CN113436889A - Cathode conductive film of solid aluminum electrolytic capacitor and preparation method and application thereof - Google Patents
Cathode conductive film of solid aluminum electrolytic capacitor and preparation method and application thereof Download PDFInfo
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 108
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 104
- 239000003990 capacitor Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000007787 solid Substances 0.000 title claims description 23
- 239000011888 foil Substances 0.000 claims abstract description 110
- 238000000034 method Methods 0.000 claims abstract description 76
- 229910052751 metal Inorganic materials 0.000 claims abstract description 16
- 239000002184 metal Substances 0.000 claims abstract description 16
- 238000000151 deposition Methods 0.000 claims abstract description 13
- 238000007740 vapor deposition Methods 0.000 claims abstract description 13
- 238000000605 extraction Methods 0.000 claims abstract description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 41
- 229910052709 silver Inorganic materials 0.000 claims description 38
- 239000004332 silver Substances 0.000 claims description 38
- 238000000231 atomic layer deposition Methods 0.000 claims description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- 229910052799 carbon Inorganic materials 0.000 claims description 18
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 16
- 238000005229 chemical vapour deposition Methods 0.000 claims description 14
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 13
- 239000002131 composite material Substances 0.000 claims description 12
- 239000010949 copper Substances 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 229910052697 platinum Inorganic materials 0.000 claims description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052737 gold Inorganic materials 0.000 claims description 4
- 239000010931 gold Substances 0.000 claims description 4
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- 239000000956 alloy Substances 0.000 claims description 2
- 239000007791 liquid phase Substances 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 7
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 18
- 239000010409 thin film Substances 0.000 description 15
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- 230000001502 supplementing effect Effects 0.000 description 14
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- 239000011261 inert gas Substances 0.000 description 12
- 239000010453 quartz Substances 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 11
- 238000004140 cleaning Methods 0.000 description 11
- 239000001257 hydrogen Substances 0.000 description 11
- 229910052739 hydrogen Inorganic materials 0.000 description 11
- 239000007789 gas Substances 0.000 description 9
- 238000001816 cooling Methods 0.000 description 8
- 229920001467 poly(styrenesulfonates) Polymers 0.000 description 8
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 8
- 230000008021 deposition Effects 0.000 description 7
- 238000011010 flushing procedure Methods 0.000 description 7
- 239000012159 carrier gas Substances 0.000 description 6
- 229910001873 dinitrogen Inorganic materials 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 239000012299 nitrogen atmosphere Substances 0.000 description 6
- GKWLILHTTGWKLQ-UHFFFAOYSA-N 2,3-dihydrothieno[3,4-b][1,4]dioxine Chemical compound O1CCOC2=CSC=C21 GKWLILHTTGWKLQ-UHFFFAOYSA-N 0.000 description 5
- 229920000128 polypyrrole Polymers 0.000 description 5
- SHWZFQPXYGHRKT-FDGPNNRMSA-N (z)-4-hydroxypent-3-en-2-one;nickel Chemical compound [Ni].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O SHWZFQPXYGHRKT-FDGPNNRMSA-N 0.000 description 4
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- 238000000643 oven drying Methods 0.000 description 4
- 230000000379 polymerizing effect Effects 0.000 description 4
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- 230000000052 comparative effect Effects 0.000 description 3
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- 238000007654 immersion Methods 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 229960002796 polystyrene sulfonate Drugs 0.000 description 3
- 239000011970 polystyrene sulfonate Substances 0.000 description 3
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- FYMCOOOLDFPFPN-UHFFFAOYSA-K iron(3+);4-methylbenzenesulfonate Chemical compound [Fe+3].CC1=CC=C(S([O-])(=O)=O)C=C1.CC1=CC=C(S([O-])(=O)=O)C=C1.CC1=CC=C(S([O-])(=O)=O)C=C1 FYMCOOOLDFPFPN-UHFFFAOYSA-K 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 229920000767 polyaniline Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- -1 (2, 2-dimethylpropionate) silver (I) triethylphosphine Chemical compound 0.000 description 1
- VEJOYRPGKZZTJW-FDGPNNRMSA-N (z)-4-hydroxypent-3-en-2-one;platinum Chemical compound [Pt].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O VEJOYRPGKZZTJW-FDGPNNRMSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- ZKXWKVVCCTZOLD-FDGPNNRMSA-N copper;(z)-4-hydroxypent-3-en-2-one Chemical compound [Cu].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O ZKXWKVVCCTZOLD-FDGPNNRMSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- WHRAZOIDGKIQEA-UHFFFAOYSA-L iron(2+);4-methylbenzenesulfonate Chemical compound [Fe+2].CC1=CC=C(S([O-])(=O)=O)C=C1.CC1=CC=C(S([O-])(=O)=O)C=C1 WHRAZOIDGKIQEA-UHFFFAOYSA-L 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- PSZYNBSKGUBXEH-UHFFFAOYSA-M naphthalene-1-sulfonate Chemical compound C1=CC=C2C(S(=O)(=O)[O-])=CC=CC2=C1 PSZYNBSKGUBXEH-UHFFFAOYSA-M 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- MBUJACWWYFPMDK-UHFFFAOYSA-N pentane-2,4-dione;platinum Chemical compound [Pt].CC(=O)CC(C)=O MBUJACWWYFPMDK-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- PCCVSPMFGIFTHU-UHFFFAOYSA-N tetracyanoquinodimethane Chemical compound N#CC(C#N)=C1C=CC(=C(C#N)C#N)C=C1 PCCVSPMFGIFTHU-UHFFFAOYSA-N 0.000 description 1
