CN109036852B - Three-dimensional porous aluminum electrode foil and preparation method thereof - Google Patents
Three-dimensional porous aluminum electrode foil and preparation method thereof Download PDFInfo
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- CN109036852B CN109036852B CN201810913489.XA CN201810913489A CN109036852B CN 109036852 B CN109036852 B CN 109036852B CN 201810913489 A CN201810913489 A CN 201810913489A CN 109036852 B CN109036852 B CN 109036852B
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 251
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 210
- 239000011888 foil Substances 0.000 title claims abstract description 186
- 238000002360 preparation method Methods 0.000 title claims description 5
- 239000000843 powder Substances 0.000 claims abstract description 83
- 238000000034 method Methods 0.000 claims abstract description 65
- 239000002131 composite material Substances 0.000 claims abstract description 47
- 239000000758 substrate Substances 0.000 claims abstract description 44
- 238000011282 treatment Methods 0.000 claims abstract description 39
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 25
- 239000000835 fiber Substances 0.000 claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 claims abstract description 17
- 239000011812 mixed powder Substances 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 238000001125 extrusion Methods 0.000 claims abstract description 7
- 238000005452 bending Methods 0.000 claims abstract description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 38
- 230000036571 hydration Effects 0.000 claims description 31
- 238000006703 hydration reaction Methods 0.000 claims description 31
- 239000000203 mixture Substances 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 17
- 238000005097 cold rolling Methods 0.000 claims description 16
- 230000003746 surface roughness Effects 0.000 claims description 16
- 230000003647 oxidation Effects 0.000 claims description 14
- 238000007254 oxidation reaction Methods 0.000 claims description 14
- 239000003792 electrolyte Substances 0.000 claims description 10
- 229910000838 Al alloy Inorganic materials 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims description 4
- 229910002113 barium titanate Inorganic materials 0.000 claims description 4
- 229910052593 corundum Inorganic materials 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 4
- 238000009703 powder rolling Methods 0.000 claims description 3
- 239000002356 single layer Substances 0.000 claims description 3
- 238000005096 rolling process Methods 0.000 claims 1
- 238000005336 cracking Methods 0.000 abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 28
- 239000002253 acid Substances 0.000 description 27
- 239000000463 material Substances 0.000 description 27
- 239000003990 capacitor Substances 0.000 description 17
- 238000003825 pressing Methods 0.000 description 15
- 229910052786 argon Inorganic materials 0.000 description 14
- 239000000919 ceramic Substances 0.000 description 14
- 238000013329 compounding Methods 0.000 description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 9
- 238000007669 thermal treatment Methods 0.000 description 9
- 230000002829 reductive effect Effects 0.000 description 8
- 238000005530 etching Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- 239000002002 slurry Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000005056 compaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000011268 mixed slurry Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004804 winding 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
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/002—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of porous nature
- B22F7/004—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of porous nature comprising at least one non-porous part
-
- 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
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
- H01G9/055—Etched foil electrodes
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Composite Materials (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
- Powder Metallurgy (AREA)
- Cell Electrode Carriers And Collectors (AREA)
Abstract
The invention provides a novel three-dimensional porous aluminum electrode foil, which comprises an aluminum foil substrate and a composite porous aluminum film formed by mixed powder on two surfaces of the aluminum foil substrate, wherein the total thickness of the electrode foil is 80-200 mu m, the voltage is 300-600V, the bending frequency is 50-340 times, and the specific volume is 0.70-2.55 mu F/cm2. The invention also provides a method for preparing the novel three-dimensional porous aluminum electrode foil, which comprises the following steps of firstly, uniformly mixing aluminum-containing powder, aluminum fibers and high-dielectric oxide powder to obtain mixed powder; uniformly dispersing the mixed powder on two sides of an aluminum foil substrate, and compacting to form a close-packed porous foil; then carrying out thermalization treatment on the porous foil, and controlling the porosity to be 35-45% and the thickness to be 80-200 μm through extrusion treatment; and finally, carrying out formation energizing treatment on the porous aluminum electrode foil after the thermalization treatment. The three-dimensional porous aluminum electrode foil provided by the invention has the properties of high specific volume, high strength and the like, and the composite porous aluminum film on the aluminum foil substrate has the characteristics of no cracking, no falling off, good binding force and the like in the production process.
Description
Technical Field
The invention relates to a novel three-dimensional porous aluminum electrode foil for an aluminum electrolytic capacitor, in particular to an anode electrode foil for medium-high voltage and ultrahigh voltage aluminum electrolytic capacitors and a manufacturing method thereof.
