CN111105933A - High-compactness, acid-resistant and oxidation-resistant solid capacitor carbon foil production process - Google Patents
High-compactness, acid-resistant and oxidation-resistant solid capacitor carbon foil production process Download PDFInfo
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- CN111105933A CN111105933A CN201811260340.2A CN201811260340A CN111105933A CN 111105933 A CN111105933 A CN 111105933A CN 201811260340 A CN201811260340 A CN 201811260340A CN 111105933 A CN111105933 A CN 111105933A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 54
- 239000007787 solid Substances 0.000 title claims abstract description 30
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- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 25
- 239000002253 acid Substances 0.000 title claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 239000003990 capacitor Substances 0.000 title claims description 20
- 238000003756 stirring Methods 0.000 claims abstract description 48
- 238000002156 mixing Methods 0.000 claims abstract description 34
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- 238000000034 method Methods 0.000 claims abstract description 25
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- 229920005749 polyurethane resin Polymers 0.000 claims description 10
- -1 polyoxyethylene Polymers 0.000 claims description 8
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 claims description 7
- HJVAFZMYQQSPHF-UHFFFAOYSA-N 2-[bis(2-hydroxyethyl)amino]ethanol;boric acid Chemical compound OB(O)O.OCCN(CCO)CCO HJVAFZMYQQSPHF-UHFFFAOYSA-N 0.000 claims description 7
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 7
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 7
- 150000004645 aluminates Chemical class 0.000 claims description 7
- 239000007822 coupling agent Substances 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 7
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- 239000004593 Epoxy Substances 0.000 claims description 6
- 125000005037 alkyl phenyl group Chemical group 0.000 claims description 6
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 6
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 229940116411 terpineol Drugs 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
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- 238000002791 soaking Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 claims description 4
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical group COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 claims description 4
- 239000002518 antifoaming agent Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000005868 electrolysis reaction Methods 0.000 abstract description 4
- 238000005476 soldering Methods 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 3
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- 238000005516 engineering process Methods 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 description 2
- 230000020477 pH reduction Effects 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- WAPNOHKVXSQRPX-UHFFFAOYSA-N 1-phenylethanol Chemical compound CC(O)C1=CC=CC=C1 WAPNOHKVXSQRPX-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
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Images
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
- H01G9/045—Electrodes or formation of dielectric layers thereon characterised by the material based on aluminium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
- H01G9/0425—Electrodes or formation of dielectric layers thereon characterised by the material specially adapted for cathode
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
- H01G9/055—Etched foil electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to a production process of a high-compactness, acid-resistant and oxidation-resistant solid capacitance carbon foil, which comprises the following process steps: adding a half of adhesive into a high molecular solvent, adding a nano conductive carbon fiber system formed by mixing an acidified carbon nano tube and a carbon nano tube, stirring and mixing the nano conductive carbon fiber system with the other half of adhesive and a processing aid to obtain slurry, coating the slurry on two sides of a corrosion aluminum foil by using a gravure coater, wherein the coating thickness is 20-42 mu m, and carrying out interface treatment, rewinding, slitting, inspection and packaging by using a high-temperature furnace to obtain a solid capacitance carbon foil; the special nano conductive slurry is coated on two sides of the corrosion aluminum foil by a coating process, and can be tightly combined and completely covered after interface treatment, so that the process difficulty is reduced, the compactness of the carbon foil is improved, the carbon foil product has excellent thermal oxidation resistance, and the adaptability to heating and patch reflow soldering temperatures in the solid aluminum electrolysis production process is wider.
Description
Technical Field
The invention relates to a production process of a high-compactness, acid-resistant and oxidation-resistant solid capacitor carbon foil, belonging to the technical field of solid capacitor carbon foils.
Background
In view of the problems of liquid electrolytic capacitors, solid aluminum electrolytic capacitors have been developed, and the use of solid aluminum electrolytic capacitors can directly improve the performance of the main board and effectively provide a stable and abundant power supply. The carbon foil of the solid capacitor is used as a special cathode foil material for the solid capacitor, generally an aluminum foil is used as a base die and is compounded with a graphite layer structure, a physical sputtering process is generally adopted in the compounding process, ions bombard the surface of a target material, argon is filled into a vacuum cavity to form a low-pressure argon atmosphere, then high voltage is used to generate glow discharge, ions are accelerated to the surface of the target material, the target material is bombarded, an upper graphite layer and a lower graphite layer are respectively plated through magnetron sputtering, the carbon foil point-like carbon particles prepared by the process are spread and coated, the particles are close to a single layer, and the rolled lines of the aluminum foil are visible; or chemical vapor deposition process, which utilizes one or more gaseous compounds or simple substances containing film elements to perform chemical reaction on the surface of the substrate to generate a film, wherein the carbon foil prepared by the process has poor precision covering performance due to the fact that a punctiform particle accumulation coating contains accumulation pores, and crack regions are easy to appear due to micro-stirring control of the process, so that the acid resistance and oxidation resistance of the carbon foil are influenced, and the service life is shortened.
