CN107142485A - A kind of method of mesohigh anode high-purity aluminum foil surface generalization modification - Google Patents
A kind of method of mesohigh anode high-purity aluminum foil surface generalization modification Download PDFInfo
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- CN107142485A CN107142485A CN201710350396.6A CN201710350396A CN107142485A CN 107142485 A CN107142485 A CN 107142485A CN 201710350396 A CN201710350396 A CN 201710350396A CN 107142485 A CN107142485 A CN 107142485A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/22—Light metals
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/16—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions using inhibitors
- C23G1/18—Organic inhibitors
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/30—Electroplating: Baths therefor from solutions of tin
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/06—Wires; Strips; Foils
- C25D7/0614—Strips or foils
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F1/00—Electrolytic cleaning, degreasing, pickling or descaling
- C25F1/02—Pickling; Descaling
- C25F1/04—Pickling; Descaling in solution
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G13/00—Apparatus specially adapted for manufacturing capacitors; Processes specially adapted for manufacturing capacitors not provided for in groups H01G4/00 - H01G11/00
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—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
Abstract
The invention discloses a kind of method of mesohigh anode high-purity aluminum foil surface generalization modification, it is related to the manufacture field of aluminium electrolutic capacitor mesohigh anode high-purity aluminum foil and etched foil.Aim to provide a kind of uniformity that can improve the tunnel pore size distribution of aluminium foil corrosion hair engaging aperture, reduce the self-corrosion thinning of aluminium foil, thus can further improve the specific capacitance of aluminium foil and the method for warping resistance performance.The technical scheme that the present invention is provided comprises the steps：Step 1：High-purity aluminum foil is pre-processed in alkaline solution；Step 2：Aluminium foil by pretreatment is handled using the step current method of anode+negative electrode one；Step 3：High-temperature oxydation.
Description
Technical field
The invention belongs to manufacture field of the aluminium electrolutic capacitor with mesohigh anode high-purity aluminum foil and etched foil, especially one
The method for planting the high-purity aluminum foil surface generalization modification of mesohigh anode.
Background technology
With the continuous diminution and the development of High Density Packaging of complete electronic set volume, it is desirable to based in component
High-pressure aluminum electrolytic capacitor has the characteristics of high power capacity and miniaturization, to meet the development need of electronic product.
Current medium-high voltage aluminum electrolytic capacitor is with the general method by electrochemical corrosion of anode aluminium foil in anode aluminium foil table
Face generates substantial amounts of Tunnel-hole to expand its surface area, that is, improves the specific capacitance of capacitor, with realize capacitor high power capacity and
Minimize purpose.In order to ensure that mesohigh anode electrode paper tinsel has required winding performance, the electrode foil after corrosion must also
With certain tensile strength and buckling performance, it is therefore desirable to keep certain thickness in the middle of corrosive aluminum foil and be not corroded
Aluminum layer.In addition in order that the aluminium foil combination property after corrosion is optimized, it is necessary to improve aluminium foil surface erosion in corrosion process
The uniformity of pore size distribution, avoid as far as possible and the generation in hole and the self-corrosion phenomenon of aluminium foil surface is reduced during hair engaging aperture.
The technique that mesohigh anode high-purity aluminum foil corrodes mainly includes：Before corrosion at pretreatment, hair engaging aperture processing and reaming
Reason.During aluminium foil hair engaging aperture, the form and distribution mode in hole are mainly determined by the surface state of aluminium foil, and the surface state of aluminium foil is main
Determined by corrosion fore-pretreatment method.Aluminium foil surface pretreatment mainly includes heat treatment, acid, alkali process, cathodic polarization processing, oxygen
Change processing and deposition inert metal processing etc..At present, the electrical property of mesohigh corrosive aluminum foil is improved both at home and abroad mainly by
The trace elements such as ppm grades Pb, Sn, In are added in high-pressure aluminium foil, these trace elements are made in aluminium by annealing heat treatment process
Paper tinsel surface is enriched with, and the trace element being enriched with the subsequent hair engaging aperture of aluminium foil will constitute the substantial amounts of micro- electricity of corrosion with aluminum substrate
Pond, so as to improve the uniformity of aluminium foil corrosion hair engaging aperture.Improved although the result of the approach is the Tunnel-hole uniformity of generation,
Simultaneously because the surface density of corrosion micro cell is too high, the corrosion thinning and Tunnel-hole of aluminium foil simultaneously also seriously increase in hole, and the former makes corruption
The specific capacitance of erosion aluminium foil is improved, and the latter will limit the further raising of specific capacitance and reduce the mechanicalness of corrosive aluminum foil
Energy.