Background
The electrode foil is a key raw material of an aluminum electrolytic capacitor, and the aluminum electrolytic capacitor is one of three components which must be used by various household appliances, computers, communication equipment, automation equipment and the like. The quality of the electrode foil is related to the service life of the capacitor, and directly influences the service life of the electronic whole machine. With the rapid development of the electronic industry, the aluminum electrolytic capacitor is more widely used, and the requirements of miniaturization, long service life and high reliability are increasingly urgent, and the electrode foil processing technology also becomes one of the core technologies for manufacturing the aluminum electrolytic capacitor, and the requirement of high specific volume, especially high strength, must be met to obtain the miniaturization requirement. The traditional electrode foil forms tunnel-type holes by implementing electrochemical etching treatment, the surface area can be increased, but the length of the tunnel hole diameter is difficult to uniformly control, the KDK and JCC control is ideal at present, but the foil with high specific volume is corroded, the problem caused by poor strength is difficult to cut and wind, and the electrode foil is not suitable for capacitor miniaturization. In the formation and energization stage, the thickness of the oxide film increases with the increase of the voltage, the aluminum matrix remained in the aluminum foil is reduced, the strength is greatly reduced, and the high specific volume electrode foil is difficult to be applied to high-voltage and ultrahigh-voltage aluminum electrolytic capacitors. In addition, the traditional etching process needs a large amount of environmental pollution raw materials such as hydrochloric acid, sulfuric acid and nitric acid, and brings great pressure to environmental protection treatment.
In recent years, instead of a method of forming an electrode foil for an aluminum anode, in which a surface area is increased by etching, a sintered body of porous aluminum powder prepared by sputtering, vapor deposition, sintering, or the like has been proposed, and, as disclosed in chinese patents CN 102714098B, CN102804302A and CN 103688327A, CN 104409215A, CN 104919552A, a sintered body of aluminum powder prepared by preparing a slurry from aluminum and aluminum alloy powder, coating the slurry on a metal substrate, and then sintering the slurry to form a porous sintered layer has an effect of increasing the specific surface area of the foil. It was confirmed that the surface area of the electrode foil for aluminum electrolytic capacitors obtained by the sintered body of the porous aluminum powder was equal to or larger than the pit area formed by the etching treatment. However, sputtering and evaporation are difficult to increase in thickness, suitable for cathode or low voltage foils, require fewer defects due to high and high voltages, reduce leakage current, increase the lifetime of capacitors, and use of high dielectric materials such as TiO2High dielectric constant materials have problems of poor binding force, easy film falling and difficult practical application for high pressure and ultrahigh pressure. These methods have problems of poor strength, large leakage current, difficulty in stabilization into anode energization production and capacitor winding production, and the like. Patent CN 104919552a discloses a method for manufacturing a sintered coating by etching, but the acid-base treatment makes environmental treatment difficult and makes stable production difficult.
Disclosure of Invention
In order to overcome the defects and shortcomings of the prior art, the invention provides a three-dimensional porous aluminum electrode foil of a high-specific-volume high-strength aluminum electrolytic capacitor, which has high strength and high specific volume and meets the requirements of electrode materials for medium-high voltage and ultrahigh voltage aluminum electrolytic capacitors. In another aspect, a method for preparing the three-dimensional porous aluminum electrode foil by metal powder rolling is provided.
According to the technical scheme, the novel three-dimensional porous aluminum electrode foil comprises an aluminum foil substrate and a composite porous aluminum film formed on two sides of the aluminum foil substrate by mixed powder, and the total thickness of the three-dimensional porous aluminum electrode foil is 80-200 mu m.
According to the novel three-dimensional porous aluminum electrode foil provided by the technical scheme, the voltage of the novel three-dimensional porous aluminum electrode foil is 300-600V, the bending times are 50-340 times, and the specific volume is 0.70-2.55 mu F/cm2。
According to the novel three-dimensional porous aluminum electrode foil provided by the technical scheme, the thickness of the aluminum foil base material is 20-100 mu m, and the purity is not lower than 99.92%.
According to the novel three-dimensional porous aluminum electrode foil provided by the technical scheme, the thickness of the composite porous aluminum film single layer is 20-100 μm, and in other embodiments, the thickness of the composite porous aluminum film single layer is 30 μm, 35 μm, 40 μm, 45 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm or 100 μm.
According to the novel three-dimensional porous aluminum electrode foil provided by the technical scheme, the novel three-dimensional porous aluminum electrode foil is prepared by metal powder rolling, and the porosity of the novel three-dimensional porous aluminum electrode foil is 35% -45%.
According to the technical scheme, in the mixed powder, the aluminum-containing powder accounts for 95-99%, the aluminum fiber accounts for 0.5-5%, and the high dielectric oxide powder accounts for 0.05-2%. The high dielectric oxide added in the invention has the functions of bonding and supporting, can prevent the aluminum powder from seriously deforming due to the increase of the reduction amount, and simultaneously ensures the porosity.
According to the novel three-dimensional porous aluminum electrode foil provided by the technical scheme, the aluminum-containing powder is selected from at least one of aluminum or aluminum alloy powder.
According to the novel three-dimensional porous aluminum electrode foil provided by the technical scheme, the high-dielectric oxide powder is selected from Al2O3、TiO2And barium titanate.