Disclosure of Invention
The invention aims to provide a high-compactness, acid-resistant and oxidation-resistant solid capacitor carbon foil production process, aiming at the defects of the prior art, the high-compactness, acid-resistant and oxidation-resistant solid capacitor carbon foil production process adopts unique nano conductive slurry, is coated on two sides of a corrosion aluminum foil by a coating process, can be tightly combined and completely covered after interface treatment, is beneficial to reducing the process difficulty and improving the compactness of the carbon foil, and the carbon foil product has excellent thermal oxidation resistance and wider adaptability to heating and patch reflow soldering temperatures in the solid aluminum electrolysis production process.
The invention is realized by the following technical scheme:
a high-compactness, acid-resistant and oxidation-resistant solid capacitance carbon foil production process comprises the following process steps:
(1) preparing slurry:
① soaking and acidifying carbon nanotubes in a mixed solution of concentrated nitric acid and concentrated sulfuric acid for 1-2 h, washing with deionized water to neutrality, drying to obtain acidified carbon nanotubes, and mixing with carbon nanotubes to obtain a nano conductive carbon fiber system;
② adding a binder which accounts for half of the volume of the total binder into a high molecular solvent, wherein the high molecular solvent is selected from several of diethylene glycol monobutyl ether, polyoxyethylene alkyl phenyl ether, methyl benzyl alcohol, N-dimethyl acetamide and terpineol, the binder is one or more of polyester acrylic resin, waterborne polyurethane resin, epoxy acrylic resin and polyurethane resin, stirring and mixing the mixture, adding a nano conductive carbon fiber system, and stirring and mixing the nano conductive carbon fiber system and the high molecular solvent according to the mass ratio of (2-5): 70;
③ adding the other half of the adhesive into the stirring kettle of step ②, stirring and mixing, wherein the mass ratio of the total adhesive to the polymer solvent is (15-20): 70;
④, sequentially adding processing aids into the stirred tank in the step ③, wherein the processing aids comprise triallyl isocyanurate, triethanolamine borate, aluminate coupling agent, antioxidant 1010, polyvinylpyrrolidone and defoamer 3168 in a mass ratio of 4:5:3:1:2:3, and the mass ratio of the processing aids to the high-molecular solvent is (0.4-1.2): 70, and stirring and mixing to obtain slurry;
(2) coating, namely placing the etched aluminum foil on a gravure coater, and coating the slurry prepared in the step (1) on two sides to obtain a foil tape, wherein the coating thickness is 20-42 mu m;
(3) interface treatment: feeding the foil strip into a high-temperature furnace, wherein the heating rate of the high-temperature furnace is 20 ℃/min, heating to 400-450 ℃, preserving heat for 2-3 h, and then reducing the temperature to room temperature at the cooling rate of 10 ℃/min;
(4) rewinding and slitting: inspecting damage of the foil tape subjected to the step (3) by foil reversing, and removing the damage by using a cutting machine;
(5) and (3) inspecting and packaging: and inspecting the foil tape, packaging and warehousing to obtain the solid capacitance carbon foil.
The invention has the beneficial effects that:
(1) the special slurry is adopted, the nano conductive carbon fiber system is dispersed in a high molecular carrier, and the high molecular carrier which is formed by grafting carboxyl and hydroxyl active groups on the interface, an adhesive, a high molecular solvent and a processing aid through acidification has surface tension suitable for covering a carbon foil, improves the interface performance of the nano conductive carbon fiber system and the high molecular solvent, avoids agglomeration and ensures excellent coverage; (2) the coating method is used for replacing the traditional physical sputtering or chemical vapor deposition method, so that the carbon-containing slurry is spread with the carbon layer, the carbon layer can be completely and uniformly loaded on the surface of the corroded aluminum foil substrate, the slurry is bonded with the aluminum substrate through interaction by high-temperature interface treatment, the load is effectively transferred, poor interface reactants can be inhibited, the combination is reliable, the carbon foil is not easy to fall off, the process difficulty is greatly reduced, the compactness of the carbon foil is improved, the carbon foil product has excellent thermal oxidation resistance, and the adaptability to heating and patch reflow soldering temperatures in the solid aluminum electrolysis production process is wider.
