CN111816447A - Preparation method of conductive polymer film in solid aluminum electrolytic capacitor - Google Patents
Preparation method of conductive polymer film in solid aluminum electrolytic capacitor Download PDFInfo
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- CN111816447A CN111816447A CN202010789634.5A CN202010789634A CN111816447A CN 111816447 A CN111816447 A CN 111816447A CN 202010789634 A CN202010789634 A CN 202010789634A CN 111816447 A CN111816447 A CN 111816447A
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- aluminum foil
- conductive polymer
- polymer film
- electrolytic capacitor
- aluminum electrolytic
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 120
- 229920001940 conductive polymer Polymers 0.000 title claims abstract description 42
- 239000003990 capacitor Substances 0.000 title claims abstract description 32
- 239000007787 solid Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000011888 foil Substances 0.000 claims abstract description 91
- 239000007800 oxidant agent Substances 0.000 claims abstract description 49
- 238000001035 drying Methods 0.000 claims abstract description 45
- 230000001590 oxidative effect Effects 0.000 claims abstract description 42
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 14
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 11
- 238000004140 cleaning Methods 0.000 claims abstract description 11
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims abstract description 9
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims abstract description 9
- 238000005470 impregnation Methods 0.000 claims abstract description 8
- 238000002791 soaking Methods 0.000 claims abstract description 6
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 4
- 239000000178 monomer Substances 0.000 claims description 16
- 229920000642 polymer Polymers 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 12
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 claims description 12
- GKWLILHTTGWKLQ-UHFFFAOYSA-N 2,3-dihydrothieno[3,4-b][1,4]dioxine Chemical compound O1CCOC2=CSC=C21 GKWLILHTTGWKLQ-UHFFFAOYSA-N 0.000 claims description 8
- OXHNLMTVIGZXSG-UHFFFAOYSA-N 1-Methylpyrrole Chemical compound CN1C=CC=C1 OXHNLMTVIGZXSG-UHFFFAOYSA-N 0.000 claims description 7
- 239000002019 doping agent Substances 0.000 claims description 7
- RIUYABVRXQBKJW-UHFFFAOYSA-N 1-(1h-pyrrol-3-yl)octan-1-one Chemical compound CCCCCCCC(=O)C=1C=CNC=1 RIUYABVRXQBKJW-UHFFFAOYSA-N 0.000 claims description 6
- VPUAYOJTHRDUTK-UHFFFAOYSA-N 1-ethylpyrrole Chemical compound CCN1C=CC=C1 VPUAYOJTHRDUTK-UHFFFAOYSA-N 0.000 claims description 6
- RFSKGCVUDQRZSD-UHFFFAOYSA-N 3-methoxythiophene Chemical compound COC=1C=CSC=1 RFSKGCVUDQRZSD-UHFFFAOYSA-N 0.000 claims description 6
- NJAURUMTVMVSGR-UHFFFAOYSA-N 3-pentoxythiophene Chemical compound CCCCCOC=1C=CSC=1 NJAURUMTVMVSGR-UHFFFAOYSA-N 0.000 claims description 6
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000012752 auxiliary agent Substances 0.000 claims description 6
- 239000004094 surface-active agent Substances 0.000 claims description 6
- 229930192474 thiophene Natural products 0.000 claims description 6
- WRDWWAVNELMWAM-UHFFFAOYSA-N 4-tert-butylaniline Chemical compound CC(C)(C)C1=CC=C(N)C=C1 WRDWWAVNELMWAM-UHFFFAOYSA-N 0.000 claims description 3
- 150000004996 alkyl benzenes Chemical class 0.000 claims description 3
- -1 alkyl naphthalene sulfonate Chemical compound 0.000 claims description 3
- 150000008052 alkyl sulfonates Chemical class 0.000 claims description 3
- 239000002280 amphoteric surfactant Substances 0.000 claims description 3
- 239000003945 anionic surfactant Substances 0.000 claims description 3
- 229940077388 benzenesulfonate Drugs 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- VSHTWPWTCXQLQN-UHFFFAOYSA-N n-butylaniline Chemical compound CCCCNC1=CC=CC=C1 VSHTWPWTCXQLQN-UHFFFAOYSA-N 0.000 claims description 3
- 239000002736 nonionic surfactant Substances 0.000 claims description 3
- VMPITZXILSNTON-UHFFFAOYSA-N o-anisidine Chemical compound COC1=CC=CC=C1N VMPITZXILSNTON-UHFFFAOYSA-N 0.000 claims description 3
- 230000007797 corrosion Effects 0.000 abstract description 9
- 238000005260 corrosion Methods 0.000 abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 9
- 239000002904 solvent Substances 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 241000519995 Stachys sylvatica Species 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 2
- 150000002170 ethers Chemical class 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000002794 monomerizing effect Effects 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- H01G9/022—Electrolytes; Absorbents