According to the novel three-dimensional porous aluminum electrode foil provided by the technical scheme, in the subsequent actual production, single particle size is difficult to classify, the price is high, a large amount of waste is generated, and the production cost is increased, so that the particle size adopted in the material mixing process is different, the maximum particle size is 20 micrometers, the minimum particle size is 0.5 micrometers, and the shapes are different, namely, spindle, strip, cylinder, fiber and sheet. Although the problems of filtration and uniform dispersion of the mixed slurry are caused by the overlapping, and the specific capacity is reduced, the integral thermalization composite effect is obvious, the phenomena of serious compaction, porosity reduction and cracking are not easy to occur, and the production cost is greatly saved. Thus in some embodiments the particle size of the aluminium-containing powder is 1 to 20 μm; in other embodiments, the aluminum-containing powder has a particle size of 3 to 15 μm. In addition, the voltage of the three-dimensional porous aluminum electrode foil can be controlled by controlling the particle size of the powder, and the voltage of the obtained three-dimensional porous aluminum electrode foil is also reduced a little by reducing the particle size of the powder in general.
According to the novel three-dimensional porous aluminum electrode foil provided by the technical scheme, the diameter of the aluminum fiber is 3-10 mu m, and the length of the aluminum fiber is 1-500 mu m; according to the technical scheme, the novel three-dimensional porous aluminum electrode foil is high-dielectric oxidized powder, the purity is not lower than 99.9%, and the granularity is 0.2-5 mu m.
According to the novel three-dimensional porous aluminum electrode foil provided by the technical scheme, the three-dimensional porous aluminum electrode foil is prepared by combining mixed powder on an aluminum foil through extrusion and thermalization treatment and performing formation treatment.
In another aspect, the invention provides a method for preparing the novel three-dimensional porous aluminum electrode foil, which comprises the following steps:
1) uniformly mixing aluminum-containing powder, aluminum fibers and high-dielectric oxide powder to obtain mixed powder;
2) uniformly dispersing the mixed powder on two sides of an aluminum foil substrate, and compacting to form a close-packed porous foil;
3) carrying out thermalization treatment on the densely-packed porous foil, and controlling the porosity to be 35-45% and the thickness to be 80-200 μm through extrusion treatment to finally form a composite mesh-shaped porous aluminum electrode foil;
4) and carrying out formation energizing treatment on the porous aluminum electrode foil after the thermalization treatment.
According to the method provided by the technical scheme, the powder is mixedIn the aluminum-containing composite material, the aluminum-containing powder accounts for 95 to 99 percent, the aluminum fiber accounts for 0.5 to 5 percent and the high dielectric oxide powder accounts for 0.05 to 2 percent by weight; wherein the aluminum-containing powder is selected from at least one of aluminum or aluminum alloy powder, and the high dielectric oxide powder is selected from Al2O3、TiO2And barium titanate.
According to the method provided by the technical scheme, the particle size of the aluminum-containing powder is 1-20 μm; the diameter of the aluminum fiber is 3-10 μm, and the length is 1-500 μm; high dielectric oxidation powder with purity not lower than 99.9% and granularity 0.2-5 micron.
According to the method provided by the technical scheme, the compaction treatment is performed by cold roll pressing, and the pressure is controlled to be 50-300 Kg; the extrusion treatment is also carried out by cold rolling at a temperature of 300 ℃ and a pressure of 15-20 Kg.
According to the method provided by the technical scheme, the mixed powder is uniformly dispersed on two surfaces of the aluminum substrate, namely the surface roughness of the mixed powder is controlled to be not more than +/-8 mu m.
According to the method provided by the technical scheme, the extrusion foil is subjected to thermalization treatment, so that the aluminum substrate and the powder are directly thermally fused to form the thermalized porous aluminum electrode foil with a firm porous net structure, wherein the thermalization treatment is carried out under the vacuum or inert gas condition.
According to the method provided by the technical scheme, the temperature of the thermalization treatment is 550-670 ℃, and the treatment time is 1-30 min.
According to the method provided by the technical scheme, the inert gas is selected from N2Or Ar2。
According to the method provided by the technical scheme, the reductive electrolyte is added in the hydration process of the formation energy endowing treatment.
According to the method provided by the technical scheme, the reductive electrolyte added in the hydration process of the formation energizing treatment is hydrogen peroxide or citric acid, and the content of the reductive electrolyte is 0.01-0.5%; in other embodiments, the reducing electrolyte is hydrogen peroxide, and the content of the reducing electrolyte is 0.05% -0.10%. The addition of reducing substances in the energizing treatment process can eliminate the surface stress and residual decomposers of the composite aluminum foil and increase the bonds and the capacity among the composite aluminum foil particles. Thereby thoroughly solving the problems of cracking and foil breakage during production and greatly improving the bending strength.
The "aluminum foil" in the present invention is not limited to plain foil, etched foil and formed foil, but plain foil is preferred.
The "aluminum alloy powder" as used herein means a powder having a purity of 99.92% or more, a D50 average particle diameter of 1 to 15 μm, and containing Si, Fe, Cu, Mn, Mg, etc.
All ranges cited herein are inclusive, unless expressly stated to the contrary. For example, "the temperature of the thermal treatment is 550 ℃" and 670 ℃ ", which means that the reaction temperature T is in the range of 550 ℃. ltoreq.T.ltoreq.670 ℃.
The term "or" as used herein means that alternatives, if appropriate, can be combined, that is, the term "or" includes each listed individual alternative as well as combinations thereof. For example, "the reducing electrolyte is hydrogen peroxide or citric acid" means that the reducing electrolyte may be one of hydrogen peroxide or citric acid, or a combination of one or more thereof.