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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
-
- 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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Polyoxymethylene Polymers And Polymers With Carbon-To-Carbon Bonds (AREA)
Abstract
The invention discloses a cathode conductive film of a solid-state aluminum electrolytic capacitor and a preparation method and application thereof, belonging to the field of aluminum electrolytic capacitors. The method comprises the following steps: depositing a conductive metal film on the surface of the anode foil dielectric layer of the aluminum electrolytic capacitor by using a vapor deposition method; and leading out a cathode electrode of the deposited conductive layer, namely preparing the conductive film on the surface of the anode foil dielectric layer of the aluminum electrolytic capacitor. The gas phase chemical method used by the invention avoids the problem that solution molecules are difficult to enter micro holes on the surface of the anode aluminum foil in the liquid phase method, so that the conductive film has high step coverage rate in the micro-nano holes, and the capacity extraction rate of the capacitor is improved. The conductive film prepared by the gas phase chemical method has the advantages of compact structure, less impurities, good uniformity and the like.
Description
Technical Field
The invention belongs to the field of aluminum electrolytic capacitors, and particularly relates to a cathode conductive film of a solid aluminum electrolytic capacitor, and a preparation method and application thereof.
Background
The solid-state aluminum electrolytic capacitor is a common energy storage device, has the excellent characteristics of small volume, high capacity, low cost, high frequency, low impedance and the like, and has wide application prospect in many fields. The performance of the conductive cathode in the solid-state aluminum electrolytic capacitor is a key influencing factor for restricting the performance of a solid-state device, so that the development of the solid-state conductive cathode with excellent characteristics is the core of the research of the solid-state aluminum electrolytic capacitor. The method for preparing the conductive cathode of the solid aluminum electrolytic capacitor is mainly a liquid phase method. The solid cathode prepared by the liquid phase method has the advantages of simple operation, easy implementation of large-scale production and the like, but the influence of surface tension and molecular size cannot be avoided in the liquid phase method, and a solvent or a dispersant and the like cannot easily enter a micro-nano porous structure on the surface of the anode foil of the electrolytic capacitor; acidic substances, strong oxidants and the like in the solution can damage the dielectric layer on the surface of the anode foil of the aluminum electrolytic capacitor, so that the problems of low actual lead-out capacity, reduced voltage resistance, increased leakage current and the like of the solid aluminum electrolytic capacitor are caused, impurities from the solvent are easily remained in the conductive layer prepared by the solution method, the conductivity of the conductive film is reduced, and the equivalent series resistance and the loss of the solid capacitor are increased. However, the traditional conductive cathode thin film (manganese oxide, tetracyano-p-quinodimethane, conductive polymer and the like) prepared on the anode foil dielectric layer of the solid-state aluminum electrolytic capacitor by adopting a liquid phase method at present has not strong enough adhesive force with the dielectric layer, and the conductive film of the materials is not compact enough, so that the problems of shortened service life of the capacitor and the like caused by the erosion of moisture and the like in a working condition environment on the anode foil dielectric layer can not be effectively resisted.
Through research and study of literature, in the industry of solid-state aluminum electrolytic capacitors: in 2006, penjia et al used a chemical oxidation method to synthesize conductive polyaniline as a solid cathode. In 1996, Yasuo Kudoh et al deposited manganese oxide layers on the dielectric layer of the solid aluminum electrolytic capacitor in advance by two methods, and then prepared polypyrrole as a solid cathode by an electrochemical method. In 2007, kokui prepared an all-solid-state conductive polyaniline electrolytic capacitor using an immersion method. In comparison with the above literature reports, we have found that the conductivity of the conductive polymer material prepared by chemical polymerization or electro-polymerization is low, and the organic solvent used in both methods causes a large environmental load.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a cathode conductive film of a solid aluminum electrolytic capacitor, and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the invention discloses a preparation method of a cathode conductive film of a solid-state aluminum electrolytic capacitor, which comprises the following steps:
depositing a conductive metal film on the surface of the anode foil dielectric layer of the aluminum electrolytic capacitor by using a vapor deposition method;
and leading out a cathode electrode of the deposited conductive layer, namely preparing the conductive film on the surface of the anode foil dielectric layer of the aluminum electrolytic capacitor.