Drawings
FIG. 1 is a sectional SEM structural diagram of a carbon foil obtained in example 1 of the present invention.
FIG. 2 is a graph showing the oxidation resistance of the carbon foil prepared in example 1 of the present invention.
Detailed Description
The following further describes embodiments of the present invention with reference to the drawings.
The invention relates to the following components: carbon nanotubes were purchased from Tianjin Chirshatai chemical Co., Ltd; polyester acrylic resins are available from san chemical materials, inc, yozhou; the aqueous polyurethane resin is purchased from Guangdong Yuebeautification chemical company, Inc.; epoxy acrylic resin is available from Bai Qian chemical Co., Ltd in Shandong; triallyl isocyanurate is available from new materials, Inc. of riedit, Beijing Ke; diethylene glycol butyl ether was purchased from chemical technology ltd, cautious, Shanghai; polyoxyethylene alkylphenyl ethers are available from southbound Ricker chemical Limited; polyurethane resins are available from fast commercial ltd, generation, guangzhou; methylbenzyl alcohol was purchased from chemical reagents ltd, wungjiang, guangdong; n, N-Dimethylacetamide was purchased from Lv Sen chemical Co., Lin Yi, Inc.; terpineol was purchased from co-industrial chemicals, ltd, thaizhou; the aluminate coupling agent is purchased from Yongtai chemical industry business in Linyi Shang City; the triethanolamine borate is purchased from Shenzhen Taida chemical Co., Ltd; antioxidant 1010 was purchased from north Heibbon chemical technology, Inc.; polyvinylpyrrolidone is available from Guangdong Yue beautification industries, Inc., and defoamer 3168 is available from good and many new materials, Inc. in Dongguan; an ultrasonic oscillator is arranged at the bottom of the side of the stirring kettle, and the ultrasonic oscillator is 600-1200W and is synchronously opened and closed with a stirrer of the stirring kettle. The synchronous oscillation can accelerate and refine the stirring effect and improve the uniformity of the slurry, the volume ratio of the concentrated nitric acid to the concentrated sulfuric acid in the mixed solution of the concentrated nitric acid and the concentrated sulfuric acid is 1:1, and the slurry is immersed;
example 1
A high-compactness, acid-resistant and oxidation-resistant solid capacitance carbon foil production process comprises the following process steps:
(1) preparing slurry:
① soaking and acidifying carbon nanotube in mixed solution of concentrated nitric acid and concentrated sulfuric acid for 1.5h, washing with deionized water to neutral, oven drying to obtain acidified carbon nanotube, mixing with carbon nanotube at a mass ratio of 2:1 to obtain nanometer conductive carbon fiber system;
② the high molecular solvent is composed of diethylene glycol monobutyl ether, polyoxyethylene alkyl phenyl ether, methyl benzyl alcohol, N-dimethyl acetamide and terpineol which are added into a stirring kettle in sequence according to the mass ratio of 3:1: 3: 2: 1;
the adhesive is polyester acrylic resin, waterborne polyurethane resin, epoxy acrylic resin and polyurethane resin in a mass ratio of 2: 3:1:1, stirring and mixing for 30min at the stirring speed of 105r/min and the temperature of 42 ℃;
adding an adhesive which accounts for half of the volume of the total adhesive into a high molecular solvent, stirring and mixing for 0.8h at the stirring speed of 55r/min, and then adding a nano conductive carbon fiber system, wherein the mass ratio of the nano conductive carbon fiber system to the high molecular solvent is 2.6: 70, mixing for 1.3h at the stirring speed of 65 r/min;
③ adding the other half of the adhesive into the stirring kettle of step ②, and mixing for 26min at the stirring speed of 40r/min, wherein the mass ratio of the total adhesive to the polymer solvent is 17: 70;
④, sequentially adding processing aids into the stirring kettle in the step ③, wherein the mass ratio of the processing aids to the high molecular solvent is 0.8:70, the processing aids are triallyl isocyanurate, triethanolamine borate, aluminate coupling agent, antioxidant 1010, polyvinylpyrrolidone and defoamer 3168 in the mass ratio of 4:5:3:1:2:3, and the processing aids are added and stirred and mixed for 1.4 hours at the stirring speed of 62r/min to obtain slurry;
(2) coating, namely placing the etched aluminum foil on a gravure coater, and coating the slurry prepared in the step (1) on two sides to obtain a foil tape, wherein the coating thickness is 28 micrometers;
(3) interface treatment: feeding the foil strip into a high-temperature furnace, wherein the heating rate of the high-temperature furnace is 20 ℃/min, heating to 430 ℃, preserving heat for 2.5h, and then reducing the temperature to room temperature at the cooling rate of 10 ℃/min;
(4) rewinding and slitting: inspecting damage of the foil tape subjected to the step (3) by foil reversing, and removing the damage by using a cutting machine;
(5) and (3) inspecting and packaging: and inspecting the foil tape, packaging and warehousing to obtain the solid capacitance carbon foil, wherein the width of the solid capacitance carbon foil is 460 mm.