It is heavy in mesohigh electric aluminum foil surface electricity that China Patent Publication No. discloses for 103774193A and 103361692A
Product zinc, the method for tin nucleus, to guide the corrosion hair engaging aperture of aluminium foil, with the effect for improving aluminium foil specific capacitance.But we send out simultaneously
Tin, the zinc nucleus deposited in existing above-mentioned patent lacks persistence when inducing aluminium foil hair engaging aperture, and analysis reason is heavy using two-step method
When product tin, zinc nucleus, because aluminium foil surface still has very thin oxidizing aqueous film, cause tin, zinc nucleus in oxidizing aqueous film
On be deposited, so as to reduce the adhesion of nucleus and foil substrate.In aluminium foil corrosion hair engaging aperture because most tin, zinc are brilliant
Core is not directly to be deposited on aluminum substrate, and nucleus is easily separated from matrix and produces dust, and reduction persistently guides the energy of aluminium foil hair engaging aperture
Power, causes aluminium foil hair engaging aperture uniformity to decline, so as to limit the further raising of aluminium foil specific capacitance.China Patent Publication No. is
103451713A discloses the corrosion pretreating method that zinc or tin nucleus are deposited in the anodic oxidation of mesohigh electric aluminum foil, this method
It is still that zinc or tin nucleus, corrosion resistance and densification due to anode oxide film are deposited on the anode oxide film not being completely dissolved
Property so that the adhesion of zinc or tin nucleus and foil substrate is lower, so as to limit the raising of specific capacitance.In addition, Chinese patent is public
The number of opening is that 104357886A and CN104733181A is disclosed in mesohigh anode high-purity aluminum foil surface chemistry and sprayed deposit
The method of disperse tin, zinc nucleus, this method is direct on aluminum substrate again after can first the moisture film of aluminium foil surface be partly dissolved
Tin, zinc nucleus are deposited, the adhesion of nucleus and matrix can be significantly improved.But because chemolysis aluminium foil surface is aqueous
Film can not uniformly, sufficiently dissolve redeposited nucleus, but while dissolving moisture film deposits nucleus simultaneously, cause portion
Nucleus is divided to be deposited directly in foil substrate, and other nucleus will be deposited in moisture film so that nucleus guides aluminium foil
Uniform hair engaging aperture is not optimal, the further raising of final limitation specific capacitance.
The content of the invention
The present invention is intended to provide a kind of method of mesohigh anode high-purity aluminum foil surface generalization modification, this method energy
Enough improve the uniformity of aluminium foil corrosion hair engaging aperture tunnel pore size distribution, reduce the self-corrosion thinning of aluminium foil, thus can further improve
The specific capacitance and warping resistance performance of aluminium foil.
In order to realize above-mentioned technique effect, the technical scheme that the present invention is provided is such：A kind of mesohigh anode is high
The method of pure aluminum foil surface generalization modification, comprises the steps：
Step 1：High-purity aluminum foil is pre-processed in alkaline solution；
Step 2：Aluminium foil by pretreatment is handled using the step current method of anode+negative electrode one；
Step 3：High-temperature oxydation.
Preferably, the alkaline solution described in step 1 refers to：0.1~2mol/L Na2CO3+ 0.1~1.5mol/L Na3PO4
+ 0.5~3mol/L NaOH+0.1~0.5mol/L corrosion inhibiter.Preferably, the treatment temperature of described step 1 is 60~95 DEG C,
Processing time is 5~60s.
Preferably, described corrosion inhibiter is the one or more in thiocarbamide, gelatin, BTA, sodium gluconate.
Preferably, described step 2 is specially：Aluminium foil by pretreatment is used into the step of anode+negative electrode one in the solution
Current method is handled；
Wherein, described solution refers to：0.1~1mol/L+0.2~1mol/L of sodium stannate sodium hydroxides+0.01~
0.05mol/L sodium potassium tartrate tetrahydrate+0.1~5ml/L kayexalates.
Preferably, the treatment temperature of described step 2 is 30~60 DEG C.
Preferably, described anodic current density scope is 5~50mA/cm2, cathode-current density scope be 10~
40mA/cm2。
Preferably, described anodic treatment times are 10~60s, and the cathode treatment time is 10~60s.
Preferably, the oxidizing temperature of the high-temperature oxydation described in step 3 is 100~400 DEG C, and oxidization time is 10~100 seconds.
Preferably, described high-purity aluminum foil refers to：{ 100 } plane texture will be formed after finished product recrystallization annealing processing
Occupation rate is more than 95%, and surface is containing micro Fe, Si, Cu, Zn, Ga, Mn element and is not enriched with Pb elements, and Al purity is
99.99% mesohigh anode high-purity aluminum foil.
The present invention is compared with conventional method, with advantages below：
1st, the purpose that high-purity aluminum foil is pre-processed in the alkaline solution containing corrosion inhibiter is to remove aluminium foil surface warp
Cross the dense oxidation film formed after finished product recrystallization annealing and form new moisture film.
2. the moisture film that can uniformly remove aluminium foil surface completely is handled using the step current method of anode+negative electrode one and direct
Tin nucleus is deposited in foil substrate, it is to avoid tin nucleus is deposited in the moisture film of aluminium foil surface, improves tin nucleus and aluminium
The adhesion of paper tinsel matrix, enhances the ability that tin nucleus persistently guides aluminium foil corrosion hair engaging aperture.
More specifically, above-mentioned anode processing intent is to remove aluminium foil surface moisture film；Cathode treatment purpose is
The Sn nucleus of even dispersion distribution is directly deposited in foil substrate.