Preferably, the geometric area size of the anode foil of the aluminum electrolytic capacitor is adjustable.
Preferably, the vapor deposition method includes an atomic layer deposition method, a chemical vapor deposition method, and a plasma-enhanced atomic layer deposition method.
Preferably, the material of the conductive metal thin film is selected from alloy materials including aluminum, nickel, copper, zinc, silver, gold, and platinum and aluminum, nickel, copper, zinc, silver, gold, and platinum.
Preferably, the cathode electrode extraction of the deposited conductive layer is performed using conductive carbon paste, silver paste, aluminum foil or silver wire.
The invention also discloses the solid aluminum electrolytic capacitor cathode conductive film prepared by the preparation method.
The invention also discloses application of the cathode conductive film of the solid aluminum electrolytic capacitor as a cathode of the solid aluminum electrolytic capacitor.
The invention also discloses application of the cathode conductive film of the solid aluminum electrolytic capacitor in preparing a pre-deposited layer of the composite conductive cathode of the solid aluminum electrolytic capacitor.
And further, preparing a composite conductive layer on the surface of the prepared cathode conductive film of the solid-state aluminum electrolytic capacitor, and then using conductive carbon paste, silver paste, aluminum foil or silver wires as a cathode leading-out end of the composite conductive layer.
Compared with the prior art, the invention has the following beneficial effects:
1) the invention discloses a method for preparing a metal-based conductive cathode film on the surface of an anode foil dielectric layer of an aluminum electrolytic capacitor by adopting a vapor deposition method for the first time, and main reactants of the vapor deposition method are gaseous molecules and can easily and uniformly enter micro-nano-scale pores. Meanwhile, the product of the vapor deposition method has better adhesive force with the substrate, and the prepared conductive film has no residual impurities. And because of the ultrahigh conductivity and excellent temperature characteristic of metal, the conductive metal-based thin film prepared by the vapor deposition method has the advantages of high conductivity, good wide-temperature performance, high conformality on a complex porous surface, high step coverage rate and strong adhesion with a substrate, and the compactness of the metal-based conductive thin film can also play a role in better protecting a medium. And the vapor deposition method can realize accurate control on the thickness of the film and has high repeatability. Therefore, the vapor deposition method used by the invention avoids the problem that solution molecules are difficult to enter micro holes on the surface of the anode aluminum foil in the liquid phase method, so that the conductive film has high step coverage rate in the micro-nano holes, and the capacity extraction rate of the capacitor is improved.
2) The use of the vapor deposition method can effectively avoid the damage of acidic substances and strong oxidants in the solution to the aluminum foil dielectric layer during the preparation by the liquid phase method.
3) The conductive film prepared by the gas phase method has the advantages of compact structure, less impurities, good uniformity and the like.
4) The conductive film obtained by the gas phase method can be directly used as the cathode of the solid-state aluminum electrolytic capacitor and can also be used as a pre-deposition layer of the composite conductive cathode layer. When the conductive film prepared by the vapor deposition technology is used as a pre-deposition layer of the cathode of the solid-state aluminum electrolytic capacitor, the dielectric layer can be effectively prevented from being damaged when the composite conductive layer is subsequently prepared due to the advantages of compact structure, good uniformity, high coverage degree to the dielectric layer, strong adhesive force with the dielectric layer and the like.
5) Compared with other conductive materials, the metal conductive film prepared by the invention has ultrahigh conductivity, and can effectively improve the frequency performance of the solid-state aluminum electrolytic capacitor.
6) The metal conductive film prepared by the invention is compact, can effectively resist the erosion of moisture to the anode foil dielectric layer, and improves the service life of the device.
Drawings
FIG. 1 is a schematic structural diagram of a solid-state aluminum electrolytic capacitor;
FIG. 2 is a SEM image of a cross-section of a vapor deposited conductive metal film on an aluminum anode foil dielectric layer.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the accompanying drawings:
referring to fig. 1 and fig. 2, the principle of preparing a conductive film on the surface of an anode foil dielectric layer of an aluminum electrolytic capacitor according to the present invention is illustrated, in which a vapor chemical deposition method is used to deposit a conductive metal film on the surface of the anode foil dielectric layer of the aluminum electrolytic capacitor, and a cathode electrode is led out from the deposited conductive layer, i.e., the conductive film is prepared on the surface of the anode foil dielectric layer of the aluminum electrolytic capacitor.