The invention has the beneficial effects that:
the invention provides a novel three-dimensional porous aluminum electrode foil, which comprises an aluminum foil substrate and composite porous aluminum films formed on two surfaces of the aluminum foil substrate by mixed powder, is suitable for medium-high voltage and ultrahigh voltage aluminum electrolytic capacitors, has the characteristics of good mechanical property and high specific volume, and has the characteristics of no cracking, no falling, good binding force and the like in the production process of the composite porous aluminum films on the aluminum foil substrate. And can realize energized and stabilized production.
The invention provides a preparation method of a novel three-dimensional porous aluminum electrode foil, which is a foil rolled by metal powder, wherein powder is uniformly distributed on an aluminum substrate, and then the foil is rolled to form a closely packed porous foil, the closely packed porous foil is subjected to thermalization treatment to form a composite mesh-shaped porous aluminum electrode foil, the composite aluminum foil is subjected to formation energization, and environment-friendly reductive hydration treatment is performed in the formation energization stage to realize modification and reformation of a composite mesh structure, the porous aluminum electrode foil is not required to be subjected to treatments of etching, surface roughening or elimination of surface oxide film thickness and the like, the production stability and high strength requirements are ensured, and the high-specific-volume and high-strength electrode foil suitable for medium-high-voltage and ultrahigh-voltage aluminum electrolytic capacitors is formed.
Detailed Description
The following are preferred embodiments of the present invention, and the present invention is not limited to the following preferred embodiments. It should be noted that various changes and modifications based on the inventive concept herein will occur to those skilled in the art and are intended to be included within the scope of the present invention. The starting materials used in the examples are all commercially available.
Comparative example 1
And (3) forming tunnel holes in the annealed soft optical foil with the thickness of 130 mu m by using a known etching process, and then carrying out formation-anodic oxidation to obtain the electrode foil. The process is a manufacturing method of a large amount of electrode foils for producing aluminum electrolytic capacitors on the market at present.
Comparative example 2
Pushing aluminum powder with the average grain diameter D50 of 3 mu m onto an aluminum foil base material with the average grain diameter of 30 mu m through powder spraying or a screw pump, controlling the surface uniformity of a single surface through a scraper so that the surface roughness of the powder is not more than +/-8 mu m, and preliminarily compacting the aluminum powder by cold rolling under the pressure of 100 Kg; then, carrying out 630 ℃ thermal treatment on the aluminum foil with the surface coated with the aluminum powder of 800mm under the protection of argon under the support of a ceramic roller, controlling the porosity and the thickness by a cold pressing roller when cooling to 300 ℃, preferably controlling the pressure to be 15Kg and the porosity to be 40%, repeating the process, and compounding 50 mu m of aluminum powder on the other surface of the aluminum substrate to obtain a thermal composite porous foil with the total thickness of 130 mu m; and carrying out a conventional mixed acid energizing formation process on the thermalized composite foil to obtain the electrode foil with high specific volume and high strength.
Example 1
Aluminum powder with the average grain diameter D50 of 3 mu m is pushed to an aluminum foil base material with the diameter of 30 mu m through powder spraying or a screw pump, the surface uniformity of a single surface is controlled through a scraper, the surface roughness of the powder is enabled to be not more than +/-8 mu m, the pressure is controlled to be 200Kg through cold rolling 1, the aluminum powder is preliminarily compacted, and the thickness of the single surface is controlled to be 50 mu m; then, carrying out 570 ℃ thermalization treatment on the aluminum foil with the surface coated with aluminum powder of 800mm under the protection of argon under the support of a ceramic roller, and controlling the porosity and the thickness by a cold pressing roller 2 when the aluminum foil is cooled to 300 ℃, wherein the preferable pressure is 20Kg, and the porosity is 40%; repeating the above process, compounding aluminum powder of 50 μm on the other side of the aluminum substrate to obtain a thermalized composite porous foil with a total thickness of 130 μm, performing mixed acid energizing on the thermalized composite porous aluminum foil, adding 0.05% hydrogen peroxide into a hydration tank in the hydration process, and performing a conventional mixed acid energizing formation process to obtain the electrode foil with high specific volume and high strength.
Example 2
Pushing aluminum powder with the average particle size D50 of 5 microns onto an aluminum foil base material with the average particle size of 30 microns through powder spraying or a screw pump, controlling the surface uniformity of a single surface through a scraper so that the surface roughness of the powder is not more than +/-8 microns, and preliminarily compacting the aluminum powder by cold rolling 1 under the pressure of 150 Kg; then, carrying out 570 ℃ thermalization treatment on the aluminum foil with the surface coated with aluminum powder of 800mm under the protection of argon under the support of a ceramic roller, and controlling the porosity and the thickness by using a cold pressing roller 2 when the aluminum foil is cooled to 300 ℃, wherein the preferable pressure is 20Kg, and the porosity is 35%; repeating the above process, and compounding 50 μm aluminum powder on the other surface of the aluminum substrate to obtain a total thickness of 130 μm thermal compound porous foil; and (3) carrying out mixed acid energizing on the thermalized composite foil, adding 0.05% hydrogen peroxide into a hydration tank in the hydration process, and then carrying out a conventional mixed acid energizing formation process to obtain the electrode foil with high specific volume and high strength.