- H01G9/025—Solid electrolytes
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Abstract
The invention provides a preparation method of a conductive polymer film in a solid-state aluminum electrolytic capacitor, which comprises the following steps: step S1, providing a formed aluminum foil; step S2, soaking the formed aluminum foil into the reducing solution, taking out and drying; step S3, taking out and drying the formed aluminum foil treated in step S2 in the impregnation oxidizing solution; step S4, repeating the step S2 and the step S3 as a whole for a plurality of times, blanking and directly baking the formed aluminum foil for 30-40 min; step S5, cleaning the formed aluminum foil processed in the step S4 to finish the preparation of the conductive polymer film in the solid aluminum electrolytic capacitor; the oxidizing liquid comprises an oxidizing agent, wherein the oxidizing agent comprises at least one of ammonium persulfate, sodium persulfate and potassium permanganate; in step S4, the baking temperature is higher than the decomposition temperature of the oxidizing agent. The conductive polymer film obtained by the preparation method disclosed by the disclosure has good formability on the surface of the aluminum foil, and can solve the problem of corrosion of the residual oxidant to the aluminum foil.
Description
Technical Field
The disclosure relates to a preparation method of a conductive polymer film in a solid-state aluminum electrolytic capacitor.
Background
Capacitors are a basic type of electronic components and are widely used in various electronic products. The solid-state aluminum electrolytic capacitor is a novel electrolytic capacitor developed along with the continuous improvement of the requirements of electronic products on high-frequency characteristics in recent decades. The method has wide application in modern communication, computers, high-performance civil and military electronic products.
The solid-state aluminum electrolytic capacitor is a novel electrolytic capacitor developed along with the continuous improvement of the requirement of electronic products on high-frequency characteristics in recent decades. The method has wide application in modern communication, computers, high-performance civil and military electronic products. Compared with a liquid aluminum electrolytic capacitor, the solid aluminum electrolytic capacitor has more stable performance by using the conductive polymer to replace liquid electrolyte.
The above description is merely provided as background and is not an admission that the above "background" constitutes prior art to the present disclosure.
Disclosure of Invention
In some embodiments, the present disclosure provides a method of preparing a conductive polymer film in a solid aluminum electrolytic capacitor, comprising the steps of: step S1, providing a formed aluminum foil; step S2, soaking the formed aluminum foil into the reducing solution, taking out and drying; step S3, taking out and drying the formed aluminum foil treated in step S2 in the impregnation oxidizing solution; step S4, repeating the step S2 and the step S3 as a whole for a plurality of times, blanking and directly baking the formed aluminum foil for 30-40 min; step S5, cleaning the formed aluminum foil processed in the step S4 to finish the preparation of the conductive polymer film in the solid aluminum electrolytic capacitor; the oxidizing liquid comprises an oxidizing agent, wherein the oxidizing agent comprises at least one of ammonium persulfate, sodium persulfate and potassium permanganate; in step S4, the baking temperature is higher than the decomposition temperature of the oxidizing agent.
In some embodiments, the oxidizing agent is ammonium persulfate or sodium persulfate.
In some embodiments, the oxidizing liquid further comprises a dopant; the dopant includes at least one of an alkyl sulfonate, an alkyl naphthalene sulfonate, or an alkyl benzene sulfonate.
In some embodiments, the oxidizing solution further comprises an auxiliary agent; the auxiliary agent comprises at least one of an anionic surfactant, a nonionic surfactant, an amphoteric surfactant and a compound surfactant.
In some embodiments, the reducing liquid comprises a polymer monomer; the polymer monomer comprises at least one of pyrrole, N-methylpyrrole, N-ethylpyrrole, 3-octanoyl pyrrole, thiophene, 3, 4-ethylenedioxythiophene, 3-methoxythiophene, 3-pentoxythiophene, aniline, 4-tert-butyl aniline, N-butyl aniline or o-methoxyaniline.