3. the aluminium foil high-temperature oxydation that will be handled by the step current method of anode+negative electrode one, obtains Al2O3/SnO2Complex oxide film
With Al-Sn counterdiffusion microcells, SnO2Particle does not dissolve in acid solution as semiconductor, is conducive to anode current to concentrate on SnO2Particle
On, make topical solutions acidity raising, cause SnO2Al near particle2O3Film dissolves, so as to induce aluminium foil uniformly to corrode hair
Hole.In addition, Al2O3/SnO2The effect of complex oxide film and Al-Sn counterdiffusion microcell induced corrosion hair engaging aperture will be than tin nucleus more
Persistently, so as to further improve the ability of guiding aluminium foil corrosion hair engaging aperture.
4. the thickness that micro corrosion inhibiter is added in alkaline pre-treatment solution when aluminium foil pretreatment can be greatly reduced subtracts
It is thin and result in more even curface state.
Brief description of the drawings
Fig. 1 is the Sn nucleus schematic diagrames that aluminium foil surface deposits Dispersed precipitate；
Fig. 2 is the transformation schematic diagram of surface recombination structure when aluminium foil surface passes through short time high temperature oxidation processes；
Fig. 3 is the transformation schematic diagram of surface recombination structure when aluminium foil surface passes through long-time high-temperature oxydation；
Fig. 4 is the scanning electron microscope (SEM) photograph of the aluminium foil surface after comprehensively modifying is handled.
Embodiment
With reference to embodiment, the claim to the present invention is described in further detail, but is not constituted pair
Any limitation of the present invention, any limited number of time modification made in the claims in the present invention protection domain, still the present invention's
In claims.
Embodiment 1
It is 99.99% by Al purity, thickness is 110 μm, and the process homogenization that { 100 } plane texture occupation rate is more than 95% is moved back
Surface is containing micro Fe, Si, Cu, Zn, Ga, Mn element after fire and is not enriched with Pb elements these electrode potentials mesohigh higher than aluminium
Anode high-purity aluminum foil is 80 DEG C in temperature, contains the phosphate dihydrate sodium+2mol/L hydroxides of 1mol/L sodium carbonate+0.5mol/L ten
Pre-processed in sodium+0.2mol/L thiourea solutions, pretreatment time is 10 seconds, to remove aluminium foil surface densification after annealing
Oxide-film and new moisture film is formed in aluminium foil surface.It it is 30 DEG C in temperature, solution is by the aluminium foil containing moisture film
In 0.5mol/L sodium stannate+0.4mol/L sodium hydroxide+0.03mol/L sodium potassium tartrate tetrahydrates handle, use anodic current density for
10mA/cm2, processing time is to use within 30 seconds cathode-current density immediately to remove aluminium foil surface moisture film, afterwards for 10mA/
cm2, processing time is Sn nucleus to be deposited in foil substrate in 20 seconds.
By above-mentioned preparation Al2O3/SnO2The aluminium foil of complex oxide film and Al-Sn counterdiffusion microcells carries out hair engaging aperture corrosion, hair engaging aperture
Solution is 0.8mol/L hydrochloric acid+3.6mol/L sulfuric acid+0.8mol/L mixed solution, and temperature is 75 DEG C；Reaming corrosion is carried out again,
Reaming solution is 0.07mol/L salpeter solution, and temperature is 70 DEG C；Post-process as salpeter solution, clean, drying, finally according to
Professional standard carries out 520V chemical conversions.
Surface is answered when the Sn nucleus and progress high temperature oxidation process of the present embodiment pretreatment aluminium foil surface deposition Dispersed precipitate
The schematic diagram for closing the transformation of structure refers to Fig. 1-Fig. 3：Wherein, Fig. 1 is to be gone out using one-step method processing in foil substrate Direct precipitation
The schematic diagram of the Sn nucleus of even dispersion distribution；Fig. 2 is the Sn nucleus superficial oxidation generation SnO after short time high temperature is aoxidized2
Film, while counterdiffusion will occur with aluminium foil for the Sn nucleus contacted with aluminum substrate, forms Al-Sn counterdiffusion microcells, the other tables of aluminium foil
Face oxidation generation Al2O3The schematic diagram of oxide-film；Fig. 3 is to pass through long period high-temperature oxydation, and Sn nucleus disappears, and forms SnO2Film
With Al-Sn counterdiffusion microcells, the other surfaces of aluminium foil form thicker Al2O3The schematic diagram of oxide-film；In addition, the present invention is to carrying out
The aluminium foil that surface has carried out comprehensively modifying processing has done ESEM shape appearance figure, refers to Fig. 4.
