CN111883362A - Graphene aluminum-based conductive coating and preparation method thereof - Google Patents
Graphene aluminum-based conductive coating and preparation method thereof Download PDFInfo
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- CN111883362A CN111883362A CN202010735553.7A CN202010735553A CN111883362A CN 111883362 A CN111883362 A CN 111883362A CN 202010735553 A CN202010735553 A CN 202010735553A CN 111883362 A CN111883362 A CN 111883362A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/022—Electrolytes; Absorbents
- H01G9/025—Solid electrolytes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/0029—Processes of manufacture
- H01G9/0036—Formation of the solid electrolyte layer
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/15—Solid electrolytic capacitors
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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Abstract
The invention provides a graphene aluminum-based conductive coating which is prepared by coating a graphene-containing conductive agent, a dispersing agent and silica sol on an aluminum-based substrate. The coating does not contain organic resin, has good conductivity, strong adhesive force and good high-temperature resistance (above 300 ℃), and is completely prepared by a water-based system in a coating process, so that the coating is environment-friendly and pollution-free.
Description
Technical Field
The invention belongs to the field of aluminum electrolytic capacitors, and particularly relates to a graphene aluminum-based conductive coating and a preparation method thereof.
Background
The common capacitor (namely the liquid aluminum electrolytic capacitor) dielectric material is electrolyte, and the commonly known mainboard slurry explosion is the good work of the electrolytic capacitor, because the electrolyte expands due to overheating in the long-term use process of the mainboard, the electrolyte exceeds the boiling point to generate slurry explosion after overheating to a certain degree, and in addition, the electrolyte reacts with aluminum oxide to possibly cause slurry explosion under the condition that a host is electrified. Compared with the common capacitor (namely the liquid aluminum electrolytic capacitor), the solid capacitor adopts the conductive polymer product as the dielectric material, the material can not react with aluminum oxide, and the explosion phenomenon can not occur after the power is on; meanwhile, the product is a solid product, and the situation of explosion caused by thermal expansion does not exist naturally.
At present, a solid capacitor (solid aluminum electrolytic capacitor) adopted by a high-end mainboard is formed by coating high-temperature-resistant conductive polymers on an aluminum foil, the high-temperature-resistant conductive polymer material is high in cost and uneven in conductivity, waste liquid and emission generated in the synthetic preparation process are harmful to the environment, the high-temperature-resistant conductive polymer material is not environment-friendly, most of resin cannot resist the high temperature of more than 300 ℃, part of resin begins to decompose when the resin is at 260 ℃ due to the characteristics of the resin, the resin cannot be used at high temperature, most of the resin is an oily system, and the environment is greatly polluted.
Disclosure of Invention
Based on the above background art, the problems of environmental pollution, high cost and limitation of high temperature resistance existing in the coating of high temperature resistant conductive polymers adopted by aluminum-based materials are solved by the following scheme:
a graphene aluminum-based conductive coating is prepared by coating a conductive agent containing graphene, a dispersant and silica sol on an aluminum-based substrate.
Further, the conductive agent also comprises carbon nanotubes.
Further, the weight ratio of the conductive agent to the silica of the silica sol is 1:3-1: 2.
Further, the dispersing agent is one or more of polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, acrylic acid, acrylonitrile or polyether.
The preparation method of the graphene aluminum-based conductive coating comprises the following steps:
1) uniformly mixing and dispersing a conductive agent, deionized water, a dispersing agent and silica sol to prepare graphene water-based adhesive;
2) carrying out blade coating on the graphene aqueous adhesive on an aluminum-based substrate to form a film, and drying;
3) and (4) performing high-temperature treatment under the protection of inert gas.
Further, the drying temperature is 50-100 ℃, and the high-temperature treatment temperature is 300-.
Further, the aluminum-based material is subjected to a roughening treatment before the blade coating.
Further, the roughening treatment is plasma treatment or sand blasting treatment.
A solid capacitor is provided with the graphene aluminum-based conductive coating.
The graphene aluminum-based conductive coating is prepared by coating a conductive agent containing graphene, a dispersing agent and silica sol on an aluminum substrate, and the coating does not contain organic resin, has good conductivity, strong adhesive force and good high temperature resistance (above 300 ℃), can completely adopt a water-based system during coating preparation, and is environment-friendly and pollution-free.