Example 3
Pushing aluminum powder with the average grain diameter D50 of 3 mu m onto an aluminum foil base material with the average grain diameter of 30 mu m through powder spraying or a screw pump, controlling the surface uniformity of a single surface through a scraper so that the surface roughness of the powder is not more than +/-8 mu m, and preliminarily compacting the aluminum powder by cold rolling 1 under the pressure of 100 Kg; then, carrying out 630 ℃ heat treatment on the aluminum foil with the surface coated with the aluminum powder of 800mm under the protection of argon under the support of a ceramic roller, controlling the porosity and the thickness by a cold pressing roller 2 when the aluminum foil is cooled to 300 ℃, preferably controlling the pressure to be 15Kg and the porosity to be 40%, repeating the process, and compounding 50 mu m of aluminum powder on the other surface of the aluminum substrate to obtain a heat treatment composite porous foil with the total thickness of 130 mu m; and (3) carrying out mixed acid energizing on the thermalized composite foil, adding 0.05% hydrogen peroxide into a hydration tank in the hydration process, and then carrying out a conventional mixed acid energizing formation process to obtain the electrode foil with high specific volume and high strength.
Example 4
Mixing aluminum powder with the average grain size D50 of 3 mu m, aluminum fiber with the diameter of 3-10 mu m and the length of 10-100 mu m and high dielectric oxidation powder with the average grain size of 0.5-2 mu m into a uniform mixture by a dry powder mixer, wherein the weight ratio of the three is 95:4: 1; then the mixed material is pushed to an aluminum foil substrate with the thickness of 30 mu m through a screw pump, the uniformity of the surface of a single surface is controlled through a scraper, the surface roughness of the powder is enabled to be not more than +/-8 mu m, the mixed material is preliminarily compacted through cold rolling 1 under the pressure of 100 Kg; then, carrying out 570 ℃ heat treatment on the aluminum foil with the surface coated with the aluminum mixture in 800mm under the protection of argon under the support of a ceramic roller, controlling the porosity and the thickness by a cold pressing roller 2 when the aluminum foil is cooled to 300 ℃, preferably, controlling the pressure to be 15Kg and the porosity to be 45%, repeating the process, and compounding 50 mu m of aluminum powder on the other surface of the aluminum substrate to obtain a heat treatment composite porous foil with the total thickness of 130 mu m; and (3) carrying out mixed acid energizing on the thermalized composite foil, adding 0.05% hydrogen peroxide into a hydration tank in the hydration process, and then carrying out a conventional mixed acid energizing formation process to obtain the electrode foil with high specific volume and high strength.
Example 5
Mixing aluminum powder with the average grain size D50 of 3 mu m, aluminum fiber with the diameter of 3-10 mu m and the length of 10-100 mu m and high dielectric oxidation powder with the average grain size of 0.5-2 mu m into a uniform mixture by a dry powder mixer, wherein the weight ratio of the three is 95:4: 1; then the mixed material is pushed to an aluminum foil substrate with the thickness of 30 mu m through a screw pump, the uniformity of the surface of a single surface is controlled through a scraper, the surface roughness of the powder is enabled to be not more than +/-8 mu m, the mixed material is preliminarily compacted through cold rolling 1 under the pressure of 100 Kg; then, carrying out 630 ℃ thermal treatment on the aluminum foil with the surface coated with the aluminum mixture in a thickness of 800mm under the protection of argon under the support of a ceramic roller, controlling the porosity and the thickness by a cold pressing roller 2 when the aluminum foil is cooled to 300 ℃, preferably controlling the pressure to be 15Kg and the porosity to be 40%, repeating the process, and compounding 50 mu m aluminum powder on the other surface of the aluminum substrate to obtain a thermal composite porous foil with the total thickness of 130 mu m; and (3) carrying out mixed acid energizing on the thermalized composite foil, adding 0.05% hydrogen peroxide into a hydration tank in the hydration process, and then carrying out a conventional mixed acid energizing formation process to obtain the electrode foil with high specific volume and high strength.
Example 6
Mixing aluminum powder with the average grain size D50 of 3 mu m, aluminum fiber with the diameter of 3-10 mu m and the length of 10-100 mu m and high dielectric oxidation powder with the average grain size of 0.5-2 mu m into a uniform mixture by a dry powder mixer, wherein the weight ratio of the three is 96:3: 1; then the mixed material is pushed to an aluminum foil substrate with the thickness of 30 mu m through a screw pump, the uniformity of the surface of a single surface is controlled through a scraper, the surface roughness of the powder is enabled to be not more than +/-8 mu m, the mixed material is preliminarily compacted through cold rolling 1 under the pressure of 100 Kg; then, the aluminum foil 800mm coated with the aluminum mixture on the surface is heated under the protection of argon gas at 600 ℃ under the support of a ceramic roller, when the aluminum foil is cooled to 300 ℃, the porosity and the thickness are controlled by a cold pressing roller 2, the preferred pressure is 15Kg, the porosity is 40%, the above process is repeated, and 50 μm of aluminum powder is compounded on the other surface of the aluminum substrate, so that the heated composite porous foil with the total thickness of 130 μm is obtained; and (3) carrying out mixed acid energizing on the thermalized composite foil, adding 0.05% hydrogen peroxide into a hydration tank in the hydration process, and then carrying out a conventional mixed acid energizing formation process to obtain the electrode foil with high specific volume and high strength.