Embodiment 2
It is 99.99% by Al purity, thickness is 110 μm, and the process homogenization that { 100 } plane texture occupation rate is more than 95% is moved back
Surface is containing micro Fe, Si, Cu, Zn, Ga, Mn element after fire and is not enriched with Pb elements these electrode potentials mesohigh higher than aluminium
Anode high-purity aluminum foil is 80 DEG C in temperature, contains the phosphate dihydrate sodium+2mol/L hydroxides of 1mol/L sodium carbonate+0.5mol/L ten
Pre-processed in sodium+0.2mol/L thiourea solutions, pretreatment time is 10 seconds, to remove aluminium foil surface densification after annealing
Oxide-film and new moisture film is formed in aluminium foil surface.It it is 30 DEG C in temperature, solution is by the aluminium foil containing moisture film
Handled in 0.5mol/L sodium stannate+0.4mol/L sodium hydroxide+0.03mol/L sodium potassium tartrate tetrahydrate+0.2mol/L thiocarbamides, using sun
Electrode current density is 30mA/cm2, processing time be 30 seconds to remove aluminium foil surface moisture film, afterwards immediately use cathode current
Density is 10mA/cm2, processing time is Sn nucleus to be deposited in foil substrate in 20 seconds.
By above-mentioned preparation Al2O3/SnO2The aluminium foil of complex oxide film and Al-Sn counterdiffusion microcells carries out hair engaging aperture corrosion, hair engaging aperture
Solution is 0.8mol/L hydrochloric acid+3.6mol/L sulfuric acid+0.8mol/L mixed solution, and temperature is 75 DEG C；Reaming corrosion is carried out again,
Reaming solution is 0.07mol/L salpeter solution, and temperature is 70 DEG C；Post-process as salpeter solution, clean, drying, finally according to
Professional standard carries out 520V chemical conversions.
Embodiment 3
It is 99.99% by Al purity, thickness is 110 μm, and the process homogenization that { 100 } plane texture occupation rate is more than 95% is moved back
Surface is containing micro Fe, Si, Cu, Zn, Ga, Mn element after fire and is not enriched with Pb elements these electrode potentials mesohigh higher than aluminium
Anode high-purity aluminum foil is 80 DEG C in temperature, contains the phosphate dihydrate sodium+2mol/L hydroxides of 1mol/L sodium carbonate+0.5mol/L ten
Pre-processed in sodium+0.2mol/L thiourea solutions, pretreatment time is 10 seconds, to remove aluminium foil surface densification after annealing
Oxide-film and new moisture film is formed in aluminium foil surface.It it is 30 DEG C in temperature, solution is by the aluminium foil containing moisture film
In 0.5mol/L sodium stannate+0.4mol/L sodium hydroxide+0.03mol/L sodium potassium tartrate tetrahydrates handle, use anodic current density for
30mA/cm2, processing time is to use within 30 seconds cathode-current density immediately to remove aluminium foil surface moisture film, afterwards for 30mA/
cm2, processing time is Sn nucleus to be deposited in foil substrate in 20 seconds.
By above-mentioned preparation Al2O3/SnO2The aluminium foil of complex oxide film and Al-Sn counterdiffusion microcells carries out hair engaging aperture corrosion, hair engaging aperture
Solution is 0.8mol/L hydrochloric acid+3.6mol/L sulfuric acid+0.8mol/L mixed solution, and temperature is 75 DEG C；Reaming corrosion is carried out again,
Reaming solution is 0.07mol/L salpeter solution, and temperature is 70 DEG C；Post-process as salpeter solution, clean, drying, finally according to
Professional standard carries out 520V chemical conversions.
Embodiment 4：
It is 99.99% by Al purity, thickness is 110 μm, and the process homogenization that { 100 } plane texture occupation rate is more than 95% is moved back
Surface is containing micro Fe, Si, Cu, Zn, Ga, Mn element after fire and is not enriched with Pb elements these electrode potentials mesohigh higher than aluminium
Anode high-purity aluminum foil is 80 DEG C in temperature, contains the phosphate dihydrate sodium+2mol/L hydroxides of 1mol/L sodium carbonate+0.5mol/L ten
Pre-processed in sodium+0.2mol/L thiourea solutions, pretreatment time is 10 seconds, to remove aluminium foil surface densification after annealing
Oxide-film and new moisture film is formed in aluminium foil surface.It it is 30 DEG C in temperature, solution is by the aluminium foil containing moisture film
In 0.5mol/L sodium stannate+0.4mol/L sodium hydroxide+0.03mol/L sodium potassium tartrate tetrahydrates handle, use anodic current density for
10mA/cm2, processing time is to use within 30 seconds cathode-current density immediately to remove aluminium foil surface moisture film, afterwards for 10mA/
cm2, processing time is Sn nucleus to be deposited in foil substrate in 20 seconds.Finally by the aluminium foil handled by one-step method at 300 DEG C
High-temperature oxydation, oxidization time is 30 seconds, and uniform Al is prepared in foil substrate2O3/SnO2Complex oxide film and Al-Sn are mutual
Spread microcell.
By above-mentioned preparation Al2O3/SnO2The aluminium foil of complex oxide film and Al-Sn counterdiffusion microcells carries out hair engaging aperture corrosion, hair engaging aperture
Solution is 0.8mol/L hydrochloric acid+3.6mol/L sulfuric acid+0.8mol/L mixed solution, and temperature is 75 DEG C；Reaming corrosion is carried out again,
Reaming solution is 0.07mol/L salpeter solution, and temperature is 70 DEG C；Post-process as salpeter solution, clean, drying, finally according to
Professional standard carries out 520V chemical conversions.
