CN103451713B - The corrosion pretreating method of mesohigh electric aluminum foil anodic oxidation deposition zinc or tin nucleus - Google Patents
The corrosion pretreating method of mesohigh electric aluminum foil anodic oxidation deposition zinc or tin nucleus Download PDFInfo
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- CN103451713B CN103451713B CN201310381440.1A CN201310381440A CN103451713B CN 103451713 B CN103451713 B CN 103451713B CN 201310381440 A CN201310381440 A CN 201310381440A CN 103451713 B CN103451713 B CN 103451713B
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Abstract
A corrosion pretreating method for mesohigh electric aluminum foil anodic oxidation deposition zinc or tin nucleus, carries out anodic oxidation treatment by mesohigh electric aluminum foil in sulfuric acid or phosphoric acid or chromic acid or oxalic acid, generates the oxide film with micropore; Then the mesohigh aluminium foil after anodic oxidation treatment is soaked in the basic solution dissolving in ZnO or SnO, make Properties of Porous Alumina Membranes corrosion thinning, expose active aluminum and zincic acid root or stannate radicle generation replacement(metathesis)reaction bottom micropore and generate zinc nucleus or tin nucleus.In the aluminium foil corrosion course of processing, zinc nucleus or tin nucleus can guide aluminium foil hair engaging aperture, reduce and hole probability, Al
2o
3film can suppress the corrosion thinning of aluminium foil, improves ratio capacitance and the warping resistance performance of mesohigh electric aluminum foil.
Description
Technical field
The present invention relates to anode foil for aluminum electrolytic capacitor corrosion technology field, the corrosion pretreating method of especially a kind of mesohigh electric aluminum foil anodic oxidation deposition zinc or tin nucleus.
Background technology
The development with High Density Packaging is constantly reduced in order to what adapt to complete electronic set volume, miniaturization is the inexorable trend of aluminium electrolutic capacitor development, by to having, { high-purity aluminum foil of 100} texture carries out electrolytic corrosion to expand its specific surface area, to improve ratio capacitance, is the most effective technological approaches of aluminium electrolutic capacitor miniaturization.
At present, the electrolytic corrosion process of mesohigh aluminium foil generally comprises pre-treatment, the aftertreatment of hair engaging aperture burn into reaming burn into.High-pressure aluminium foil surface forms equally distributed high-density, size (aperture, hole length) rational Tunnel-hole is the key obtaining high specific capacitance.The weave construction of light paper tinsel, especially surface quality (greasy dirt, impurity, defect concentration and distribution, oxide thickness etc.) have a significant impact the distribution of initial pit, density and pit growth.The ununiformity of surface tissue causes surperficial pit skewness, and pit size differs greatly, very unfavorable to the specific surface area improving aluminium foil, and then has a strong impact on the raising of aluminium foil specific volume.By certain pre-treatment, change the state of mesohigh aluminium foil surface oxide film or passive film, as composition, structure and defect, effectively can improve the homogeneity of hair engaging aperture, improve the ratio capacitance of aluminium foil.Therefore, rationally, effective pretreatment technology is one of gordian technique improving etched foil ratio capacitance.Existing preconditioning technique comprises: acid, alkaline pretreatment, electrolysis pretreatment and electroless plating metal etc.China Patent Publication No. is that 101425392A has invented add the bismuth-containing of 0.001 ~ 0.025% or the compound of indium in the treatment solution of alkali, acid, mixed base or mixing acid, or the pretreatment technology of its mixture, improves the ratio capacitance of aluminium foil.China Patent Publication No. is that 101976612A to have invented with 0.15 ~ 0.6mol/LNaOH+0.01 ~ 1%ZnO mixing solutions as aluminium foil cleaning and pretreatment fluid, has the effect improving aluminium foil ratio capacitance.Although above patented technology technique is simple, industrial production is easy to realize, and its ratio capacitance improves limited efficiency.China Patent Publication No. is that 1993786A utilizes shielding film technological invention to prepare the organic micro-spheres of one deck arranging rule at aluminium foil surface, guides it to form the orderly Tunnel-hole of high-density, can significantly improve the specific volume of aluminium foil during aluminium foil corrosion.This technology due to flow process complexity loaded down with trivial details, controlling factor is more, also rests on the laboratory study stage at present, has no industrial report in enormous quantities.
