CN108611670B - Preparation method of high-thermal-conductivity insulating base material - Google Patents
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
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- C25D11/04—Anodisation of aluminium or alloys based thereon
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- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/61—Additives non-macromolecular inorganic
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/66—Additives characterised by particle size
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/66—Additives characterised by particle size
- C09D7/69—Particle size larger than 1000 nm
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/026—Anodisation with spark discharge
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/18—After-treatment, e.g. pore-sealing
- C25D11/24—Chemical after-treatment
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
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- C08K2003/0812—Aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
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- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a preparation method of a high-thermal-conductivity insulating base material, which comprises the steps of firstly preparing a high-thermal-conductivity insulating composite material, secondly oxidizing an aluminum substrate by adopting a micro-arc oxidation process, coating the prepared high-thermal-conductivity insulating composite material on the surface of the oxidized aluminum substrate in a screen printing mode or a spraying mode, and curing to obtain the high-thermal-conductivity insulating base material. The breakdown voltage can reach 50KV/mm, and the insulation resistance can reach 1 x 1014Omega cm, the thermal conductivity can reach 15W/m.K, and the requirements of the PCB industry on the high-thermal-conductivity insulating base material in the market can be met.
Description
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a preparation method of a high-thermal-conductivity insulating base material.
Background
With the progress of science and technology, the requirements on heat conduction materials are higher and higher due to the development of microelectronic integration technology and high-power motors, and the traditional metal and metal oxide heat conduction materials cannot meet the requirements on material insulation and heat conduction in some special occasions. The polymer material has the characteristics of chemical corrosion resistance, excellent electrical insulation performance, excellent mechanical and fatigue resistance and the like, and is widely applied to the current electronic and electrical industry, however, most polymer materials have extremely low thermal conductivity which is generally far less than 1W/m.K, and the application of the polymer materials in the electronic industry is limited.
At present, the most effective method for improving the thermal conductivity of the polymer material is mainly to add a proper amount of high thermal conductive filler into the polymer matrix, and for the thermal conductive material mainly playing the role of insulation, the thermal conductive filler is generally selected from metal oxides (BeO, MgO, Al)2O3NiO, etc.), carbide (SiC, BC, etc.) and metal nitride (AlN, Si, etc.)3N4BN, etc.). The filling type heat conduction insulating high polymer material is formed by adding heat conduction fillers into a common insulating high polymer material and forming a heat conduction network similar to a net or a chain in a high polymer matrix through the interaction between the heat conduction fillers, so that the heat conduction performance is improved.
However, since the powders with good thermal conductivity, such as AlN and BN, are expensive in the thermal conductive filler, and the production cost of the downstream industry is increased, the process for preparing the insulating substrate with high thermal conductivity by using the cheap powders as the filler is urgently needed.
Disclosure of Invention
The invention aims to provide a preparation method of a high-thermal-conductivity insulating base material, which solves the problem that the existing high-thermal-conductivity insulating base material is high in price.
The technical scheme adopted by the invention is that the preparation method of the high-thermal-conductivity insulating base material comprises the following specific steps:
step 1, preparing a high-thermal-conductivity insulating composite material;
step 2, oxidizing the aluminum substrate by adopting a micro-arc oxidation process;
and 3, coating the high-thermal-conductivity insulating composite material prepared in the step 1 on the surface of the aluminum substrate oxidized in the step 2 in a screen printing mode or a spraying mode, and curing to obtain the high-thermal-conductivity insulating base material.
The present invention is also characterized in that,
the filler used in the high-thermal-conductivity insulating composite material in the step 1 is one or more of white carbon black, silicon carbide powder, aluminum oxide powder, nano diamond powder, aluminum/aluminum oxide core-shell powder and the like; the average grain diameter of the filler is 100 nm-5 mu m; the shape of the filler is one or a mixture of a plurality of flaky, dendritic or spherical shapes and the like; the organic carrier is one or more of epoxy resin, phenolic resin, acrylic resin, N-dimethylformamide, dibasic ester, ethyl acetate, diethylenetriamine, polyamide resin, 2-ethyl-4-methylimidazole and other organic substances; wherein the mass ratio of the filler to the organic carrier is 1: 1 to 4.