Example 7
Mixing aluminum powder with the average grain size D50 of 3 mu m, aluminum fiber with the diameter of 3-10 mu m and the length of 10-100 mu m and high dielectric oxidation powder with the average grain size of 0.5-2 mu m by a dry powder mixer to obtain a uniform mixture, wherein the weight ratio of the three is 96:3: 1; then the mixed material is pushed to an aluminum foil substrate with the thickness of 30 mu m through a screw pump, the uniformity of the surface of a single surface is controlled through a scraper, the surface roughness of the powder is not more than +/-8 mu m, the mixed material is preliminarily compacted through cold rolling 1 under the pressure of 300 Kg; then, carrying out 630 ℃ thermal treatment on the aluminum foil with the surface coated with the aluminum mixture in a thickness of 800mm under the protection of argon under the support of a ceramic roller, controlling the porosity and the thickness by a cold pressing roller 2 when the aluminum foil is cooled to 300 ℃, preferably, controlling the pressure to be 10Kg and the porosity to be 40%, repeating the process, and compounding 50 mu m aluminum powder on the other surface of the aluminum substrate to obtain a thermal composite porous foil with the total thickness of 130 mu m; and (3) carrying out mixed acid energizing on the thermalized composite foil, adding 0.05% hydrogen peroxide into a hydration tank in the hydration process, and then carrying out a conventional mixed acid energizing formation process to obtain the electrode foil with high specific volume and high strength.
Example 8
Mixing aluminum powder with the average grain size D50 of 3 mu m, aluminum fiber with the diameter of 3-10 mu m and the length of 10-100 mu m and high dielectric oxidation powder with the average grain size of 0.5-2 mu m into a uniform mixture by a dry powder mixer, wherein the weight ratio of the three is 96:2: 2; then the mixed material is pushed to an aluminum foil substrate with the thickness of 30 mu m through a screw pump, the uniformity of the surface of a single surface is controlled through a scraper, the surface roughness of the powder is enabled to be not more than +/-8 mu m, the mixed material is preliminarily compacted through cold rolling 1 under the pressure of 250 Kg; then, carrying out 630 ℃ thermal treatment on the aluminum foil with the surface coated with the aluminum mixture in a thickness of 800mm under the protection of argon under the support of a ceramic roller, controlling the porosity and the thickness by a cold pressing roller 2 when the aluminum foil is cooled to 300 ℃, preferably, controlling the pressure to be 10Kg and the porosity to be 45%, repeating the process, and compounding 50 mu m aluminum powder on the other surface of the aluminum substrate to obtain a thermal composite porous foil with the total thickness of 130 mu m; and (3) carrying out mixed acid energizing on the thermalized composite foil, adding 0.05% hydrogen peroxide into a hydration tank in the hydration process, and then carrying out a conventional mixed acid energizing formation process to obtain the electrode foil with high specific volume and high strength.
Example 9
Mixing aluminum powder with the average grain size D50 of 3 mu m, aluminum fiber with the diameter of 3-10 mu m and the length of 10-100 mu m and high dielectric oxidation powder with the average grain size of 0.5-2 mu m by a dry powder mixer into a uniform mixture, wherein the weight ratio of the three is 96:2: 2; then the mixed material is pushed to an aluminum foil substrate with the thickness of 30 mu m through a screw pump, the uniformity of the surface of a single surface is controlled through a scraper, the surface roughness of the powder is not more than +/-8 mu m, the pressure is controlled to be 50Kg through cold rolling 1, and the mixed material is preliminarily compacted; then, the aluminum foil 800mm coated with the aluminum mixture on the surface is heated under the protection of argon at 640 ℃ under the support of a ceramic roller, when the aluminum foil is cooled to 300 ℃, the porosity and the thickness are controlled by a cold pressing roller 2, the preferred pressure is 10Kg, the porosity is 35 percent, the above process is repeated, and 50 mu m of aluminum powder is compounded on the other surface of the aluminum substrate, so that the heated composite porous foil with the total thickness of 130 mu m is obtained; and (3) carrying out mixed acid energizing on the thermalized composite foil, adding 0.05% hydrogen peroxide into a hydration tank in the hydration process, and then carrying out a conventional mixed acid energizing formation process to obtain the electrode foil with high specific volume and high strength.