Summary of the invention
The present invention is directed to the deficiency of existing mesohigh aluminium foil preconditioning technique, the corrosion pretreating method of a kind of mesohigh electric aluminum foil anodic oxidation deposition zinc or tin nucleus is provided, can under the prerequisite of holding anode aluminium foil physical strength and buckling performance, improve Tunnel-hole hair engaging aperture homogeneity, reduce and hole probability, thus improve its specific surface area and electrostatic specific volume.
Technical scheme of the present invention is as follows: the corrosion pretreating method of a kind of mesohigh electric aluminum foil anodic oxidation deposition zinc or tin nucleus, comprise the steps: mesohigh electric aluminum foil at sulphuric acid soln, or phosphoric acid solution, or chromic acid solution, or carry out anodic oxidation treatment in oxalic acid solution, generate the oxide film with micropore; Then the mesohigh aluminium foil after anodic oxidation treatment is soaked in the basic solution dissolving in ZnO or SnO, make Properties of Porous Alumina Membranes corrosion thinning, expose active aluminum and zincic acid root or stannate radicle generation replacement(metathesis)reaction bottom micropore and generate zinc nucleus or tin nucleus, finally with deionized water, aluminium foil is rinsed well.
Described sulphuric acid anodizing treatment condition are for aluminium foil is placed in temperature is 15 ~ 25 DEG C, and mass percent is in the sulphuric acid soln of 15 ~ 25%, and to apply current density be 5 ~ 20mAcm
-2anodic current carries out anodic oxidation 10 ~ 60s.
Described phosphoric acid anodizing treatment condition are for aluminium foil is placed in temperature is 20 ~ 25 DEG C, and mass percent is in the phosphoric acid solution of 10 ~ 15%, and to apply current density be 5 ~ 20mAcm
-2anodic current carries out anodic oxidation 10 ~ 60s.
Described chromic acid anodizing treatment condition are for aluminium foil is placed in temperature is 35 ± 2 DEG C, and mass percent is in the chromic acid solution of 3.5 ~ 5%, and to apply current density be 5 ~ 20mAcm
-2anodic current carries out anodic oxidation 10 ~ 60s.
Described oxalic acid anodizing treatment condition are for aluminium foil is placed in temperature is 15 ~ 20 DEG C, and mass percent is in the oxalic acid solution of 4 ~ 6%, and to apply current density be 5 ~ 25mAcm
-2anodic current carries out anodic oxidation 10 ~ 60s.
Describedly by the technical qualification that the mesohigh aluminium foil after anodic oxidation treatment soaks in the basic solution dissolving in ZnO or SnO be: temperature is 30 ~ 50 DEG C, be 1 ~ 10%NaOH containing mass percent, or KOH, or NaOH and KOH, and dissolve in the basic solution that mass percent is 0.01 ~ 1%ZnO or SnO, soak time is 20 ~ 120s.
The technological merit that the present invention gives prominence to is:
Aluminium foil passes through at sulphuric acid soln, or phosphoric acid solution, or chromic acid solution, or after oxalic acid solution Anodic Oxidation, generates microporous alumina film at aluminium foil surface.This film has unique structure, nestles up metallic aluminum surface and has the quite thin blocking layer of one deck.Aluminium foil after anodic oxidation is placed in the basic solution dissolving in ZnO or SnO soak, anode oxide film generation uniform dissolution, there is dissolving bottom micropore and expose active aluminum, generate zinc nucleus or tin nucleus with the zincic acid root be transformed in alkaline solution or stannate radicle generation replacement(metathesis)reaction.When aluminium foil enter in etchant solution carry out corrosion hair engaging aperture time, the Zn nucleus on surface or Sn nucleus and aluminium are formed in a large number and the microbattery of disperse, the impact eliminated or reduce because aluminium foil surface greasy dirt, impurity, heat oxide film cause hair engaging aperture uneven, zinc nucleus or tin nucleus guide the even hair engaging aperture of aluminium foil as active site, reduce and hole probability.Anode oxide film can suppress the corrosion thinning of aluminium foil surface simultaneously, improves the physical strength of aluminium foil.By pretreatment process of the present invention, relative to traditional acid, alkali, mixing acid or mixed base dipping pretreatment technique, pit is more evenly distributed, and electrostatic specific volume improves more remarkable.
Embodiment
The invention will be further described by the following examples.