In the step 2, the thickness of the micro-arc oxidation layer on the surface of the aluminum substrate is 10-100 microns, the porosity is controlled within the range of 0.5-2%, and the structure of the oxidation layer is gamma-Al2O3、α-Al2O3One or a mixture of the two.
And 3, coating the high-thermal-conductivity insulating composite material on the surface of the aluminum substrate oxidized in the step 2, wherein the thickness of the high-thermal-conductivity insulating composite material is controlled to be 5-300 micrometers.
In the step 3, the curing mode can be thermal curing or UV light curing, wherein the thermal curing temperature is 80-150 ℃, the curing time is 0.5-2 hours, the power of a UV light curing machine for UV light curing is 1-20 KW, the conveying speed of a conveying belt is 1-10 m/min, and the distance between an aluminum substrate and a UV lamp is 3-20 cm.
The beneficial effect of the invention is that,
1. according to the preparation method of the high-thermal-conductivity insulating base material, the high-thermal-conductivity insulating composite material is prepared, and then the aluminum substrate is oxidized by adopting a micro-arc oxidation process; and (3) coating the prepared high-thermal-conductivity insulating composite material on the surface of the oxidized aluminum substrate in a screen printing mode or a spraying mode, and curing to obtain the high-thermal-conductivity insulating base material.
2. Compared with the existing high-thermal-conductivity insulating base material, the preparation method of the high-thermal-conductivity insulating base material has the advantages of simpler process and lower cost.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention provides a preparation method of a high-thermal-conductivity insulating base material, which is implemented according to the following steps:
step 1, preparing a high-thermal-conductivity insulating composite material;
the filler used in the high heat-conducting insulating composite material is one or more of white carbon black, silicon carbide powder, aluminum oxide powder, nano diamond powder, aluminum/aluminum oxide core-shell powder and the like; the average grain diameter of the filler is 100 nm-5 mu m; the shape of the filler is one or a mixture of a plurality of flaky, dendritic or spherical shapes and the like; the organic carrier is one or more of epoxy resin, phenolic resin, acrylic resin, N-dimethylformamide, dibasic ester, ethyl acetate, diethylenetriamine, polyamide resin, 2-ethyl-4-methylimidazole and other organic substances; wherein the mass ratio of the filler to the organic carrier is 1: 1 to 4
Step 2, oxidizing the aluminum substrate by adopting a micro-arc oxidation process;
the thickness of the micro-arc oxidation layer on the surface of the aluminum substrate is 10-100 microns, the porosity is controlled within the range of 0.5-2 percent, and the structure of the oxidation layer is gamma-Al2O3、α-Al2O3One or a mixture of the two.
And 3, coating the high-thermal-conductivity insulating composite material prepared in the step 1 on the surface of the aluminum substrate oxidized in the step 2 in a screen printing mode or a spraying mode, and curing to obtain the high-thermal-conductivity insulating base material.
In the step 3, the curing mode can be thermal curing or UV light curing, wherein the thermal curing temperature is 80-150 ℃, the curing time is 0.5-2 hours, the power of a UV light curing machine for UV light curing is 1-20 KW, the conveying speed of a conveying belt is 1-10 m/min, and the distance between an aluminum substrate and a UV lamp is 3-20 cm.
Example 1
Step 1, preparing a high-thermal-conductivity insulating composite material: the used fillers are white carbon black and aluminum oxide powder, and the mass ratio of the fillers is 1: 1; the average particle size of the filler is 100 nm; the shape of the filler is sheet-shaped; the organic carrier is epoxy resin, phenolic resin, N-dimethylformamide and dibasic ester, wherein the mass ratio of white carbon black, aluminum oxide powder, epoxy resin, phenolic resin, N-dimethylformamide to dibasic ester is 1: 1: 4: 2: 1: 5; the mass ratio of the filler to the organic carrier is 1: 1.
step 2, oxidizing the aluminum substrate by adopting a micro-arc oxidation process: the thickness of the micro-arc oxidation layer on the surface of the aluminum substrate is 10 microns, the porosity is controlled to be 0.5 percent, and the structure of the oxidation layer is gamma-Al2O3。
And 3, coating the high-thermal-conductivity insulating composite material prepared in the step 1 on the surface of the aluminum substrate oxidized in the step 2 in a screen printing mode or a spraying mode, wherein the coating thickness is 100 microns, and curing to obtain the high-thermal-conductivity insulating base material: the curing mode can be thermal curing, the temperature of the thermal curing is 150 ℃, and the curing time is 0.5 hour.