Embodiment 5
It is 99.99% by Al purity, thickness is 110 μm, and the process homogenization that { 100 } plane texture occupation rate is more than 95% is moved back
Surface is containing micro Fe, Si, Cu, Zn, Ga, Mn element after fire and is not enriched with Pb elements these electrode potentials mesohigh higher than aluminium
Anode high-purity aluminum foil is 80 DEG C in temperature, contains the phosphate dihydrate sodium+2mol/L hydroxides of 1mol/L sodium carbonate+0.5mol/L ten
Pre-processed in sodium+0.2mol/L sodium gluconate solutions, pretreatment time is 10 seconds, to remove aluminium foil surface by annealing
Fine and close oxide-film and new moisture film is formed in aluminium foil surface afterwards.It is 30 DEG C, solution in temperature by the aluminium foil containing moisture film
To be handled in 0.5mol/L sodium stannate+0.4mol/L sodium hydroxide+0.03mol/L sodium potassium tartrate tetrahydrates, using anodic current density
For 10mA/cm2, processing time is to use within 30 seconds cathode-current density immediately to remove aluminium foil surface moisture film, afterwards for 10mA/
cm2, processing time is Sn nucleus to be deposited in foil substrate in 20 seconds.Finally by the aluminium foil handled by one-step method at 400 DEG C
High-temperature oxydation, oxidization time is 30 seconds, and uniform Al is prepared in foil substrate2O3/SnO2Complex oxide film and Al-Sn are mutual
Spread microcell.
By above-mentioned preparation Al2O3/SnO2The aluminium foil of complex oxide film and Al-Sn counterdiffusion microcells carries out hair engaging aperture corrosion, hair engaging aperture
Solution is 0.8mol/L hydrochloric acid+3.6mol/L sulfuric acid+0.8mol/L mixed solution, and temperature is 75 DEG C；Reaming corrosion is carried out again,
Reaming solution is 0.07mol/L salpeter solution, and temperature is 70 DEG C；Post-process as salpeter solution, clean, drying, finally according to
Professional standard carries out 520V chemical conversions.
Embodiment 6：
It is 99.99% by Al purity, thickness is 110 μm, and the process homogenization that { 100 } plane texture occupation rate is more than 95% is moved back
Surface is containing micro Fe, Si, Cu, Zn, Ga, Mn element after fire and is not enriched with Pb elements these electrode potentials mesohigh higher than aluminium
Anode high-purity aluminum foil is 80 DEG C in temperature, contains the phosphate dihydrate sodium+2mol/L hydroxides of 1mol/L sodium carbonate+0.5mol/L ten
Pre-processed in sodium+0.2mol/L sodium gluconate solutions, pretreatment time is 10 seconds, to remove aluminium foil surface by annealing
Fine and close oxide-film and new moisture film is formed in aluminium foil surface afterwards.It is 30 DEG C, solution in temperature by the aluminium foil containing moisture film
To be handled in 0.5mol/L sodium stannate+0.4mol/L sodium hydroxide+0.03mol/L sodium potassium tartrate tetrahydrate+2ml/L PSSA, using sun
Electrode current density is 10mA/cm2, processing time be 30 seconds to remove aluminium foil surface moisture film, afterwards immediately use cathode current
Density is 10mA/cm2, processing time is Sn nucleus to be deposited in foil substrate in 10 seconds.Finally by by one-step method processing
Aluminium foil is 30 seconds in 400 DEG C of high-temperature oxydations, oxidization time, and uniform Al is prepared in foil substrate2O3/SnO2Combined oxidation
Film and Al-Sn counterdiffusion microcells.
By above-mentioned preparation Al2O3/SnO2The aluminium foil of complex oxide film and Al-Sn counterdiffusion microcells carries out hair engaging aperture corrosion, hair engaging aperture
Solution is 0.8mol/L hydrochloric acid+3.6mol/L sulfuric acid+0.8mol/L mixed solution, and temperature is 75 DEG C；Reaming corrosion is carried out again,
Reaming solution is 0.07mol/L salpeter solution, and temperature is 70 DEG C；Post-process as salpeter solution, clean, drying, finally according to
Professional standard carries out 520V chemical conversions.
Embodiment 7
It is 99.99% by Al purity, thickness is 110 μm, and the process homogenization that { 100 } plane texture occupation rate is more than 95% is moved back
Surface is containing micro Fe, Si, Cu, Zn, Ga, Mn element after fire and is not enriched with Pb elements these electrode potentials mesohigh higher than aluminium
Anode high-purity aluminum foil is 80 DEG C in temperature, contains the phosphate dihydrate sodium+2mol/L hydroxides of 1mol/L sodium carbonate+0.5mol/L ten
Pre-processed in sodium+0.2mol/L sodium gluconate solutions, pretreatment time is 10 seconds, to remove aluminium foil surface by annealing
Fine and close oxide-film and new moisture film is formed in aluminium foil surface afterwards.It is 30 DEG C, solution in temperature by the aluminium foil containing moisture film
To be handled in 0.5mol/L sodium stannate+0.4mol/L sodium hydroxide+0.03mol/L sodium potassium tartrate tetrahydrate+2ml/L PSSA, using sun
Electrode current density is 10mA/cm2, processing time be 30 seconds to remove aluminium foil surface moisture film, afterwards immediately use cathode current
Density is 10mA/cm2, processing time is Sn nucleus to be deposited in foil substrate in 10 seconds.Finally by by one-step method processing
Aluminium foil is 60 seconds in 400 DEG C or so high-temperature oxydations, oxidization time, and uniform Al is prepared in foil substrate2O3/SnO2It is compound
Oxide-film and Al-Sn counterdiffusion microcells.