In some embodiments, the polymeric monomer is selected from at least one of pyrrole, N-methylpyrrole, N-ethylpyrrole, 3-octanoylpyrrole, thiophene, 3, 4-ethylenedioxythiophene, 3-methoxythiophene, 3-pentyloxythiophene.
In some embodiments, in step S2, the drying temperature is 30-50 ℃ and the drying time is 0.5-5 min; in step S3, the drying temperature is 30-50 deg.C and the drying time is 0.5-5 min.
In some embodiments, in step S2, the time for immersing the formed aluminum foil into the reducing solution is 0.5-3 min; in step S3, the time for immersing the formed aluminum foil in the oxidizing solution is 0.5-3 min.
In some embodiments, in step S4, the baking temperature is 10-20 ℃ above the decomposition temperature of the oxidizing agent.
In some embodiments, in step S4, the decomposition rate of the residual oxidant in the conductive polymer film after baking is 80% to 90%.
Detailed Description
It is to be understood that the disclosed embodiments are merely exemplary of the disclosure that may be embodied in various forms, and that specific details disclosed herein are not to be interpreted as limiting, but merely as a basis for the claims and as a representative basis for teaching one skilled in the art to variously employ the disclosure.
In some embodiments, a method of making a conductive polymer film in a solid state aluminum electrolytic capacitor comprises the steps of:
step S1, providing a formed aluminum foil;
step S2, soaking the formed aluminum foil into the reducing solution, taking out and drying;
step S3, taking out and drying the formed aluminum foil treated in step S2 in the impregnation oxidizing solution;
step S4, repeating the step S2 and the step S3 as a whole for a plurality of times, blanking and directly baking the formed aluminum foil for 30-40 min;
step S5, cleaning the formed aluminum foil processed in the step S4 to finish the preparation of the conductive polymer film in the solid aluminum electrolytic capacitor;
wherein,
the oxidizing liquid comprises an oxidizing agent, and the oxidizing agent comprises at least one of ammonium persulfate, sodium persulfate and potassium permanganate;
in step S4, the baking temperature is higher than the decomposition temperature of the oxidizing agent.
The conductive polymer film in the solid aluminum electrolytic capacitor can be formed by oxidizing and polymerizing polymer monomers, specifically, a formed aluminum foil is respectively soaked in a reducing solution and an oxidizing solution, the polymer monomers in the reducing solution and an oxidizing agent in the oxidizing solution are attached to the surface of the formed aluminum foil, and in the drying process, the polymer monomers and the oxidizing agent rapidly react to form the conductive polymer film on the surface of the formed aluminum foil. However, the inventors found that an oxidizing agent which does not participate in the reaction inevitably remains on the surface of the formed aluminum foil after the multiple oxidation polymerization, and the remaining oxidizing agent corrodes the surface of the formed aluminum foil, and particularly, when the solvent of the reducing solution and the oxidizing solution is water, the solvent water remaining on the surface of the formed aluminum foil further promotes the hydrolysis and ionization of the oxidizing agent, and the corrosion of the aluminum foil is promoted, so that the bad phenomena such as corrosion marks and white spots occur on the surface of the aluminum foil, and the capacity extraction rate of the aluminum foil is low, and the leakage current is large.
In order to remove the residual oxidizing agent on the surface of the formed aluminum foil, a possible operation is to wash the surface of the formed aluminum foil directly after the blanking with clean (or warm) water. However, the inventors have found that the oxidizing agent is easily hydrolyzed and ionized in water, and the washing operation using clean (or warm) water provides conditions for the hydrolytic ionization of the oxidizing agent, thereby resulting in failure to fundamentally solve the corrosion of the aluminum foil by the residual oxidizing agent.
The formed aluminum foil is directly baked at high temperature for 30-40min after blanking, the high-temperature baking can quickly decompose the oxidant remained on the surface of the formed aluminum foil (namely, remained in the conductive polymer film), the high-temperature baking can ensure that the residual oxidant is fully decomposed after 30-40min, so that the residual oxidant loses strong oxidizing property, and the high-temperature baking can accelerate the volatilization of residual solvent (such as water) after 30-40min, so that the corrosion of the residual oxidant to the aluminum foil can be fundamentally solved. And (3) after high-temperature baking, cleaning to remove oxidant decomposition products and residual oxidant which is not decomposed, thus finishing the preparation of the conductive polymer film in the solid-state aluminum electrolytic capacitor.