In the galvanic corrosion of anode aluminium foil, adopt purity to be 99.99%, thickness is 120 μm, the aluminium foil that cubic texture occupancy rate is greater than 95%.Technical process of the present invention is: anodic oxidation+alkali cleaning pre-treatment, the aftertreatment of hair engaging aperture burn into reaming burn into.Its concrete steps are as follows:
(1) anodic oxidation+alkali cleaning pre-treatment: by mesohigh electric aluminum foil in sulphuric acid soln, or in phosphoric acid solution, or in chromic acid solution, or carry out anodic oxidation treatment in oxalic acid solution, generate the oxide film with micropore; Then the mesohigh aluminium foil after anodic oxidation treatment is soaked in the basic solution dissolving in ZnO or SnO, make Properties of Porous Alumina Membranes corrosion thinning, expose active aluminum and zincic acid root or stannate radicle generation replacement(metathesis)reaction bottom micropore and generate zinc nucleus or tin nucleus, finally with deionized water, aluminium foil is rinsed well.
(2) hair engaging aperture corrosion: pretreated aluminium foil being placed on temperature is 65 ~ 80 DEG C, and be in the mixing solutions of 1% ~ 10% hydrochloric acid and 20% ~ 40% sulfuric acid containing mass percent, applying current density is 400 ~ 1000mAcm
-2direct current carry out hair engaging aperture corrosion 50 ~ 180s.
(3) reaming corrosion: aluminium foil complete for hair engaging aperture being placed on temperature is in 65 ~ 80 DEG C of reaming corrosive fluids, corrosive fluid main component is 1% ~ 10%(mass percent) hydrochloric acid or 3% ~ 10%(mass percent) salpeter solution, applying current density is 50 ~ 200mAcm
-2direct current carry out reaming corrosion 400 ~ 1000s.
(4) aftertreatment: aluminium foil complete for secondary chambering being placed on temperature is 65 ~ 70 DEG C is soak 30 ~ 180s in the salpeter solution of 0.13% ~ 10% containing mass percent.
Last basis " People's Republic of China (PRC) electron trade standard SJ/T11140-1997: electrode foil for aluminum electrolytic capacitors " is carried out 520V and is changed into.
Comparative example
Adopt traditional mixing acid pretreatment technology, pretreatment fluid used is 1MHCl+7MH
2sO
4, temperature is 80 DEG C, and aluminium foil is directly soaked 120s in pretreatment fluid, then carries out above-mentioned hair engaging aperture burn into reaming burn into aftertreatment and 520V changes into process.
Embodiment 1
Aluminium foil being placed in temperature is 20 DEG C, and mass percent is the H of 20%
2sO
4in solution, applying current density is 5mAcm
-2anodic current carries out anodic oxidation 30s, and then aluminium foil is placed in temperature is 40 DEG C, mass percent is soak 30s in the mixing solutions of 5%NaOH and 0.05%ZnO, then carries out the hair engaging aperture burn into reaming burn into aftertreatment identical with comparative example and 520V changes into process.
Embodiment 2
Aluminium foil being placed in temperature is 20 DEG C, and mass percent is the H of 20%
2sO
4in solution, applying current density is 10mAcm
-2anodic current carries out anodic oxidation 30s, and then aluminium foil is placed in temperature is 40 DEG C, mass percent is soak 30s in the mixing solutions of 5%NaOH and 0.05%ZnO, then carries out the hair engaging aperture burn into reaming burn into aftertreatment identical with comparative example and 520V changes into process.
Embodiment 3
Aluminium foil being placed in temperature is 20 DEG C, and mass percent is the H of 20%
2sO
4in solution, applying current density is 10mAcm
-2anodic current carries out anodic oxidation 10s, and then aluminium foil is placed in temperature is 40 DEG C, mass percent is soak 30s in the mixing solutions of 5%NaOH and 0.1%ZnO, then carries out the hair engaging aperture burn into reaming burn into aftertreatment identical with comparative example and 520V changes into process.
Embodiment 4
Aluminium foil being placed in temperature is 20 DEG C, and mass percent is the H of 20%
2sO
4in solution, applying current density is 10mAcm
-2anodic current carries out anodic oxidation 30s, and then aluminium foil is placed in temperature is 40 DEG C, mass percent is soak 30s in the mixing solutions of 5%NaOH and 0.1%ZnO, then carries out the hair engaging aperture burn into reaming burn into aftertreatment identical with comparative example and 520V changes into process.
Embodiment 5
Aluminium foil being placed in temperature is 20 DEG C, and mass percent is the H of 20%
2sO
4in solution, applying current density is 10mAcm
-2anodic current carries out anodic oxidation 50s, and then aluminium foil is placed in temperature is 40 DEG C, mass percent is soak 30s in the mixing solutions of 5%NaOH and 0.1%ZnO, then carries out the hair engaging aperture burn into reaming burn into aftertreatment identical with comparative example and 520V changes into process.