Example 10
Mixing aluminum powder with the average grain size D50 of 3 mu m, aluminum fiber with the diameter of 3-10 mu m and the length of 10-100 mu m and high dielectric oxidation powder with the average grain size of 0.5-2 mu m by a dry powder mixer into a uniform mixture, wherein the weight ratio of the three is 96:2: 2; then the mixed material is pushed to an aluminum foil substrate with the thickness of 30 mu m through a screw pump, the uniformity of the surface of a single surface is controlled through a scraper, the surface roughness of the powder is enabled to be not more than +/-8 mu m, the mixed material is preliminarily compacted through cold rolling 1 under the pressure of 100 Kg; then, carrying out 630 ℃ thermal treatment on the aluminum foil with the surface coated with the aluminum mixture in a thickness of 800mm under the protection of argon under the support of a ceramic roller, controlling the porosity and the thickness by a cold pressing roller 2 when the aluminum foil is cooled to 300 ℃, preferably, controlling the pressure to be 10Kg and the porosity to be 45%, repeating the process, and compounding 50 mu m aluminum powder on the other surface of the aluminum substrate to obtain a thermal composite porous foil with the total thickness of 130 mu m; and (3) carrying out mixed acid energizing on the thermalized composite foil, adding 0.1% hydrogen peroxide into a hydration tank in the hydration process, and then carrying out a conventional mixed acid energizing formation process to obtain the electrode foil with high specific volume and high strength.
Example 11
Mixing aluminum powder with the average grain size D50 of 3 mu m, aluminum fiber with the diameter of 3-10 mu m and the length of 10-100 mu m and high dielectric oxidation powder with the average grain size of 0.5-2 mu m by a dry powder mixer into a uniform mixture, wherein the weight ratio of the three is 96:2: 2; then the mixed material is pushed to an aluminum foil substrate with the thickness of 30 mu m through a screw pump, the uniformity of the surface of a single surface is controlled through a scraper, the surface roughness of the powder is enabled to be not more than +/-8 mu m, the mixed material is preliminarily compacted through cold rolling 1 under the pressure of 100 Kg; then, carrying out 630 ℃ thermal treatment on the aluminum foil with the surface coated with the aluminum mixture in a thickness of 800mm under the protection of argon under the support of a ceramic roller, controlling the porosity and the thickness by a cold pressing roller 2 when the aluminum foil is cooled to 300 ℃, preferably, controlling the pressure to be 10Kg and the porosity to be 45%, repeating the process, and compounding 50 mu m aluminum powder on the other surface of the aluminum substrate to obtain a thermal composite porous foil with the total thickness of 130 mu m; and (3) carrying out mixed acid energizing on the thermalized composite foil, adding 0.4% hydrogen peroxide into a hydration tank in the hydration process, and then carrying out a conventional mixed acid energizing formation process to obtain the electrode foil with high specific volume and high strength.
Example 12
Mixing aluminum powder with the average grain size D50 of 5 mu m, aluminum fiber with the diameter of 3-10 mu m and the length of 10-100 mu m and high dielectric oxidation powder with the average grain size of 0.5-2 mu m by a dry powder mixer into a uniform mixture, wherein the weight ratio of the three is 96:2: 2; then the mixed material is pushed to an aluminum foil substrate with the thickness of 30 mu m through a screw pump, the uniformity of the surface of a single surface is controlled through a scraper, the surface roughness of the powder is enabled to be not more than +/-8 mu m, the mixed material is preliminarily compacted through cold rolling 1 under the pressure of 100 Kg; then, carrying out 630 ℃ thermal treatment on the aluminum foil with the surface coated with the aluminum mixture in a thickness of 800mm under the protection of argon under the support of a ceramic roller, controlling the porosity and the thickness by a cold pressing roller 2 when the aluminum foil is cooled to 300 ℃, preferably, controlling the pressure to be 10Kg and the porosity to be 35%, repeating the process, and compounding 50 mu m aluminum powder on the other surface of the aluminum substrate to obtain a thermal composite porous foil with the total thickness of 130 mu m; and (3) carrying out mixed acid energizing on the thermalized composite foil, adding 0.1% hydrogen peroxide into a hydration tank in the hydration process, and then carrying out a conventional mixed acid energizing formation process to obtain the electrode foil with high specific volume and high strength.
Example 13
Mixing aluminum powder with the average grain size D50 of 5 mu m, aluminum fiber with the diameter of 3-10 mu m and the length of 10-100 mu m and high dielectric oxidation powder with the average grain size of 0.5-2 mu m by a dry powder mixer into a uniform mixture, wherein the weight ratio of the three is 96:2: 2; then the mixed material is pushed to an aluminum foil substrate with the thickness of 30 mu m through a screw pump, the uniformity of the surface of a single surface is controlled through a scraper, the surface roughness of the powder is enabled to be not more than +/-8 mu m, the mixed material is preliminarily compacted through cold rolling 1 under the pressure of 100 Kg; then, carrying out 630 ℃ thermal treatment on the aluminum foil with the surface coated with the aluminum mixture in a thickness of 800mm under the protection of argon under the support of a ceramic roller, controlling the porosity and the thickness by a cold pressing roller 2 when the aluminum foil is cooled to 300 ℃, preferably, controlling the pressure to be 10Kg and the porosity to be 35%, repeating the process, and compounding 50 mu m aluminum powder on the other surface of the aluminum substrate to obtain a thermal composite porous foil with the total thickness of 130 mu m; and (3) carrying out mixed acid energizing on the thermalized composite foil, adding 0.4% hydrogen peroxide into a hydration tank in the hydration process, and then carrying out a conventional mixed acid energizing formation process to obtain the electrode foil with high specific volume and high strength.