Drawings
Adhesion test adhesion grade distribution diagram in the embodiment of FIG. 1
Detailed Description
The invention discovers that a high-temperature-resistant coating with good conductivity and strong adhesive force can be formed by coating a graphene-containing conductive agent, a dispersing agent and silica sol on an aluminum substrate, so that the specific embodiment of the invention provides a graphene aluminum-based conductive coating, and the coating is prepared by coating the graphene-containing conductive agent, the dispersing agent and the silica sol on the aluminum-based substrate.
The graphene aluminum-based conductive coating of the embodiment of the invention is light as an excellent material, has super-strong conductivity, has electron mobility 100 times higher than that of carbon tubes and crystalline silicon, and can reach 15000cm2/(V.s) at room temperature. The resistivity is much lower than that of aluminum, copper and silver, and is only about 10-6 omega cm. Meanwhile, the thermal conductivity coefficient is as high as 5300W/m.K, which is far higher than that of other traditional metal materials, such as copper, aluminum and the like. SiO2 in the silica sol can not be decomposed at high temperature such as 350 ℃, but part of SiO2 and aluminum on the surface of the coating can generate Al2O3 at high temperature in the protection of inert atmosphere, so that the coating and the aluminum foil are bonded by chemical bonds, and the adhesive force of the coating on the aluminum foil is improved.
According to the graphene aluminum-based conductive coating provided by the embodiment of the invention, the number of graphene layers is less than 30.
According to the graphene aluminum-based conductive coating provided by the embodiment of the invention, the conductive agent further comprises carbon nanotubes. The carbon nano tube has the characteristics of excellent electrical conductivity, light weight, high thermal conductivity coefficient and the like, the excellent characteristics enable graphene and the carbon nano tube to be used as perfect fillers in the conductive coating, the electrical conductivity is excellent, the weight is light, the thermal conductivity coefficient is high, and the problems of weight reduction, electric conduction, heat dissipation and the like of the solid capacitor can be well solved. The carbon nano tube is combined with the graphene in a linear surface mode, so that the whole coating can be better covered, a conductive network in the coating is formed, and the conductivity of the coating is improved. With the maturity of the preparation process of graphene and carbon nanotubes, the product price is continuously reduced, and the quality is continuously improved.
According to the graphene aluminum-based conductive coating provided by the embodiment of the invention, the pipe diameter of the carbon nano tube is within 50 nm.
In the graphene aluminum-based conductive coating according to the embodiment of the present invention, the addition amount of the carbon nanotube is within 50% by weight, preferably within 30% by weight of the conductive agent.
The graphene aluminum-based conductive coating provided by the embodiment of the invention comprehensively considers the adhesive force and the conductive performance of the coating, and the weight ratio of the conductive agent to the silicon dioxide of the silica sol is 1:3-1: 2.
According to the graphene aluminum-based conductive coating provided by the embodiment of the invention, the dispersing agent is one or more of polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, acrylic acid, acrylonitrile or polyether, and the dispersing agent enables the graphene to have good wettability with water, can promote the graphene to be dispersed, wetted and stripped better, and can improve the stability of the coating slurry.
According to the graphene aluminum-based conductive coating provided by the embodiment of the invention, the aluminum-based substrate is an aluminum foil.
The specific embodiment of the invention also provides a preparation method of the graphene aluminum-based conductive coating, which comprises the following steps:
1) uniformly mixing and dispersing a conductive agent, deionized water, a dispersing agent and silica sol to prepare graphene water-based adhesive;
2) carrying out blade coating on the graphene aqueous adhesive on an aluminum-based substrate to form a film, and drying;
3) and (4) performing high-temperature treatment under the protection of inert gas.
According to the preparation method of the graphene aluminum-based conductive coating, the drying temperature is 50-100 ℃, the drying time is 0.5-5h, the high-temperature treatment temperature is 300-600 ℃, and the high-temperature treatment time is 1-10 h.
According to the preparation method of the graphene aluminum-based conductive coating, the aluminum-based material is roughened before blade coating, and the micro surface of the roughened aluminum foil is roughened and becomes hydrophilic from hydrophobic, so that the binding force between the coating and the aluminum-based surface is improved.
According to the preparation method of the graphene aluminum-based conductive coating, the roughening treatment is plasma treatment or sand blasting treatment.