Comparative example 1
(1) Preparation work: and cutting the anode foil with the anode leading-out end by using an aluminum foil cutting die, and supplementing the cut edge.
(2) The cathode conductive layer is prepared by a dipping method. The method specifically comprises the following steps: putting the anode foil obtained after the treatment in the step (1) into a prepared poly (3, 4-ethylenedioxythiophene)/polystyrene sulfonate solution (PEDOT/PSS), and vacuumizing and impregnating; taking out and drying.
(3) And (3) dripping a layer of conductive carbon paste on the surface of the anode foil obtained in the step (2), solidifying at room temperature, dripping silver paste, and placing silver wires as cathode leading-out terminals.
The conductivity of the cathode conductive layer prepared in this example was tested as follows: 102.5S/cm.
Comparative example 2
(1) Preparation work: and cutting the anode foil with the anode leading-out end by using an aluminum foil cutting die, and supplementing the cut edge.
(2) The cathode conductive layer is prepared by in-situ polymerization. The method specifically comprises the following steps: respectively immersing the anode foil obtained after the treatment in the step (1) into a 3, 4-ethylenedioxythiophene solution (EDOT) and an iron p-toluenesulfonate solution; taking out and drying.
(3) And (3) dripping a layer of conductive carbon paste on the surface of the anode foil obtained in the step (2), solidifying at room temperature, dripping silver paste, and placing silver wires as cathode leading-out terminals.
The conductivity of the cathode conductive layer prepared in this example was tested as follows: 9.27S/cm.
Example 1
(1) Preparation work: and cutting the anode foil with the anode leading-out end by using an aluminum foil cutting die, and supplementing the cut edge.
(2) Aluminum metal (Al) thin films are deposited by Atomic Layer Deposition (ALD) techniques. The method specifically comprises the following steps: placing the anode foil obtained after the treatment in the step (1) into an ALD reaction chamber, vacuumizing to 0.5Pa, and depositing at 250 ℃; introducing a precursor Trimethylaluminum (TMA) for 3s into the reaction chamber, cleaning for 20s by using high-purity inert gas, and flushing reaction byproducts and residual precursor; and (3) introducing 10s of hydrogen plasma into the reaction chamber, and then cleaning the reaction chamber for 20s by using high-purity inert gas to flush out reaction byproducts and residual gas. And cooling to room temperature, and taking out the aluminum foil.
(3) And (3) dripping a layer of conductive carbon paste on the surface of the anode foil obtained in the step (2), solidifying at room temperature, dripping silver paste, and placing silver wires as cathode leading-out terminals.
The conductivity of the cathode conductive layer prepared in this example was tested as follows: 0.3X 105S/cm。
Example 2
(1) Preparation work: and cutting the anode foil with the anode leading-out end by using an aluminum foil cutting die, and supplementing the cut edge.
(2) A metallic silver (Ag) thin film is deposited by Atomic Layer Deposition (ALD). The method specifically comprises the following steps: putting the anode foil obtained after the treatment in the step (1) into an ALD reaction chamber, vacuumizing to 0.5Pa, and keeping the deposition temperature at 140 ℃; setting the inlet temperature of the precursor to 125 ℃, introducing 3s of precursor (2, 2-dimethylpropionate) silver (I) triethylphosphine into the reaction chamber, cleaning for 9s by using high-purity inert gas, and flushing reaction byproducts and residual precursor; and (3) introducing a hydrogen plasma of 7s into the reaction chamber, cleaning for 9s by using a high-purity inert gas, and flushing reaction byproducts and residual gas. And cooling to room temperature, and taking out the aluminum foil.
(3) And (3) dripping a layer of conductive carbon paste on the surface of the anode foil obtained in the step (2), solidifying at room temperature, dripping silver paste, and placing silver wires as cathode leading-out terminals.
The conductivity of the cathode conductive layer prepared in this example was tested as follows: 2X 107S/cm。
Example 3
(1) Preparation work: and cutting the anode foil with the anode leading-out end by using an aluminum foil cutting die, and supplementing the cut edge.
(2) A thin film of metallic platinum (Pt) is deposited by Atomic Layer Deposition (ALD). The method specifically comprises the following steps: putting the anode foil obtained after the treatment in the step (1) into an ALD reaction chamber, vacuumizing to 0.5Pa, and keeping the deposition temperature at 250 ℃; setting the inlet temperature of the precursor to 155 ℃, introducing a precursor acetylacetone platinum for 8s into the reaction chamber, cleaning for 20s by using high-purity inert gas, and flushing reaction byproducts and residual precursor; after 5s of ozone is introduced into the reaction chamber, the reaction chamber is cleaned for 20s by using high-purity inert gas, and reaction byproducts and residual gas are flushed away. And cooling to room temperature, and taking out the aluminum foil.