In some embodiments, the oxidizing agent is ammonium persulfate or sodium persulfate. The persulfate oxidizer has moderate oxidizability and is more suitable for preparing the conductive polymer film in the actual production process; if the oxidizing agent used is too oxidative, the formation rate of the conductive polymer may be too fast, thereby affecting the uniformity of the conductive polymer film. In some embodiments, the oxidizing agent is ammonium persulfate.
In some embodiments, the oxidizing liquid further comprises a dopant; the dopant includes at least one of an alkyl sulfonate, an alkyl naphthalene sulfonate, or an alkyl benzene sulfonate. The dopant can increase the conductivity of the conductive polymer film.
In some embodiments, the oxidizing solution further comprises an auxiliary agent; the auxiliary agent comprises at least one of an anionic surfactant, a nonionic surfactant, an amphoteric surfactant and a compound surfactant.
In step S3, the solvent used in the oxidizing solution may be a solvent capable of dissolving the oxidizing agent, including, but not limited to, alcohols, ketones, ethers, water, and mixed solvents thereof.
In some embodiments, the reducing liquid comprises a polymer monomer; the polymer monomer comprises at least one of pyrrole, N-methylpyrrole, N-ethylpyrrole, 3-octanoyl pyrrole, thiophene, 3, 4-ethylenedioxythiophene, 3-methoxythiophene, 3-pentoxythiophene, aniline, 4-tert-butyl aniline, N-butyl aniline or o-methoxyaniline.
In some embodiments, the polymeric monomer is selected from at least one of pyrrole, N-methylpyrrole, N-ethylpyrrole, 3-octanoylpyrrole, thiophene, 3, 4-ethylenedioxythiophene, 3-methoxythiophene, 3-pentyloxythiophene.
In step S2, the solvent used in the reducing solution may be a solvent capable of dissolving the polymer monomer, including, but not limited to, alcohols, ketones, ethers, water, and mixed solvents thereof.
Although the drying process is performed after each single impregnation of the reducing solution or the oxidizing solution, firstly, the drying process should not be too long based on the actual production operation, otherwise, the single drying time is continuously accumulated after the steps S2 and S3 are repeated for many times, thereby seriously affecting the production efficiency of the product, secondly, the drying process should not be too high based on the actual production operation, because the main purpose of the drying process is to accelerate the reaction between the polymer monomer and the oxidizing agent, thereby improving the on-line production efficiency, if the drying temperature is too high, the reaction speed between the polymer monomer and the oxidizing agent is too fast, thereby causing the formed conductive polymer film to be unevenly distributed on the surface of the formed aluminum foil, and particularly, if the drying temperature is too high, the formed aluminum foil is not too slow to cool, thereby causing the polymer monomer/oxidizing agent to react too fast on the surface of the formed aluminum foil in the next cycle of impregnation process, further aggravating the non-uniformity of the conductive polymer film on the surface of the formed aluminum foil. In some embodiments, in step S2, the drying temperature is 30-50 ℃ and the drying time is 0.5-5 min; in step S3, the drying temperature is 30-50 deg.C and the drying time is 0.5-5 min. In some embodiments, in step S2, the drying time is 0.5-1 min; in step S3, the drying time is 0.5-1 min.
In some embodiments, in step S2, the time for immersing the formed aluminum foil into the reducing solution is 0.5-3 min; in step S3, the time for immersing the formed aluminum foil in the oxidizing solution is 0.5-1 min. In some embodiments, in step S2, the time for immersing the formed aluminum foil into the reducing solution is 0.5-1 min; in step S3, the time for immersing the formed aluminum foil in the oxidizing solution is 0.5-1 min.
In some embodiments, in step S4, the baking temperature is 10-20 ℃ above the decomposition temperature of the oxidizing agent. When the baking temperature is within the above range, the oxidizing agent remaining on the surface of the formed aluminum foil can be rapidly decomposed and the solvent can be rapidly volatilized, and unnecessary energy loss and damage to the formed polymer film due to an excessively high baking temperature can be avoided. In some embodiments, in step S4, the baking temperature is 80-150 ℃.