By above-mentioned preparation Al2O3/SnO2The aluminium foil of complex oxide film and Al-Sn counterdiffusion microcells carries out hair engaging aperture corrosion, hair engaging aperture
Solution is 0.8mol/L hydrochloric acid+3.6mol/L sulfuric acid+0.8mol/L mixed solution, and temperature is 75 DEG C；Reaming corrosion is carried out again,
Reaming solution is 0.07mol/L salpeter solution, and temperature is 70 DEG C；Post-process as salpeter solution, clean, drying, finally according to
Professional standard carries out 520V chemical conversions.
Embodiment 8：
It is 99.99% by Al purity, thickness is 110 μm, and the process homogenization that { 100 } plane texture occupation rate is more than 95% is moved back
Surface is containing micro Fe, Si, Cu, Zn, Ga, Mn element after fire and is not enriched with Pb elements these electrode potentials mesohigh higher than aluminium
Anode high-purity aluminum foil is 80 DEG C in temperature, contains the phosphate dihydrate sodium+2mol/L hydroxides of 1mol/L sodium carbonate+0.5mol/L ten
Pre-processed in sodium+0.2mol/L sodium gluconate solutions, pretreatment time is 10 seconds, to remove aluminium foil surface by annealing
Fine and close oxide-film and new moisture film is formed in aluminium foil surface afterwards.It is 30 DEG C, solution in temperature by the aluminium foil containing moisture film
To be handled in 1mol/L sodium stannate+0.8mol/L sodium hydroxide+0.05mol/L sodium potassium tartrate tetrahydrate+5ml/L PSSA, using anode
Current density is 10mA/cm2, processing time be 30 seconds to remove aluminium foil surface moisture film, afterwards immediately using cathode current it is close
Spend for 10mA/cm2, processing time is Sn nucleus to be deposited in foil substrate in 10 seconds.The aluminium that will finally be handled by one-step method
Paper tinsel is 30 seconds in 300 DEG C or so high-temperature oxydations, oxidization time, and uniform Al is prepared in foil substrate2O3/SnO2Composite oxygen
Change film and Al-Sn counterdiffusion microcells.
By above-mentioned preparation Al2O3/SnO2The aluminium foil of complex oxide film and Al-Sn counterdiffusion microcells carries out hair engaging aperture corrosion, hair engaging aperture
Solution is 0.8mol/L hydrochloric acid+3.6mol/L sulfuric acid+0.8mol/L mixed solution, and temperature is 75 DEG C；Reaming corrosion is carried out again,
Reaming solution is 0.07mol/L salpeter solution, and temperature is 70 DEG C；Post-process as salpeter solution, clean, drying, finally according to
Professional standard carries out 520V chemical conversions.
Embodiment 9：
It is 99.99% by Al purity, thickness is 110 μm, and the process homogenization that { 100 } plane texture occupation rate is more than 95% is moved back
Surface is containing micro Fe, Si, Cu, Zn, Ga, Mn element after fire and is not enriched with Pb elements these electrode potentials mesohigh higher than aluminium
Anode high-purity aluminum foil is 80 DEG C in temperature, contains the phosphate dihydrate sodium+2mol/L hydroxides of 1mol/L sodium carbonate+0.5mol/L ten
Pre-processed in sodium+0.2mol/L sodium gluconate solutions, pretreatment time is 30 seconds, to remove aluminium foil surface by annealing
Fine and close oxide-film and new moisture film is formed in aluminium foil surface afterwards.It is 30 DEG C, solution in temperature by the aluminium foil containing moisture film
To be handled in 1mol/L sodium stannate+0.8mol/L sodium hydroxide+0.05mol/L sodium potassium tartrate tetrahydrate+5ml/L PSSA, using anode
Current density is 10mA/cm2, processing time be 30 seconds to remove aluminium foil surface moisture film, afterwards immediately using cathode current it is close
Spend for 10mA/cm2, processing time is Sn nucleus to be deposited in foil substrate in 10 seconds.
By above-mentioned preparation Al2O3/SnO2The aluminium foil of complex oxide film and Al-Sn counterdiffusion microcells carries out hair engaging aperture corrosion, hair engaging aperture
Solution is 0.8mol/L hydrochloric acid+3.6mol/L sulfuric acid+0.8mol/L mixed solution, and temperature is 75 DEG C；Reaming corrosion is carried out again,
Reaming solution is 0.07mol/L salpeter solution, and temperature is 70 DEG C；Post-process as salpeter solution, clean, drying, finally according to
Professional standard carries out 520V chemical conversions.