According to the preparation method of the graphene aluminum-based conductive coating, the conductive agent, the deionized water, the dispersing agent and the silica sol are uniformly mixed and dispersed by using the grinding and dispersing equipment, wherein the grinding and dispersing equipment is a high-speed dispersing machine, a planetary ball mill, a high-energy ball mill, a vibration ball mill, a sand mill or a homogenizer and the like.
According to the preparation method of the graphene aluminum-based conductive coating, disclosed by the specific embodiment of the invention, a high-temperature inert gas protection furnace is used for high-temperature treatment under the protection of inert gas, and the protection furnace is a tubular furnace, an atmosphere protection box type furnace, a high-temperature vacuum atmosphere furnace and the like.
According to the preparation method of the graphene aluminum-based conductive coating, the inert gas is nitrogen, helium, argon and the like.
The specific embodiment of the invention also provides a solid capacitor which is provided with the graphene aluminum-based conductive coating, and the capacitor can be widely applied to various electronic products, such as computers, projectors and the like.
The following is a further description by way of specific examples.
Examples
Description of the test:
and (3) conductivity test: the coated aluminum foil is cut into samples with proper sizes (the minimum sample size is 4mm x 10mm), an SZT-C test bench is adopted, an ST2258B-F02 type probe is used in a matching mode, the samples are placed on the test bench, the prepared rubber pad is arranged below the samples, the test stability is improved, an R □ grade is selected, and the coefficient is adjusted to measure to obtain the sheet resistance.
And (3) testing the adhesive force: the high temperature adhesive tape (yellow) was taken out at a uniform speed and cut to a length of about 75mm, the tape was placed over the aluminum foil which had been treated at a high temperature, the tape was stuck to the pole piece with a finger, pressed flat, held with one end of the tape suspended in the air, and the tape was torn off smoothly within 0.5 to 1 second at an angle as close to 60 ° as possible. The adhesion on the tape was observed and the adhesion was from weak to strong on a scale of 0 to 5 (see FIG. 1).
Example 1
Taking 4 parts of graphene, 1 part of carbon nano tube, 10 parts of silica sol (calculated by silica dioxide) (namely, 1:2 of conductive agent: silica sol effective component silica dioxide), 1 part of dispersing agent and the rest of deionized water for dispersing and grinding to obtain graphene water-based adhesive;
carrying out plasma roughening treatment on the aluminum foil, carrying out blade coating on the graphene water-based adhesive on the roughened aluminum foil by adopting an automatic coating machine to form a film, and drying at 90 ℃;
cutting and drying the coating, and performing high-temperature treatment for 1h at 350 ℃ in a high-temperature furnace under the protection of inert gas.
The conductivity test and adhesion test were performed on the high-temperature treated coating, and the results are favorable in table 1 below.
Examples 2 to 4
Compared with the embodiment 1, the dosage of the silica sol is changed, and the other dosage is unchanged, so that the ratio of the conductive agent: the silica ratio of the silica sol was changed to 1:1, 1:3, 1: 4.
Example 5
Compared with example 1, the aluminum foil for roughening was changed to a smooth foil without plasma roughening treatment, and the others were not changed.
Example 6
Compared with example 1, the temperature at high temperature was changed to 550 ℃ and the others were not changed.
Example 7
Compared with the embodiment 1, 4 parts of graphene and 1 part of carbon nano tube are changed into 5 parts of graphene and 0 part of carbon nano tube, and the rest parts are unchanged.
Comparative examples 1 to 5
Compared with example 1, the silica sol was changed to water-based polyimide, water-based epoxy resin, water-based silicone modified epoxy resin, water-based acrylic resin, and water-based silicone modified acrylic resin, respectively, and the others were not changed.
TABLE 1 parameters and testing of various examples
It can be seen from examples 1-4 that the ratio of the conductive agent to the adhesive is different, and the corresponding conductivity and adhesion are changed, and the adhesion is increased but the conductivity is decreased with the increase of the silica sol. Examples 1 and 3 have both good conductivity and adhesion.
The example 1 and the example 5 show that the adhesion force of the smooth foil is lower than that of the roughened aluminum foil, and compared with the smooth surface of the smooth foil and the rough and uneven surface of the roughened aluminum foil, the roughened aluminum foil has the advantages of easier formation of gripping force with a coating and stronger adhesion force.
It can be seen from examples 1 and 6 that the silica sol withstands a high temperature of at least 550 ℃ as the temperature rises to 550 ℃ has better conductivity and good adhesion.