(3) And (3) dripping a layer of conductive carbon paste on the surface of the anode foil obtained in the step (2), solidifying at room temperature, dripping silver paste, and placing silver wires as cathode leading-out terminals.
The conductivity of the cathode conductive layer prepared in this example was tested as follows: 1.6X 105S/cm。
Example 4
(1) Preparation work: and cutting the anode foil with the anode leading-out end by using an aluminum foil cutting die, and supplementing the cut edge.
(2) A metallic nickel (Ni) thin film is deposited by a chemical vapor deposition technique (CVD). The method specifically comprises the following steps: and (3) putting the anode foil obtained after the treatment in the step (1) into the middle of a quartz boat, and pushing the anode foil into a quartz tube (with the length of 100 cm and the inner diameter of 35 cm). Before heating to the set temperature (250 ℃), nitrogen gas with a certain flow rate is introduced into the furnace for 30 minutes, and air is discharged. Nickel acetylacetonate as a precursor was heated to 155 ℃ and introduced into a horizontal tube furnace for 3 seconds using nitrogen as a carrier gas. Then 20s of hydrogen were passed in. After growth, the tube furnace was cooled to room temperature under nitrogen atmosphere, and the aluminum foil was taken out.
(3) And (3) dripping a layer of conductive carbon paste on the surface of the anode foil obtained in the step (2), solidifying at room temperature, dripping silver paste, and placing silver wires as cathode leading-out terminals.
The conductivity of the cathode conductive layer prepared in this example was tested as follows: 1.3X 105S/cm。
Example 5
(1) Preparation work: and cutting the anode foil with the anode leading-out end by using an aluminum foil cutting die, and supplementing the cut edge.
(2) A metallic copper (Cu) film is deposited by Chemical Vapor Deposition (CVD). The method specifically comprises the following steps: and (3) putting the anode foil obtained after the treatment in the step (1) into the middle of a quartz boat, and pushing the anode foil into a quartz tube (with the length of 100 cm and the inner diameter of 35 cm). Before heating to the set temperature (250 ℃), nitrogen gas with a certain flow rate is introduced into the furnace for 30 minutes, and air is discharged. Copper (II) acetylacetonate as a precursor was heated to 130 ℃ and introduced into a horizontal tube furnace for 3 seconds using nitrogen as a carrier gas. Then 20s of hydrogen were passed in. After growth, the tube furnace was cooled to room temperature under nitrogen atmosphere, and the aluminum foil was taken out.
(3) And (3) dripping a layer of conductive carbon paste on the surface of the anode foil obtained in the step (2), solidifying at room temperature, dripping silver paste, and placing silver wires as cathode leading-out terminals.
The conductivity of the cathode conductive layer prepared in this example was tested as follows: 0.5X 105S/cm。
Example 6
(1) Preparation work: and cutting the anode foil with the anode leading-out end by using an aluminum foil cutting die, and supplementing the cut edge.
(1) A platinum (Pt) metal film was deposited by Chemical Vapor Deposition (CVD). The method specifically comprises the following steps: and (3) putting the anode foil obtained after the treatment in the step (1) into the middle of a quartz boat, and pushing the anode foil into a quartz tube (with the length of 100 cm and the inner diameter of 35 cm). Before heating to the set temperature (250 ℃), nitrogen gas with a certain flow rate is introduced into the furnace for 30 minutes, and air is discharged. Platinum (II) acetylacetonate as precursor was heated to 155 ℃ and passed into a horizontal tube furnace for 3 seconds with nitrogen as carrier gas. Then 20s of hydrogen were passed in. After growth, the tube furnace was cooled to room temperature under nitrogen atmosphere, and the aluminum foil was taken out.
(2) And (3) dripping a layer of conductive carbon paste on the surface of the anode foil obtained in the step (2), solidifying at room temperature, dripping silver paste, and placing silver wires as cathode leading-out terminals.
The conductivity of the cathode conductive layer prepared in this example was tested as follows: 1.3X 104S/cm。
Example 7
(1) Preparation work: and cutting the anode foil with the anode leading-out end by using an aluminum foil cutting die, and supplementing the cut edge.