Embodiment 10：
It is 99.99% by Al purity, thickness is 110 μm, and the process homogenization that { 100 } plane texture occupation rate is more than 95% is moved back
Surface is containing micro Fe, Si, Cu, Zn, Ga, Mn element after fire and is not enriched with Pb elements these electrode potentials mesohigh higher than aluminium
Anode high-purity aluminum foil is 80 DEG C in temperature, contains the phosphate dihydrate sodium+2mol/L hydroxides of 1mol/L sodium carbonate+0.5mol/L ten
Pre-processed in sodium+0.2mol/L sodium gluconate solutions, pretreatment time is 30 seconds, to remove aluminium foil surface by annealing
Fine and close oxide-film and new moisture film is formed in aluminium foil surface afterwards.It is 30 DEG C, solution in temperature by the aluminium foil containing moisture film
To be handled in 1mol/L sodium stannate+0.8mol/L sodium hydroxide+0.05mol/L sodium potassium tartrate tetrahydrate+5ml/L PSSA, using anode
Current density is 10mA/cm2, processing time be 30 seconds to remove aluminium foil surface moisture film, afterwards immediately using cathode current it is close
Spend for 10mA/cm2, processing time is Sn nucleus to be deposited in foil substrate in 10 seconds.The aluminium that will finally be handled by one-step method
Paper tinsel is 30 seconds in 300 DEG C or so high-temperature oxydations, oxidization time, and uniform Al is prepared in foil substrate2O3/SnO2Composite oxygen
Change film and Al-Sn counterdiffusion microcells.
By above-mentioned preparation Al2O3/SnO2The aluminium foil of complex oxide film and Al-Sn counterdiffusion microcells carries out hair engaging aperture corrosion, hair engaging aperture
Solution is 0.8mol/L hydrochloric acid+3.6mol/L sulfuric acid+0.8mol/L mixed solution, and temperature is 75 DEG C；Reaming corrosion is carried out again,
Reaming solution is 0.07mol/L salpeter solution, and temperature is 70 DEG C；Post-process as salpeter solution, clean, drying, finally according to
Professional standard carries out 520V chemical conversions.
Embodiment 11：
It is 99.99% by Al purity, thickness is 110 μm, and the process homogenization that { 100 } plane texture occupation rate is more than 95% is moved back
Surface is containing micro Fe, Si, Cu, Zn, Ga, Mn element after fire and is not enriched with Pb elements these electrode potentials mesohigh higher than aluminium
Anode high-purity aluminum foil is 80 DEG C in temperature, contains the phosphate dihydrate sodium+2mol/L hydroxides of 1mol/L sodium carbonate+0.5mol/L ten
Pre-processed in sodium+0.2mol/L sodium gluconate solutions, pretreatment time is 60 seconds, to remove aluminium foil surface by annealing
Fine and close oxide-film and new moisture film is formed in aluminium foil surface afterwards.It is 30 DEG C, solution in temperature by the aluminium foil containing moisture film
To be handled in 1mol/L sodium stannate+0.8mol/L sodium hydroxide+0.05mol/L sodium potassium tartrate tetrahydrate+5ml/L PSSA, using electric current
Density is 50mA/cm2, processing time is to use within 30 seconds current density immediately to remove aluminium foil surface moisture film, afterwards for 40mA/
cm2, processing time is Sn nucleus to be deposited in foil substrate in 10 seconds.Finally by the aluminium foil handled by one-step method at 300 DEG C
Left and right high-temperature oxydation, oxidization time is 30 seconds, and uniform Al is prepared in foil substrate2O3/SnO2Complex oxide film and Al-
Sn counterdiffusion microcells.
By above-mentioned preparation Al2O3/SnO2The aluminium foil of complex oxide film and Al-Sn counterdiffusion microcells carries out hair engaging aperture corrosion, hair engaging aperture
Solution is 0.8mol/L hydrochloric acid+3.6mol/L sulfuric acid+0.8mol/L mixed solution, and temperature is 75 DEG C；Reaming corrosion is carried out again,
Reaming solution is 0.07mol/L salpeter solution, and temperature is 70 DEG C；Post-process as salpeter solution, clean, drying, finally according to
Professional standard carries out 520V chemical conversions.
Comparative example 1
Al purity is 99.99%, and thickness is 120 μm, and { 100 } plane texture occupation rate is more than 95% surface enrichment micro lead
The high-purity aluminum foil of element, using traditional mixed acid pretreating process, pretreatment fluid used is 1mol/L hydrochloric acid+3mol/L sulphur
Acid, temperature is 80 DEG C, and aluminium foil is directly soaked 120 seconds in pretreatment fluid, carries out hair engaging aperture corrosion, and hair engaging aperture solution is 0.8mol/L
Hydrochloric acid+3.6mol/L sulfuric acid+0.8mol/L mixed solution, temperature is 75 DEG C；Reaming corrosion is carried out again, and reaming solution is
0.07mol/L salpeter solution, temperature is 70 DEG C；Post-process as salpeter solution, clean, drying is entered finally according to professional standard
Row 520V is melted into.