Example 2:
a high-compactness, acid-resistant and oxidation-resistant solid capacitance carbon foil production process comprises the following process steps:
(1) preparing slurry:
① soaking and acidifying carbon nanotube in mixed solution of concentrated nitric acid and concentrated sulfuric acid for 1.8h, washing with deionized water to neutral, oven drying to obtain acidified carbon nanotube, mixing with carbon nanotube at a mass ratio of 2:1 to obtain nanometer conductive carbon fiber system;
② the high molecular solvent is composed of polyoxyethylene alkyl phenyl ether, N-dimethyl acetamide and terpineol which are added into a stirring kettle in sequence according to the mass ratio of 1:2: 1;
the adhesive is prepared by mixing waterborne polyurethane resin, epoxy acrylic resin and polyurethane resin according to the mass ratio of 3:1:1 for 30min at the stirring speed of 114r/min and the temperature of 45 ℃;
adding an adhesive which accounts for half of the volume of the total adhesive into a high molecular solvent, stirring and mixing for 0.8h at the stirring speed of 55r/min, and then adding a nano conductive carbon fiber system, wherein the mass ratio of the nano conductive carbon fiber system to the high molecular solvent is 4.5: 70, mixing for 1.8 hours at the stirring speed of 68 r/min;
③ adding the other half of the adhesive into the stirring kettle of step ②, mixing for 28min at the stirring speed of 42r/min, wherein the mass ratio of the total adhesive to the polymer solvent is 18: 70;
④, sequentially adding a processing aid into the stirring kettle in the step ③, wherein the mass ratio of the processing aid to the high molecular solvent is 1.1:70, the processing aid is triallyl isocyanurate, triethanolamine borate, an aluminate coupling agent, an antioxidant 1010, polyvinylpyrrolidone and a defoaming agent 3168, and the processing aid is added and stirred for 1.8 hours at a stirring speed of 67r/min to obtain slurry;
(2) coating, namely placing the etched aluminum foil on a gravure coater, and coating the slurry prepared in the step (1) on two sides to obtain a foil tape, wherein the coating thickness is 39 micrometers;
(3) interface treatment: feeding the foil strip into a high-temperature furnace, wherein the heating rate of the high-temperature furnace is 20 ℃/min, heating to 445 ℃, preserving heat for 2.8h, and then reducing the temperature to room temperature at the cooling rate of 10 ℃/min;
(4) rewinding and slitting: inspecting damage of the foil tape subjected to the step (3) by foil reversing, and removing the damage by using a cutting machine;
(5) and (3) inspecting and packaging: and inspecting the foil tape, packaging and warehousing to obtain the solid capacitance carbon foil, wherein the width of the solid capacitance carbon foil is 500 mm.