Note: the test method of each foil performance parameter is carried out according to SJ/T11140-1997 standard.
According to the data, the three-dimensional porous aluminum electrode foil provided by the invention has the properties of high specific volume, high strength and the like, and the composite porous aluminum film on the aluminum foil substrate has the characteristics of no cracking, no falling, good binding force and the like in the production process. In the invention, the bending strength and specific volume of the finally prepared three-dimensional porous aluminum electrode foil are greatly improved by using hydrogen peroxide for hydration treatment in a formation energizing stage. Meanwhile, the high dielectric oxide added in the invention has the functions of bonding and supporting, can prevent the aluminum powder from seriously deforming due to the increase of the reduction amount, and simultaneously ensures the porosity.
Claims (6)
1. The preparation method of the three-dimensional porous aluminum electrode foil is characterized by comprising the following steps of:
(1) uniformly mixing aluminum-containing powder, aluminum fibers and high-dielectric oxide powder to obtain mixed powder;
(2) uniformly dispersing the mixed powder on two sides of an aluminum foil substrate, and compacting to form a close-packed porous foil;
(3) Carrying out thermalization treatment on the densely-packed porous foil, and controlling the porosity to be 35-45% and the thickness to be 80-200 μm through extrusion treatment to finally form a composite mesh-shaped porous aluminum electrode foil;
(4) Carrying out formation energizing treatment on the porous aluminum electrode foil subjected to the thermalization treatment; a reducing electrolyte is added in the hydration process of the formation energizing treatment; the reducing electrolyte is hydrogen peroxide, and the content of the reducing electrolyte is 0.05wt% -0.10 wt%; in the mixed powder, the aluminum-containing powder accounts for 95-99 percent, the aluminum fiber accounts for 0.5-5 percent and the high dielectric oxide powder accounts for 0.05-2 percent by weight percent; the aluminum-containing powder is selected from at least one of aluminum or aluminum alloy powder, and the high-dielectric oxide powder is selected from Al2O3、TiO2And barium titanate; the particle size of the aluminum-containing powder is 1-20 mu m; the diameter of the aluminum fiber is 3-10 μm, and the length of the aluminum fiber is 1-500 μm; the high dielectric oxidation powder has a purity of not less than 99.9% and a particle size of 0.2-5 μm.
2. The production method according to claim 1, wherein the compacting is performed by rolling with cold roller and controlling the pressure to 50-300 Kg; the extrusion treatment is carried out by cold rolling under the conditions of the temperature of 300 ℃ and the pressure of 15-20 Kg.
3. The method according to claim 1, wherein the uniformly dispersing the mixed powder on both sides of the aluminum substrate means controlling the surface roughness not to exceed ± 8 μm; the thermalization treatment is carried out under the conditions of vacuum or inert gas; the temperature of the thermalization treatment is 550-670 ℃, and the treatment time is 1-30 min; the inert gas is selected from Ar2。
4. The three-dimensional porous aluminum electrode foil obtained by the preparation method of any one of claims 1 to 3, which comprises an aluminum foil substrate and a composite porous aluminum film formed by mixed powder on two surfaces of the aluminum foil substrate, and is characterized in that the total thickness of the three-dimensional porous aluminum electrode foil is 80-200 μm; the voltage of the three-dimensional porous aluminum electrode foil is 300-600V, the bending times are 50-340 times, and the specific volume is 0.70-2.55 mu F/cm2(ii) a The thickness of the aluminum foil substrate is 20-100 mu m, and the purity is not lower than 99.92%; the thickness of the single layer of the composite porous aluminum film is 20-100 mu m; the three-dimensional porous aluminum electrode foil is prepared by metal powder rolling, and the porosity of the three-dimensional porous aluminum electrode foil is 35% -45%.
5. The three-dimensional porous aluminum electrode foil of claim 4, wherein the mixture isIn the composite powder, the aluminum-containing powder accounts for 95 to 99 percent, the aluminum fiber accounts for 0.5 to 5 percent and the high dielectric oxide powder accounts for 0.05 to 2 percent by weight; the aluminum-containing powder is selected from at least one of aluminum or aluminum alloy powder, and the high-dielectric oxide powder is selected from Al2O3、TiO2And barium titanate.
6. The three-dimensional porous aluminum electrode foil according to claim 5, wherein the aluminum-containing powder has a particle size of 1 to 20 μm; the diameter of the aluminum fiber is 3-10 μm, and the length of the aluminum fiber is 1-500 μm; the high dielectric oxidation powder has a purity of not less than 99.9% and a particle size of 0.2-5 μm.
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| CN111627714B (en) * | 2020-05-28 | 2021-08-13 | 西安交通大学 | Preparation method of porous anode aluminum foil with multi-stage mixed structure |
| CN114523112B (en) * | 2021-12-30 | 2024-03-22 | 浙江洪量新材科技有限公司 | Porous electrode foil and preparation process thereof |
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