(2) A thin film of aluminum metal (Al) is deposited by ALD technique. The method specifically comprises the following steps: putting the anode foil obtained after the treatment in the step (1) into an ALD reaction chamber, vacuumizing to 0.5Pa, and keeping the deposition temperature at 250 ℃; introducing a precursor Trimethylaluminum (TMA) for 3s into the reaction chamber, cleaning for 20s by using high-purity inert gas, and flushing reaction byproducts and residual precursor; and (3) introducing 10s of hydrogen plasma into the reaction chamber, and then cleaning the reaction chamber for 20s by using high-purity inert gas to flush out reaction byproducts and residual gas. And cooling to room temperature, and taking out the aluminum foil.
(3) And preparing the composite conductive layer by using an immersion method. Opening a certain amount of poly 3, 4-ethylenedioxythiophene/polystyrene sulfonate (PEDOT/PSS) dispersion liquid and the aluminum foil obtained after the treatment in the step (2) in a Schlenk bottle, vacuumizing, contacting the aluminum foil with the PEDOT/PSS dispersion liquid under a vacuum condition, and then soaking for 10min under the conditions of room temperature and normal pressure; drying in the shade for 12h at room temperature under normal pressure; oven drying at 80 deg.C and 200 deg.C for 10min and 40min respectively.
(4) And (4) dripping a layer of conductive carbon paste on the surface of the aluminum foil obtained after the treatment in the step (3), solidifying at room temperature, dripping silver paste, and placing silver wires as a cathode leading-out terminal.
The conductivity of the cathode conductive layer prepared in this example was tested as follows: 1.2X 104S/cm。
Example 8
(1) Preparation work: and cutting the anode foil with the anode leading-out end by using an aluminum foil cutting die, and supplementing the cut edge.
(2) A thin film of aluminum metal (Al) is deposited by ALD technique. The method specifically comprises the following steps: putting the anode foil obtained after the treatment in the step (1) into an ALD reaction chamber, vacuumizing to 0.5Pa, and keeping the deposition temperature at 250 ℃; introducing a precursor Trimethylaluminum (TMA) for 3s into the reaction chamber, cleaning for 20s by using high-purity inert gas, and flushing reaction byproducts and residual precursor; and (3) introducing 10s of hydrogen plasma into the reaction chamber, and then cleaning the reaction chamber for 20s by using high-purity inert gas to flush out reaction byproducts and residual gas. And cooling to room temperature, and taking out the aluminum foil.
(3) And (3) electrochemically polymerizing polypyrrole. Under room temperature and normal pressure, a constant current method (j is less than or equal to 5 mA-cm)-2Potential is less than or equal to 1V (relative to SCE)), and the anode obtained after the treatment of the step (2) is usedAluminum foil was electropolymerized in a solution containing 0.5M pyrrole monomer and 0.5M triisopropylnaphthalene sulfonate (TIPNS). And depositing a layer of polypyrrole on the surface of the titanium nitride to form a composite conductive layer in the solid-state aluminum electrolytic capacitor.
(4) And (4) dripping a layer of conductive carbon paste on the surface of the aluminum foil obtained in the step (3), solidifying at room temperature, dripping silver paste, and placing silver wires as cathode leading-out ends.
The conductivity of the cathode conductive layer prepared in this example was tested as follows: 3X 105S/cm。
Example 9
(1) Preparation work: and cutting the anode foil with the anode leading-out end by using an aluminum foil cutting die, and supplementing the cut edge.
(2) A thin film of aluminum metal (Al) is deposited by ALD technique. The method specifically comprises the following steps: putting the anode foil obtained after the treatment in the step (1) into an ALD reaction chamber, vacuumizing to 0.5Pa, and keeping the deposition temperature at 250 ℃; introducing a precursor Trimethylaluminum (TMA) for 3s into the reaction chamber, cleaning for 20s by using high-purity inert gas, and flushing reaction byproducts and residual precursor; and (3) introducing 10s of hydrogen plasma into the reaction chamber, and then cleaning the reaction chamber for 20s by using high-purity inert gas to flush out reaction byproducts and residual gas. And cooling to room temperature, and taking out the aluminum foil.
(3) Chemically polymerizing poly 3, 4-ethylenedioxythiophene (PEDOT). The method specifically comprises the following steps: and (3) immersing the anode foil subjected to the step (2) in a 60% EDOT monomer solution for 10min, and taking out. Oven drying at 50 deg.C for 45min, and taking out. Vacuumizing, soaking in 25% ferric p-toluenesulfonate solution for 10min, and taking out. Setting the temperature gradient to 50-60-120-200 deg.c, stoving in an oven and cooling to room temperature.
(3) And (4) dripping a layer of conductive carbon paste on the surface of the aluminum foil obtained in the step (3), solidifying at room temperature, dripping silver paste, and placing silver wires as cathode leading-out ends.