Example 3:
a high-compactness, acid-resistant and oxidation-resistant solid capacitance carbon foil production process comprises the following process steps:
(1) preparing slurry:
① soaking and acidifying carbon nanotube in mixed solution of concentrated nitric acid and concentrated sulfuric acid for 1.1h, washing with deionized water to neutral, oven drying to obtain acidified carbon nanotube, mixing with carbon nanotube at a mass ratio of 2:1 to obtain nanometer conductive carbon fiber system;
② the high molecular solvent is composed of diethylene glycol butyl ether, polyoxyethylene alkyl phenyl ether and N, N-dimethyl acetamide which are added into a stirring kettle in sequence according to the mass ratio of 3:1: 2;
the adhesive is polyester acrylic resin and epoxy acrylic resin in a mass ratio of 2:1, stirring and mixing for 30min at the stirring speed of 86r/min and the temperature of 42 ℃;
adding an adhesive which accounts for half of the volume of the total adhesive into a high molecular solvent, stirring and mixing for 0.5h at a stirring speed of 47r/min, and then adding a nano conductive carbon fiber system, wherein the mass ratio of the nano conductive carbon fiber system to the high molecular solvent is 2.2: 70, mixing for 1h at the stirring speed of 61 r/min;
③ adding the other half of the adhesive into the stirring kettle of step ②, mixing for 21min at the stirring speed of 32r/min, wherein the mass ratio of the total adhesive to the polymer solvent is 15: 70;
④, sequentially adding processing aids into the stirring kettle in the step ③, wherein the mass ratio of the processing aids to the high molecular solvent is 0.6:70, the processing aids are triallyl isocyanurate, triethanolamine borate, aluminate coupling agent, antioxidant 1010, polyvinylpyrrolidone and defoamer 3168 in the mass ratio of 4:5:3:1:2:3, and the processing aids are added and stirred and mixed for 1.1h at the stirring speed of 62r/min to obtain slurry;
(2) coating, namely placing the etched aluminum foil on a gravure coater, and coating the slurry prepared in the step (1) on two sides to obtain a foil tape with the coating thickness of 23 mu m;
(3) interface treatment: feeding the foil strip into a high-temperature furnace, wherein the heating rate of the high-temperature furnace is 20 ℃/min, heating to 410 ℃, preserving heat for 2.2h, and then reducing the temperature to room temperature at the cooling rate of 10 ℃/min;
(4) rewinding and slitting: inspecting damage of the foil tape subjected to the step (3) by foil reversing, and removing the damage by using a cutting machine;
(5) and (3) inspecting and packaging: and inspecting the foil tape, packaging and warehousing to obtain the solid capacitance carbon foil, wherein the width of the solid capacitance carbon foil is 460 mm.
The mechanism of the invention is as follows:
the carbon nano tube and the acidified carbon nano tube are used as a nano conductive carbon fiber system, the interface is grafted with carboxyl and hydroxyl active groups through acidification, the nano conductive carbon fiber system has excellent stable shape, large comparative area and more surface atomic numbers, a small amount of chemical bonds can be combined with a molecular chain of a macromolecular carrier to form stronger acting force, the decomposition reaction of removing monomers can be inhibited, the stability is improved, the particle spacing is further reduced, and thus conductive channels in different directions are established to form a conductive network;
the preparation method comprises the steps of adopting a polymer carrier consisting of an adhesive, a polymer solvent and a processing aid, dispersing a nano conductive carbon fiber system in the polymer solvent in an ultrasonic-assisted manner, and using the solvent formed by combining several of diethylene glycol butyl ether, polyoxyethylene alkyl phenyl ether, methyl benzyl alcohol, N-dimethylacetamide and terpineol to adjust the viscosity of conductive slurry, wherein the solvent has surface tension suitable for covering a carbon foil, is convenient to dissolve with the adhesive of a resin system and plays a role in dispersion and dilution, the adhesive is used for improving the interface performance of the nano conductive carbon fiber system and the polymer solvent, the agglomeration phenomenon is avoided, and the dispersibility and the bonding performance of the nano conductive carbon fiber system and the processing aid are improved;
the processing aid consists of triallyl isocyanurate, triethanolamine borate, an aluminate coupling agent, an antioxidant 1010, polyvinylpyrrolidone and a defoaming agent 3168 which respectively play roles in toughening, cracking resistance, lubricating, dispersing, film forming, antioxidation, tackifying and defoaming so as to improve the dispersing performance, anti-settling performance and surface quality of the conductive paste, and is suitable for uniformly and compactly covering the surface of a corroded aluminum foil, protecting a current collector, preventing the surface of the aluminum foil from being oxidized or corroded, and greatly reducing the ESR of the solid capacitor.
The carbon foil obtained in example 1 was kept at 400 to 650 ℃ for 30min in an air atmosphere with a commercially available comparative example, and the oxidation resistance was measured, and referring to fig. 2, the comparative example was peeled off, while the present invention maintained excellent thermal oxidation resistance.