Example 2
Step 1, preparing a high-thermal-conductivity insulating composite material: the used filler is aluminum/aluminum oxide core-shell powder; the average particle size of the filler is 5 μm; the shape of the filler is sheet-shaped; the organic carrier is epoxy resin, phenolic resin, N-dimethylformamide and dibasic ester, wherein the mass ratio of the aluminum/aluminum oxide core-shell powder to the epoxy resin to the phenolic resin to the N, N-dimethylformamide to the dibasic ester is 2: 4: 2: 1: 5; wherein the mass ratio of the filler to the organic carrier is 1: 4.
step 2, oxidizing the aluminum substrate by adopting a micro-arc oxidation process: the thickness of the micro-arc oxidation layer on the surface of the aluminum substrate is 100 microns, the porosity is controlled to be 2 percent, and the structure of the oxidation layer is gamma-Al2O3。
And 3, coating the high-thermal-conductivity insulating composite material prepared in the step 1 on the surface of the aluminum substrate oxidized in the step 2 in a screen printing mode or a spraying mode, wherein the coating thickness is 10 microns, and curing to obtain the high-thermal-conductivity insulating base material: the curing mode can be thermal curing, the temperature of the thermal curing is 80 ℃, and the curing time is 2 hours.
Example 3
Step 1, preparing a high-thermal-conductivity insulating composite material: the used fillers are white carbon black and silicon carbide powder; the average particle size of the filler is 500 nm; the shape of the filler is sheet-shaped; the organic carrier is epoxy resin, phenolic resin, N-dimethylformamide and dibasic ester, wherein the mass ratio of white carbon black, silicon carbide powder, epoxy resin, phenolic resin, N-dimethylformamide to dibasic ester is 1.5: 1: 4: 2: 1: 5; wherein the mass ratio of the filler to the organic carrier is 1: 2.
step 2, oxidizing the aluminum substrate by adopting a micro-arc oxidation process: the thickness of the micro-arc oxidation layer on the surface of the aluminum substrate is 50 microns, the porosity is controlled to be 1 percent, and the structure of the oxidation layer is gamma-Al2O3。
And 3, coating the high-thermal-conductivity insulating composite material prepared in the step 1 on the surface of the aluminum substrate oxidized in the step 2 in a screen printing mode or a spraying mode, wherein the coating thickness is 50 microns, and curing to obtain the high-thermal-conductivity insulating base material: the curing mode can be thermal curing, the temperature of the thermal curing is 150 ℃, and the curing time is 1 hour.
Example 4
Step 1, preparing a high-thermal-conductivity insulating composite material: the used filler is aluminum/aluminum oxide core-shell powder; the average particle size of the filler is 100 nm; the shape of the filler is sheet-shaped; the organic carrier is epoxy resin, phenolic resin, N-dimethylformamide and dibasic ester, wherein the mass ratio of the aluminum/aluminum oxide core-shell powder to the epoxy resin to the phenolic resin to the 2-ethyl-4-methylimidazole to the dibasic ester is 2: 4: 2: 0.5: 5; wherein the mass ratio of the filler to the organic carrier is 1: 2.
step 2, oxidizing the aluminum substrate by adopting a micro-arc oxidation process: the thickness of the micro-arc oxidation layer on the surface of the aluminum substrate is 50 microns, the porosity is controlled to be 1 percent, and the structure of the oxidation layer is gamma-Al2O3。
And 3, coating the high-thermal-conductivity insulating composite material prepared in the step 1 on the surface of the aluminum substrate oxidized in the step 2 in a screen printing mode or a spraying mode, wherein the coating thickness is 300 microns, and curing to obtain the high-thermal-conductivity insulating base material: the curing mode can be UV light curing, the power of a UV light curing machine is 1KW, the conveying speed of the conveying belt is 1 m/min, and the distance between the aluminum substrate and the UV lamp is 3 cm.