Table 1 is using the present invention to prepare Al in comparative example 1 and embodiment 1-112O3/SnO2The aluminium foil of complex oxide film is carried out
Hair engaging aperture is corroded, after anode etching and chemical conversion, corrosion thinning amount, specific capacitance and the bending times of aluminium foil, it can be seen that adopt
Al is prepared with the present invention2O3/SnO2The aluminium foil of complex oxide film and Al-Sn counterdiffusion microcells, corrosion thinning reduces 1-3 μm, than electricity
Hold and improve 6% or so, bending times improve 17% or so.
Aluminium foil corrosion Reducing thickness, specific capacitance and the bending times of the comparative example 1 of table 1 and embodiment 1-11
| Sample | Corrosion thinning amount | Specific capacitance (μ F/cm2) | Bending times |
| Comparative example | 5μm | 0.739 | 19 |
| Embodiment 1 | 1μm | 0.767 | 24 |
| Embodiment 2 | 2μm | 0.773 | 22 |
| Embodiment 3 | 1μm | 0.774 | 23 |
| Embodiment 4 | 1μm | 0.787 | 23 |
| Embodiment 5 | 3μm | 0.774 | 21 |
| Embodiment 6 | 3μm | 0.765 | 22 |
| Embodiment 7 | 2μm | 0.799 | 26 |
| Embodiment 8 | 3μm | 0.765 | 23 |
| Embodiment 9 | 1μm | 0.787 | 23 |
| Embodiment 10 | 2μm | 0.783 | 23 |
| Embodiment 11 | 3μm | 0.773 | 22 |
Above-described is only presently preferred embodiments of the present invention, all timess done in the range of the spirit and principles in the present invention
What modifications, equivalent substitutions and improvements etc., should be included within the scope of the present invention.
Claims (10)
1. a kind of method of mesohigh anode high-purity aluminum foil surface generalization modification, it is characterised in that comprise the steps：
Step 1：High-purity aluminum foil is pre-processed in alkaline solution；
Step 2：Aluminium foil by pretreatment is handled using the step current method of anode+negative electrode one；
Step 3：High-temperature oxydation.
2. a kind of method of mesohigh anode high-purity aluminum foil surface generalization modification according to claim 1, it is special
Levy and be, the alkaline solution described in step 1 refers to：0.1~2mol/L Na2CO3+ 0.1~1.5mol/L Na3PO4+ 0.5~
3mol/LNaOH+0.1~0.5mol/L corrosion inhibiter.
3. a kind of method of mesohigh anode high-purity aluminum foil surface generalization modification according to claim 1, it is special
Levy and be, the treatment temperature of described step 1 is 60~95 DEG C, and processing time is 5~60s.
4. a kind of method of mesohigh anode high-purity aluminum foil surface generalization modification according to claim 2, it is special
Levy and be, described corrosion inhibiter is the one or more in thiocarbamide, gelatin, BTA, sodium gluconate.
5. a kind of method of mesohigh anode high-purity aluminum foil surface generalization modification according to claim 1, it is special
Levy and be, described step 2 is specially：Aluminium foil by pretreatment is entered using the step current method of anode+negative electrode one in the solution
Row processing；
Wherein, described solution refers to：+ 0.01~0.05mol/L of 0.1~1mol/L sodium stannate+0.2~1mol/L sodium hydroxides
Sodium potassium tartrate tetrahydrate+0.1~5ml/L kayexalates.
6. a kind of method of mesohigh anode high-purity aluminum foil surface generalization modification according to claim 1, it is special
Levy and be, the treatment temperature of described step 2 is 30~60 DEG C.
7. a kind of method of mesohigh anode high-purity aluminum foil surface generalization modification according to claim 5, it is special
Levy and be, described anodic current density scope is 5~50mA/cm2, cathode-current density scope is 10~40mA/cm2。
8. a kind of method of mesohigh anode high-purity aluminum foil surface generalization modification according to claim 5, it is special
Levy and be, described anodic treatment times are 10~60s, the cathode treatment time is 10~60s.
9. a kind of method of mesohigh anode high-purity aluminum foil surface generalization modification according to claim 1, it is special
Levy and be, the oxidizing temperature of the high-temperature oxydation described in step 3 is 100~400 DEG C, and oxidization time is 10~100 seconds.
10. a kind of method of mesohigh anode high-purity aluminum foil surface modified integrated modification according to claim 1,
Characterized in that, described high-purity aluminum foil refers to：It will form { 100 } plane texture after finished product recrystallization annealing processing and occupy
Rate is more than 95%, and surface is containing micro Fe, Si, Cu, Zn, Ga, Mn element and is not enriched with Pb elements, and Al purity is 99.99%
Mesohigh anode high-purity aluminum foil.
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| CN108085721A (en) * | 2017-12-18 | 2018-05-29 | 广西正润新材料科技有限公司 | A kind of method and system of aluminium foil surface sol-gal process in-situ deposition tin nucleus |
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| CN108085721A (en) * | 2017-12-18 | 2018-05-29 | 广西正润新材料科技有限公司 | A kind of method and system of aluminium foil surface sol-gal process in-situ deposition tin nucleus |
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