The carbon foils obtained in examples 1 to 3 were used for capacitors and commercially available carbon foils as comparative examples, and life data was measured as follows:
the coating method is used for replacing the traditional physical sputtering or chemical vapor deposition method, so that the carbon-containing slurry spreading carbon layer can be completely and uniformly loaded on the surface of the corroded aluminum foil substrate, the slurry and the aluminum substrate are mutually bonded by high-temperature interface treatment, the load is effectively transferred, the interface reaction degree can be effectively controlled, the adverse interface reactant is inhibited, the debonding phenomenon under the action of lower stress is avoided, the bonding is reliable, the shedding is not easy, the process difficulty is greatly reduced, the carbon foil compactness is improved, the carbon foil product has excellent thermal oxidation resistance, and the adaptability to heating and patch reflow soldering temperatures in the solid aluminum electrolysis production process is wider.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are also included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (8)
1. A production process of a high-compactness, acid-resistant and oxidation-resistant solid capacitance carbon foil is characterized by comprising the following process steps:
(1) preparing slurry:
① soaking and acidifying carbon nanotubes in a mixed solution of concentrated nitric acid and concentrated sulfuric acid for 1-2 h, washing with deionized water to neutrality, drying to obtain acidified carbon nanotubes, and mixing with carbon nanotubes to obtain a nano conductive carbon fiber system;
② adding an adhesive which accounts for half of the volume of the total adhesive into a high molecular solvent, stirring and mixing, adding a nano conductive carbon fiber system, wherein the mass ratio of the nano conductive carbon fiber system to the high molecular solvent is (2-5): 70, and stirring and mixing;
③ adding the other half of the adhesive into the stirring kettle of step ②, stirring and mixing, wherein the mass ratio of the total adhesive to the polymer solvent is (15-20): 70;
④, sequentially adding processing aids into the stirred tank in the step ③, wherein the mass ratio of the processing aids to the polymer solvent is (0.4-1.2): 70, and stirring and mixing to obtain slurry;
(2) coating, namely placing the etched aluminum foil on a gravure coater, and coating the slurry prepared in the step (1) on two sides to obtain a foil tape, wherein the coating thickness is 20-42 mu m;
(3) interface treatment: feeding the foil strips into a high-temperature furnace, heating to 400-450 ℃, preserving heat for 2-3 h, and cooling to room temperature;
(4) rewinding and slitting: inspecting damage of the foil tape subjected to the step (3) by foil reversing, and removing the damage by using a cutting machine;
(5) and (3) inspecting and packaging: and inspecting the foil tape, packaging and warehousing to obtain the solid capacitance carbon foil.
2. The process of claim 1, wherein the ratio of the acidified carbon nanotubes to the carbon nanotubes in step (1) ① is 2: 1.
3. The process for producing a high-compactness, acid-resistant and oxidation-resistant solid-state capacitor carbon foil as claimed in claim 1, wherein the polymer solvent is obtained by sequentially adding several of diethylene glycol butyl ether, polyoxyethylene alkylphenyl ether, methyl benzyl alcohol, N-dimethylacetamide and terpineol into a stirring kettle, and stirring and mixing at a stirring speed of 85-115 r/min and a temperature of 40-45 ℃ for 30 min.
4. The process for producing a high-density, acid-resistant, oxidation-resistant solid-state capacitor carbon foil as claimed in claim 3, wherein the binder is one or more of polyester acrylic resin, aqueous polyurethane resin, epoxy acrylic resin and polyurethane resin.
5. The process for producing a high-density, acid-resistant and oxidation-resistant solid-state capacitor carbon foil according to claim 4, wherein the step (1) ② comprises mixing the mixture at a mixing speed of 46-58 r/min for 0.5-1 h when the binder is added, mixing the mixture at a mixing speed of 60-75 r/min for 1-2 h when the nano-conductive carbon fiber system is added, and mixing the mixture at a mixing speed of 30-45 r/min for 20-30 min when the binder is added in the step (1) ③.
6. The process for producing a high-compactness, acid-resistant and oxidation-resistant solid-state capacitor carbon foil as claimed in claim 4, wherein the processing aid is triallyl isocyanurate, triethanolamine borate, an aluminate coupling agent, an antioxidant 1010, polyvinylpyrrolidone and a defoaming agent 3168 in a mass ratio of 4:5:3:1:2:3, and the processing aid is added and stirred and mixed for 1-2 hours at a stirring speed of 60-70 r/min.
7. The process for producing a high-density, acid-resistant, oxidation-resistant solid-state capacitor carbon foil as claimed in claim 1, wherein the temperature raising rate of the high-temperature furnace in the step (3) is 20 ℃/min and the temperature lowering rate is 10 ℃/min.
8. The process for producing a high-density, acid-resistant and oxidation-resistant solid-state capacitor carbon foil as claimed in any one of claims 1 to 7, wherein the width of the solid-state capacitor carbon foil is 460mm or 500 mm.
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