In some embodiments, after the steps of taking out and drying the formed aluminum foil impregnation reducing solution in step S2 and taking out and drying the formed aluminum foil impregnation oxidizing solution in step S3, the steps of cleaning and drying the formed aluminum foil are further included. The cleaning and drying step can remove the oxidant which does not participate in the reaction on the line, help to reduce the corrosion of the oxidant to the aluminum foil, and improve the distribution uniformity of the formed conductive polymer film on the surface of the formed aluminum foil. In some embodiments, in the step of cleaning and drying the formed aluminum foil, the cleaning time is 0.5-1min, and the drying time is 0.5-1 min.
In some embodiments, in step S4, step S2 and step S3 are repeated 3-15 times as a whole.
In some embodiments, in step S4, the decomposition rate of the residual oxidant in the conductive polymer film after baking is 80% to 90%. The decomposition rate indicates the amount of the oxidizer decomposed by the high-temperature baking as a percentage of the total amount of the oxidizer remaining in the conductive polymer film.
In some embodiments, the cleaning includes at least one of soaking and spraying in step S5. In some embodiments, in step S5, the cleaning time is 10-20 min.
The disclosure is further illustrated with reference to the following examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present disclosure.
In the following examples and comparative examples, reagents, materials and instruments used were commercially available or synthetically available, unless otherwise specified.
Example 1
Providing a formed aluminum foil and placing the formed aluminum foil on a production line, immersing the formed aluminum foil into a reducing liquid tank containing 3, 4-ethylenedioxythiophene for 30s, taking out the formed aluminum foil and drying the formed aluminum foil at 40 ℃ for 30s, then immersing the formed aluminum foil into an oxidizing liquid tank containing ammonium persulfate, sodium dodecyl benzene sulfonate and a surfactant for 30s, taking out the formed aluminum foil and drying the formed aluminum foil at 40 ℃ for 30s, and alternately repeating the operation for 14 times; and after the last time of immersing in an oxidation liquid tank and drying, grabbing and forming the aluminum foil by a mechanical arm, directly baking the aluminum foil at 130 ℃ for 40min after blanking, and then soaking in clean water and spraying for 15min to finish the preparation of the conductive polymer film in the solid-state aluminum electrolytic capacitor. Wherein the decomposition rate of the residual ammonium persulfate in the baked conductive polymer film is 87%.
The surface appearance of the aluminum foil obtained in example 1 was observed with a scanning electron microscope, and the defect rate of occurrence of phenomena such as corrosion marks and white spots was less than 0.5%.
Example 2
Providing a formed aluminum foil, placing the formed aluminum foil on a production line, immersing the formed aluminum foil into a reduction liquid tank containing N-methyl pyrrole for 1min, taking out the formed aluminum foil, drying the formed aluminum foil for 30s at 40 ℃, immersing the formed aluminum foil into an oxidation liquid tank containing sodium persulfate, sodium dodecyl benzene sulfonate and a surfactant for 1min, taking out the formed aluminum foil, drying the formed aluminum foil for 30s at 40 ℃, and alternately repeating the operation for 14 times; and after the final immersion in an oxidation liquid tank and drying, the aluminum foil is formed by grabbing by a mechanical arm, the aluminum foil is directly baked for 30min at 80 ℃ after blanking, and then the aluminum foil is immersed in clean water and sprayed for 15min, so that the preparation of the conductive polymer film in the solid-state aluminum electrolytic capacitor is completed. Wherein the decomposition rate of the residual sodium persulfate in the conductive polymer film after baking was 82%.
The surface appearance of the aluminum foil obtained in example 2 was observed with a scanning electron microscope, and the defect rate of occurrence of corrosion marks, white spots, and the like was less than 0.5%.
Comparative example 1
Providing a formed aluminum foil and placing the formed aluminum foil on a production line, immersing the formed aluminum foil into a reducing liquid tank containing 3, 4-ethylenedioxythiophene for 30s, taking out the formed aluminum foil and drying the formed aluminum foil at 40 ℃ for 30s, then immersing the formed aluminum foil into an oxidizing liquid tank containing ammonium persulfate, sodium dodecyl benzene sulfonate and a surfactant for 30s, taking out the formed aluminum foil and drying the formed aluminum foil at 40 ℃ for 30s, and alternately repeating the operation for 14 times; and after the final immersion in an oxidation liquid tank and drying, the mechanical arm picks and transforms the aluminum foil into aluminum foil, the aluminum foil is directly soaked in clean water for 30min after blanking, and then is sprayed with the clean water for 15min, so that the preparation of the conductive polymer film in the solid-state aluminum electrolytic capacitor is completed.