The conductivity of the cathode conductive layer prepared in this example was tested as follows: 0.3X 103S/cm。
Example 10
(1) Preparation work: and cutting the anode foil with the anode leading-out end by using an aluminum foil cutting die, and supplementing the cut edge.
(2) A metallic nickel (Ni) thin film is deposited by a chemical vapor deposition technique (CVD). The method specifically comprises the following steps: and (3) putting the anode foil obtained after the treatment in the step (1) into the middle of a quartz boat, and pushing the anode foil into a quartz tube (with the length of 100 cm and the inner diameter of 35 cm). Before heating to the set temperature (250 ℃), nitrogen gas with a certain flow rate is introduced into the furnace for 30 minutes, and air is discharged. Nickel acetylacetonate as a precursor was heated to 155 ℃ and introduced into a horizontal tube furnace for 3 seconds using nitrogen as a carrier gas. Then 20s of hydrogen were passed in. After growth, the tube furnace was cooled to room temperature under nitrogen atmosphere, and the aluminum foil was taken out.
(3) And preparing the composite conductive layer by using an immersion method. Opening a certain amount of poly 3, 4-ethylenedioxythiophene/polystyrene sulfonate (PEDOT/PSS) dispersion liquid and the aluminum foil obtained after the treatment in the step (2) in a Schlenk bottle, vacuumizing, contacting the aluminum foil with the PEDOT/PSS dispersion liquid under a vacuum condition, and then soaking for 10min under the conditions of room temperature and normal pressure; drying in the shade for 12h at room temperature under normal pressure; oven drying at 80 deg.C and 200 deg.C for 10min and 40min respectively.
(4) And (3) dripping a layer of conductive carbon paste on the surface of the aluminum foil obtained in the step (2), solidifying at room temperature, dripping silver paste, and placing silver wires as cathode leading-out ends.
The conductivity of the cathode conductive layer prepared in this example was tested as follows: 2.5X 103S/cm。
Example 11
(1) Preparation work: and cutting the anode foil with the anode leading-out end by using an aluminum foil cutting die, and supplementing the cut edge.
(2) A metallic nickel (Ni) thin film is deposited by a chemical vapor deposition technique (CVD). The method specifically comprises the following steps: and (3) putting the anode foil obtained after the treatment in the step (1) into the middle of a quartz boat, and pushing the anode foil into a quartz tube (with the length of 100 cm and the inner diameter of 35 cm). Before heating to the set temperature (250 ℃), nitrogen gas with a certain flow rate is introduced into the furnace for 30 minutes, and air is discharged. Nickel acetylacetonate as a precursor was heated to 155 ℃ and introduced into a horizontal tube furnace for 3 seconds using nitrogen as a carrier gas. Then 20s of hydrogen were passed in. After growth, the tube furnace was cooled to room temperature under nitrogen atmosphere, and the aluminum foil was taken out.
(3) And (3) electrochemically polymerizing polypyrrole. Under room temperature and normal pressure, a constant current method (j is less than or equal to 5 mA-cm)-2And the potential is less than or equal to 1V (relative to SCE)), and electropolymerization is carried out on the anode aluminum foil obtained after the treatment of the step (2) in a solution containing 0.5M pyrrole monomer and 0.5M triisopropyl naphthalene sulfonate (TIPNS). And depositing a layer of polypyrrole on the surface of the titanium nitride to form a composite conductive layer in the solid-state aluminum electrolytic capacitor.
(4) And (3) dripping a layer of conductive carbon paste on the surface of the aluminum foil obtained in the step (2), solidifying at room temperature, dripping silver paste, and placing silver wires as cathode leading-out ends.
The conductivity of the cathode conductive layer prepared in this example was tested as follows: 3.1X 104S/cm。
Example 12
(1) Preparation work: and cutting the anode foil with the anode leading-out end by using an aluminum foil cutting die, and supplementing the cut edge.
(2) A metallic nickel (Ni) thin film is deposited by a chemical vapor deposition technique (CVD). The method specifically comprises the following steps: and (3) putting the anode foil obtained after the treatment in the step (1) into the middle of a quartz boat, and pushing the anode foil into a quartz tube (with the length of 100 cm and the inner diameter of 35 cm). Before heating to the set temperature (250 ℃), nitrogen gas with a certain flow rate is introduced into the furnace for 30 minutes, and air is discharged. Nickel acetylacetonate as a precursor was heated to 155 ℃ and introduced into a horizontal tube furnace for 3 seconds using nitrogen as a carrier gas. Then 20s of hydrogen were passed in. After growth, the tube furnace was cooled to room temperature under nitrogen atmosphere, and the aluminum foil was taken out.