In example 1 and example 7, it can be seen that the graphene carbon tube is compounded, and has a synergistic effect and better conductivity.
In comparison with comparative example 1, it can be seen that the silica sol has better conductivity and adhesion and the polyimide is more expensive compared with the polyimide under the same conditions.
Comparative examples 2 and 4, the resins without silicone modification, both had poor adhesion at low levels because the resin decomposed at high temperature, the structure was destroyed, and no good bonding to the substrate was achieved. The silicon modified resin, such as comparative example 3 and comparative example 5, has certain improvement, but is not resistant to 350 ℃, still decomposes and has a damaged structure, so that the adhesive force is enhanced, but still not strong.
Although the present invention is disclosed above, the present invention is not limited thereto. Various changes and modifications may be effected therein by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (9)
1. The graphene aluminum-based conductive coating is characterized in that the coating is prepared by coating a conductive agent containing graphene and silica sol on an aluminum-based substrate.
2. The graphene aluminum-based conductive coating according to claim 1, wherein the conductive agent further comprises carbon nanotubes.
3. The graphene aluminum-based conductive coating according to claim 1, wherein the weight ratio of the conductive agent to the silica in the silica sol is 1:3 to 1: 2.
4. The graphene aluminum-based conductive coating according to claim 1, wherein the dispersant is one or more of polyvinylpyrrolidone, sodium dodecylbenzenesulfonate, acrylic acid, acrylonitrile, or polyether.
5. A method for preparing a graphene aluminum-based conductive coating according to any one of claims 1 to 4, comprising the following steps:
1) uniformly mixing and dispersing a conductive agent, deionized water, a dispersing agent and silica sol to prepare graphene water-based adhesive;
2) carrying out blade coating on the graphene aqueous adhesive on an aluminum-based substrate to form a film, and drying;
3) and (4) performing high-temperature treatment under the protection of inert gas.
6. The method for preparing the graphene aluminum-based conductive coating according to claim 5, wherein the drying temperature is 50-100 ℃, and the high temperature treatment temperature is 300-600 ℃.
7. The method for preparing the graphene aluminum-based conductive coating according to claim 5, wherein the aluminum-based material is roughened before blade coating.
8. The method for preparing a graphene aluminum-based conductive coating according to claim 7, wherein the roughening treatment is a plasma treatment or a sand blasting treatment.
9. A solid state capacitor having a graphene aluminum-based conductive coating according to any one of claims 1 to 4.
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| CN202010735553.7A CN111883362A (en) | 2020-07-28 | 2020-07-28 | Graphene aluminum-based conductive coating and preparation method thereof |
| CN202211561572.8A CN116053041A (en) | 2020-07-28 | 2020-07-28 | Graphene-aluminum-based conductive coating and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0195172A (en) * | 1987-10-06 | 1989-04-13 | Nec Corp | Graphite paste for fluorescent display tube |
| KR20040089969A (en) * | 2003-04-15 | 2004-10-22 | (주) 유니플라텍 | Carbon ink for high temperature use and common use, a continuous type dip-coating apparatus for manufacturing carbon paper, a face-shaped heating unit for high temperature use and common use, and manufacturing method thereof |
| CN106783212A (en) * | 2016-11-22 | 2017-05-31 | 张家港智电芳华蓄电研究所有限公司 | A kind of preparation method of porous carbon electrode |
| CN109517445A (en) * | 2018-11-21 | 2019-03-26 | 济南圣泉集团股份有限公司 | A kind of electric heating ink and its preparation method and application |
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- 2020-07-28 CN CN202010735553.7A patent/CN111883362A/en active Pending
- 2020-07-28 CN CN202211561572.8A patent/CN116053041A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0195172A (en) * | 1987-10-06 | 1989-04-13 | Nec Corp | Graphite paste for fluorescent display tube |
| KR20040089969A (en) * | 2003-04-15 | 2004-10-22 | (주) 유니플라텍 | Carbon ink for high temperature use and common use, a continuous type dip-coating apparatus for manufacturing carbon paper, a face-shaped heating unit for high temperature use and common use, and manufacturing method thereof |
| CN106783212A (en) * | 2016-11-22 | 2017-05-31 | 张家港智电芳华蓄电研究所有限公司 | A kind of preparation method of porous carbon electrode |
| CN109517445A (en) * | 2018-11-21 | 2019-03-26 | 济南圣泉集团股份有限公司 | A kind of electric heating ink and its preparation method and application |
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