The surface appearance of the aluminum foil obtained in comparative example 1 was observed with a scanning electron microscope, and the defect rate of occurrence of corrosion marks, white spots, and the like was 4.5% to 5.5%.
The above detailed description describes exemplary embodiments, but is not intended to limit the combinations explicitly disclosed herein. Thus, unless otherwise specified, various features disclosed herein can be combined together to form a number of additional combinations that are not shown for the sake of brevity.
Claims (10)
1. A preparation method of a conductive polymer film in a solid aluminum electrolytic capacitor comprises the following steps:
step S1, providing a formed aluminum foil;
step S2, soaking the formed aluminum foil into the reducing solution, taking out and drying;
step S3, taking out and drying the formed aluminum foil treated in step S2 in the impregnation oxidizing solution;
step S4, repeating the step S2 and the step S3 as a whole for a plurality of times, blanking and directly baking the formed aluminum foil for 30-40 min;
step S5, cleaning the formed aluminum foil processed in the step S4 to finish the preparation of the conductive polymer film in the solid aluminum electrolytic capacitor;
wherein,
the oxidizing liquid comprises an oxidizing agent, and the oxidizing agent comprises at least one of ammonium persulfate, sodium persulfate and potassium permanganate;
in step S4, the baking temperature is higher than the decomposition temperature of the oxidizing agent.
2. The method for preparing a conductive polymer film in a solid aluminum electrolytic capacitor according to claim 1,
the oxidant is ammonium persulfate or sodium persulfate.
3. The method for preparing a conductive polymer film in a solid aluminum electrolytic capacitor according to claim 1,
the oxidizing liquid further comprises a dopant;
the dopant includes at least one of an alkyl sulfonate, an alkyl naphthalene sulfonate, or an alkyl benzene sulfonate.
4. The method for preparing a conductive polymer film in a solid aluminum electrolytic capacitor according to claim 1,
the oxidizing solution also comprises an auxiliary agent;
the auxiliary agent comprises at least one of an anionic surfactant, a nonionic surfactant, an amphoteric surfactant and a compound surfactant.
5. The method for preparing a conductive polymer film in a solid aluminum electrolytic capacitor according to claim 1,
the reducing liquid comprises a polymer monomer;
the polymer monomer comprises at least one of pyrrole, N-methylpyrrole, N-ethylpyrrole, 3-octanoyl pyrrole, thiophene, 3, 4-ethylenedioxythiophene, 3-methoxythiophene, 3-pentoxythiophene, aniline, 4-tert-butyl aniline, N-butyl aniline or o-methoxyaniline.
6. The method for preparing a conductive polymer film in a solid aluminum electrolytic capacitor according to claim 1,
the polymer monomer is at least one selected from pyrrole, N-methylpyrrole, N-ethylpyrrole, 3-octanoyl pyrrole, thiophene, 3, 4-ethylenedioxythiophene, 3-methoxythiophene and 3-pentoxythiophene.
7. The method for preparing a conductive polymer film in a solid aluminum electrolytic capacitor according to claim 1,
in step S2, the drying temperature is 30-50 ℃ and the drying time is 0.5-5 min;
in step S3, the drying temperature is 30-50 deg.C and the drying time is 0.5-5 min.
8. The method for preparing a conductive polymer film in a solid aluminum electrolytic capacitor according to claim 1,
in step S2, the time for the formed aluminum foil to be impregnated with the reducing solution is 0.5-3 min;
in step S3, the time for immersing the formed aluminum foil in the oxidizing solution is 0.5-3 min.
9. The method for preparing a conductive polymer film in a solid aluminum electrolytic capacitor according to claim 1,
in step S4, the baking temperature is 10-20 ℃ higher than the decomposition temperature of the oxidant.
10. The method for preparing a conductive polymer film in a solid aluminum electrolytic capacitor according to claim 1,
in step S4, the decomposition rate of the residual oxidizing agent in the baked conductive polymer film is 80% to 90%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010789634.5A CN111816447A (en) | 2020-08-07 | 2020-08-07 | Preparation method of conductive polymer film in solid aluminum electrolytic capacitor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114694973A (en) * | 2022-05-05 | 2022-07-01 | 肇庆绿宝石电子科技股份有限公司 | Method for preparing conducting polymer by ultrasonic wave and solid capacitor |
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Application publication date: 20201023 |