(3) Chemically polymerizing poly 3, 4-ethylenedioxythiophene (PEDOT). The method specifically comprises the following steps: and (3) immersing the anode foil subjected to the step (2) in a 60% EDOT monomer solution for 10min, and taking out. Oven drying at 50 deg.C for 45min, and taking out. Vacuumizing, soaking in 25% ferric p-toluenesulfonate solution for 10min, and taking out. Setting the temperature gradient to 50-60-120-200 deg.c, stoving in an oven and cooling to room temperature.
(4) And (3) dripping a layer of conductive carbon paste on the surface of the aluminum foil obtained in the step (2), solidifying at room temperature, dripping silver paste, and placing silver wires as cathode leading-out ends.
The conductivity of the cathode conductive layer prepared in this example was tested as follows: 6.4X 103S/cm。
Therefore, the conductivity test of the cathode conductive film of the solid-state aluminum electrolytic capacitor prepared in the above comparative example and example was carried out, and the experimental results obtained are shown in the following table 1:
table 1 conductivity of the prepared metal thin film
From the results in table 1, it can be seen that the conductivity of the conductive film obtained by the preparation method provided by the present invention is improved by 3 to 6 orders of magnitude compared with the conventional polymer conductive film prepared by the liquid phase method.
In summary, the present invention provides a method for preparing a metal-based conductive film on the surface of an anode foil dielectric layer of an aluminum electrolytic capacitor by using a gas phase chemical method, so as to solve the problems existing in the existing products and technologies: (1) the damage of the liquid solution to the anode aluminum foil dielectric layer deteriorates the voltage resistance and leakage current characteristics of the capacitor; (2) the nonuniformity of the conductive film and the residual ions in the solution reduce the conductivity of the film, increase the contact resistance of the device and reduce the frequency characteristic; (3) the solid cathode has low conductivity, which causes poor frequency characteristics of the capacitor; (4) the solid cathode conductive film is not compact enough to effectively resist the erosion of moisture to the anode foil dielectric layer.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (9)
1. A preparation method of a cathode conductive film of a solid-state aluminum electrolytic capacitor is characterized by comprising the following steps:
depositing a conductive metal film on the surface of the anode foil dielectric layer of the aluminum electrolytic capacitor by using a vapor deposition method;
and leading out a cathode electrode of the deposited conductive layer, namely preparing the conductive film on the surface of the anode foil dielectric layer of the aluminum electrolytic capacitor.
2. The method for preparing the cathode conductive film of the solid-state aluminum electrolytic capacitor as claimed in claim 1, wherein the geometric area size of the anode foil of the aluminum electrolytic capacitor is adjustable.
3. The method for preparing the cathode conductive film of the solid-state aluminum electrolytic capacitor according to claim 1, wherein the vapor deposition method comprises an atomic layer deposition method, a chemical vapor deposition method and a plasma-enhanced atomic layer deposition method.
4. The method for preparing a cathode conductive film of a solid-state aluminum electrolytic capacitor as claimed in claim 1, wherein the conductive metal film is made of an alloy material selected from the group consisting of aluminum, nickel, copper, zinc, silver, gold and platinum and aluminum, nickel, copper, zinc, silver, gold and platinum.
5. The method for preparing the cathode conductive film of the solid-state aluminum electrolytic capacitor according to claim 1, wherein the cathode electrode extraction of the deposited conductive layer is performed by using conductive carbon paste, silver paste, aluminum foil or silver wire.
6. The solid-state aluminum electrolytic capacitor cathode conductive film prepared by the preparation method of any one of claims 1 to 5.
7. Use of the solid aluminum electrolytic capacitor cathode conductive film of claim 6 as a solid aluminum electrolytic capacitor cathode.
8. The use of the conductive film of the cathode of the solid aluminum electrolytic capacitor as claimed in claim 6 in the preparation of a pre-deposited layer of the composite conductive cathode of the solid aluminum electrolytic capacitor.
9. The application of claim 8, wherein a composite conductive layer is prepared on the surface of the prepared cathode conductive film of the solid aluminum electrolytic capacitor, and then conductive carbon paste, silver paste, aluminum foil or silver wire is used as a cathode leading-out terminal of the composite conductive layer.
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| CN114242460A (en) * | 2021-12-21 | 2022-03-25 | 西安交通大学 | All-solid-state aluminum electrolytic capacitor device and ALD (atomic layer deposition) preparation method thereof |
| CN114267541A (en) * | 2021-12-21 | 2022-04-01 | 西安交通大学 | Solid tantalum electrolytic capacitor and ALD (atomic layer deposition) preparation method thereof |
| CN114974902A (en) * | 2022-06-22 | 2022-08-30 | 西安交通大学 | Method for preparing solid cathode of solid valve metal electrolytic capacitor by gas phase method |
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