Example 5
Step 1, preparing a high-thermal-conductivity insulating composite material: the used filler is aluminum/aluminum oxide core-shell powder; the average particle size of the filler is 100 nm; the shape of the filler is sheet-shaped; the organic carrier is epoxy resin, phenolic resin, N-dimethylformamide and dibasic ester, wherein the mass ratio of the aluminum/aluminum oxide core-shell powder to the epoxy resin to the phenolic resin to the 2-ethyl-4-methylimidazole to the dibasic ester is 2: 4: 2: 0.5: 5; wherein the mass ratio of the filler to the organic carrier is 1: 3.
step 2, oxidizing the aluminum substrate by adopting a micro-arc oxidation process: the thickness of the micro-arc oxidation layer on the surface of the aluminum substrate is 50 microns, the porosity is controlled to be 1 percent, and the structure of the oxidation layer is gamma-Al2O3。
And 3, coating the high-thermal-conductivity insulating composite material prepared in the step 1 on the surface of the aluminum substrate oxidized in the step 2 in a screen printing mode or a spraying mode, wherein the coating thickness is 50 microns, and curing to obtain the high-thermal-conductivity insulating base material: the curing mode can be UV light curing, the power of a UV light curing machine is 20KW, the conveying speed of the conveying belt is 10 m/min, and the distance between the aluminum substrate and the UV lamp is 20 cm.
TABLE 1 breakdown Voltage, thermal conductivity and insulation resistance Properties of high thermal conductivity insulation substrate
The invention has the advantages that:
1. according to the preparation method of the high-thermal-conductivity insulating base material, the high-thermal-conductivity insulating composite material is prepared, and then the aluminum substrate is oxidized by adopting a micro-arc oxidation process; and (3) coating the prepared high-thermal-conductivity insulating composite material on the surface of the oxidized aluminum substrate in a screen printing mode or a spraying mode, and curing to obtain the high-thermal-conductivity insulating base material.
2. Compared with the existing high-thermal-conductivity insulating base material, the preparation method of the high-thermal-conductivity insulating base material has the advantages of simpler process and lower cost.
Claims (4)
1. A preparation method of a high-thermal-conductivity insulating base material is characterized by comprising the following specific steps:
step 1, preparing a high-thermal-conductivity insulating composite material;
step 2, oxidizing the aluminum substrate by adopting a micro-arc oxidation process;
step 3, coating the high-thermal-conductivity insulating composite material prepared in the step 1 on the surface of the aluminum substrate oxidized in the step 2 in a screen printing mode or a spraying mode, and curing to obtain a high-thermal-conductivity insulating base material;
the filler used in the high-thermal-conductivity insulating composite material in the step 1 is one or more of white carbon black, silicon carbide powder, aluminum oxide powder, nano diamond powder and aluminum/aluminum oxide core-shell powder; the average grain diameter of the filler is 100 nm-5 mu m; the shape of the filler is one or a mixture of a plurality of flaky, dendritic or spherical fillers; the organic carrier is epoxy resin, phenolic resin, N-dimethylformamide and dibasic ester; wherein the ratio of the filler to the organic carrier is 1: 1 to 4.
2. The method for preparing the insulating base material with high thermal conductivity according to claim 1, wherein the thickness of the micro-arc oxide layer on the surface of the aluminum substrate oxidized in the step 2 is 10 to 100 microns, the porosity is 0.5 to 2 percent, and the structure of the oxide layer is gamma-Al2O3、α-Al2O3One or a mixture of the two.
3. The method for preparing the high thermal conductivity insulating base material according to claim 1, wherein the thickness of the high thermal conductivity insulating composite material coated on the surface of the aluminum substrate oxidized in the step 2 in the step 3 is 5 to 300 micrometers.
4. The preparation method of the insulating base material with high thermal conductivity according to claim 1, wherein the curing manner in step 3 is thermal curing or UV light curing, wherein the temperature for thermal curing is 80 ℃ to 150 ℃, and the curing time is 0.5 hour to 2 hours; the power of the UV light curing machine for UV light curing is 1 KW-20 KW, the conveying speed of the conveying belt is 1 m/min-10 m/min, and the distance between the aluminum substrate and the UV lamp is 3 cm-20 cm.
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Application publication date: 20181002 Assignee: Pucheng Zhenggong Gas Co.,Ltd. Assignor: XI'AN POLYTECHNIC University Contract record no.: X2023980034734 Denomination of invention: A preparation method for high thermal conductivity insulation substrate Granted publication date: 20200619 License type: Common License Record date: 20230419 |