparative examples 1-5;
the testing method comprises the following steps: cutting two strip-shaped substrates of 80mm×10mm on an insulating metal plate; respectively etching square copper foil patterns at the positions 10mm away from the edges at one ends of the two strip-shaped substrates; the copper foil positions of the two strip-shaped substrates were soldered together by solder paste as a test sample. And (3) carrying out a tensile test by a tensile machine provided by Sansi corporation, respectively stretching the two strip-shaped substrates in a direction far away from the copper foil pattern, wherein the stretching speed is 2mm/min, and recording the stretching damage degree and the stretching strength.
The tensile failure strength and the tensile strength of the insulated metal sheets provided in example 1 and comparative examples 1 to 5 are shown in table 1.
Table 1 tensile test results for each test specimen
| Group of | Tensile Strength (MPa) | Degree of destruction |
| Insulating Metal sheet provided in example 1 | 18.7 | Interlayer tearing of cured film and heat-conducting insulating film |
| Comparative example 1 provides an insulated metal sheet | 8.1 | Interlayer falling-off of metal plate and heat-conducting insulating film |
| Comparative example 2 provides an insulated metal sheet | 13.4 | Interlayer falling-off of metal plate and heat-conducting insulating film |
| Comparative example 3 provides an insulated metal sheet | 8.7 | Interlayer tearing of cured film and heat-conducting insulating film |
| Comparative example 4 provides an insulated metal sheet | 8.3 | Interlayer tearing of cured film and heat-conducting insulating film |
| Comparative example 5 provides an insulated metal sheet | 3.8 | Interlayer falling-off of metal plate and heat-conducting insulating film |
According to table 1, forming only the cured film on the metal substrate has substantially no effect of improving the bonding strength between the metal plate and the heat conductive insulating film; only coating a catalyst after forming a curing film on the metal substrate, and reacting the bonding strength of the metal plate and the heat-conducting insulating film; after forming a curing film on a metal substrate, sequentially coating a catalyst and potassium permanganate, wherein the catalyst and the potassium permanganate have no effect of improving the bonding strength of the metal plate and the heat-conducting insulating film; only potassium permanganate is coated after a curing film is formed on the metal substrate, so that the bonding strength of the metal plate and the heat-conducting insulating film is improved to a certain extent; and after forming a curing film on the metal substrate, sequentially coating potassium permanganate and a catalyst, wherein the bonding strength between the metal plate and the heat-conducting insulating film is highest.
Therefore, the combination strength of the metal plate and the heat conduction insulating film in the insulating metal plate manufactured by the metal plate is improved through the synergistic effect of the curing film, the potassium permanganate and the catalyst.
2. Tensile Strength test after high temperature
Sample: the insulated metal sheets provided in example 1 and comparative examples 1-2;
the testing method comprises the following steps:
(1) Placing the insulated metal plate in a tin furnace with the temperature of 288 ℃ for tin bleaching for 30min, and then cooling to room temperature to obtain the insulated metal plate after high temperature;
(2) Cutting two strip-shaped substrates of 80mm multiplied by 10mm on the insulated metal plate after the high temperature; respectively etching square copper foil patterns at the positions 10mm away from the edges at one ends of the two strip-shaped substrates; the copper foil positions of the two strip-shaped substrates were soldered together by solder paste as a test sample. The tensile test is carried out by a tensile machine provided by Sansi corporation, the two strip-shaped substrates are respectively stretched in the direction far away from the copper foil pattern, the stretching speed is 2mm/min, and the tensile strength is recorded.
The tensile strength of the insulated metal sheets provided in example 1 and comparative examples 1-2 after high temperature is shown in Table 2.
TABLE 2 tensile test results of each test specimen after high temperature
| Group of | Tensile Strength (MPa) |
| Insulating Metal sheet provided in example 1 | 17.8 |
| Comparative example 1 provides an insulated metal sheet | 5.3 |
| Comparative example 2 provides an insulated metal sheet | 10.8 |
According to table 2, after tin bleaching at high temperature, the bonding strength between the metal plate and the insulating composite film is reduced from 18.7MPa to 17.8MPa, and the bonding strength is reduced by 4.81%; after tin bleaching at high temperature, the bonding strength between the metal plate and the insulating composite film is reduced from 8.1MPa to 5.3MPa, and the bonding strength is reduced by 34.57%; after tin bleaching at high temperature, the bonding strength between the metal plate and the insulating composite film is reduced from 13.4MPa to 10.8MPa, and the bonding strength is reduced by 19.40%.
Therefore, the insulating metal sheet provided in example 1 still maintains a high bonding strength between the metal sheet and the insulating composite film after being placed at a high temperature; is suitable for use in high temperature environment.
Finally, it should be understood that the foregoing embodiments are merely illustrative of the technical solutions of the present invention, and that although the present invention has been described in detail with reference to the above preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the technical solutions of the present invention.
Claims (7)
1. A method for producing a metal plate, comprising the steps of:
coating a resin composition on the surface of a metal substrate to form a cured film;
coating an oxidant on the surface of the cured film to form an oxide layer with polar functional groups; the polar functional group is at least one of hydroxyl, carbonyl or carboxyl;
coating a catalyst on the surface of the cured film to form a catalyst layer; the catalyst is 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride.
2. The method of claim 1, wherein the oxidizing agent is a permanganate.
3. A metal sheet, characterized by being produced by the production method according to any one of claims 1 to 2.
4. A metal plate according to claim 3, wherein the metal substrate is a copper substrate, an aluminum substrate or a stainless steel substrate.
5. An insulating metal plate is characterized by comprising a metal plate, a heat-conducting insulating film and a metal foil; the metal plate is the metal plate according to claim 3 or 4; the heat-conducting insulating film contains amino groups.
6. The method for producing an insulated metal plate according to claim 5, comprising the steps of:
and sequentially laminating the metal plate, the heat-conducting insulating film and the metal foil, and pressing to obtain the insulating metal plate.
7. Use of an insulated metal sheet according to claim 5 for the manufacture of an electronic device.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104476847A (en) * | 2014-12-02 | 2015-04-01 | 广州方邦电子有限公司 | Flexible copper-clad plate having high peel strength and manufacture method thereof |
| WO2019026382A1 (en) * | 2017-08-02 | 2019-02-07 | 株式会社新技術研究所 | Composite of metal and resin |
| CN112694719A (en) * | 2020-12-29 | 2021-04-23 | 浙江华正新材料股份有限公司 | Resin composition, preparation method thereof and metal substrate |
| CN213891598U (en) * | 2020-11-26 | 2021-08-06 | 南雄鸿硕电线材料有限公司 | Anti-scratch double-conductive copper foil |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104476847A (en) * | 2014-12-02 | 2015-04-01 | 广州方邦电子有限公司 | Flexible copper-clad plate having high peel strength and manufacture method thereof |
| WO2019026382A1 (en) * | 2017-08-02 | 2019-02-07 | 株式会社新技術研究所 | Composite of metal and resin |
| CN110997314A (en) * | 2017-08-02 | 2020-04-10 | 株式会社新技术研究所 | Composite material of metal and resin |
| CN213891598U (en) * | 2020-11-26 | 2021-08-06 | 南雄鸿硕电线材料有限公司 | Anti-scratch double-conductive copper foil |
| CN112694719A (en) * | 2020-12-29 | 2021-04-23 | 浙江华正新材料股份有限公司 | Resin composition, preparation method thereof and metal substrate |
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