Embodiment 6
Aluminium foil being placed in temperature is 20 DEG C, and mass percent is the H of 20%
2sO
4in solution, applying current density is 10mAcm
-2anodic current carries out anodic oxidation 30s, and then aluminium foil to be placed in temperature be 40 DEG C, and mass percent is soak 30s in the mixing solutions of 5%KOH and 0.1%ZnO, then carries out the hair engaging aperture burn into reaming burn into aftertreatment identical with comparative example and 520V changes into process.
Embodiment 7
Aluminium foil being placed in temperature is 20 DEG C, and mass percent is the H of 20%
2sO
4in solution, applying current density is 10mAcm
-2anodic current carries out anodic oxidation 30s, and then aluminium foil is placed in temperature is 40 DEG C, mass percent is soak 30s in the mixing solutions of 2.5%NaOH, 2.5%KOH and 0.1%ZnO, then carries out the hair engaging aperture burn into reaming burn into aftertreatment identical with comparative example and 520V changes into process.
Embodiment 8
Aluminium foil being placed in temperature is 20 DEG C, and mass percent is the H of 20%
2sO
4in solution, applying current density is 10mAcm
-2anodic current carries out anodic oxidation 30s, and then aluminium foil is placed in temperature is 40 DEG C, mass percent is soak 30s in the mixing solutions of 5%NaOH and 0.05%SnO, then carries out the hair engaging aperture burn into reaming burn into aftertreatment identical with comparative example and 520V changes into process.
Embodiment 9
Aluminium foil being placed in temperature is 20 DEG C, and mass percent is the H of 20%
2sO
4in solution, applying current density is 10mAcm
-2anodic current carries out anodic oxidation 30s, and then aluminium foil is placed in temperature is 40 DEG C, mass percent is soak 30s in the mixing solutions of 5%NaOH and 0.1%SnO, then carries out the hair engaging aperture burn into reaming burn into aftertreatment identical with comparative example and 520V changes into process.
Embodiment 10
Aluminium foil being placed in temperature is 20 DEG C, and mass percent is the H of 15%
3pO
4in solution, applying current density is 10mAcm
-2anodic current carries out anodic oxidation 30s, and then aluminium foil is placed in temperature is 40 DEG C, mass percent is soak 30s in the mixing solutions of 5%NaOH and 0.1%ZnO, then carries out the hair engaging aperture burn into reaming burn into aftertreatment identical with comparative example and 520V changes into process.
Embodiment 11
Aluminium foil being placed in temperature is 35 DEG C, and mass percent is the H of 4%
2crO
4in solution, applying current density is 10mAcm
-2anodic current carries out anodic oxidation 30s, and then aluminium foil is placed in temperature is 40 DEG C, mass percent is soak 30s in the mixing solutions of 5%NaOH and 0.1%ZnO, then carries out the hair engaging aperture burn into reaming burn into aftertreatment identical with comparative example and 520V changes into process.
Embodiment 12
Aluminium foil being placed in temperature is 20 DEG C, and mass percent is the H of 5%
2c
2o
4in solution, applying current density is 10mAcm
-2anodic current carries out anodic oxidation 30s, and then aluminium foil is placed in temperature is 40 DEG C, mass percent is soak 30s in the mixing solutions of 5%NaOH and 0.1%ZnO, then carries out the hair engaging aperture burn into reaming burn into aftertreatment identical with comparative example and 520V changes into process.
Table 1 comparative example and use pretreatment process of the present invention obtain bulking value and the tensile strength of aluminium foil
Claims (1)
1. the corrosion pretreating method of a mesohigh electric aluminum foil anodic oxidation deposition zinc or tin nucleus, it is characterized in that, comprise the steps: mesohigh electric aluminum foil at sulphuric acid soln, or phosphoric acid solution, or chromic acid solution, or carry out anodic oxidation treatment in oxalic acid solution, generate the oxide film with micropore; Then the mesohigh aluminium foil after anodic oxidation treatment is soaked in the basic solution dissolving in ZnO or SnO, make Properties of Porous Alumina Membranes corrosion thinning, expose active aluminum and zincic acid root or stannate radicle generation replacement(metathesis)reaction bottom micropore and generate zinc nucleus or tin nucleus, finally with deionized water, aluminium foil is rinsed well
Described sulphuric acid anodizing treatment condition are for aluminium foil is placed in temperature is 15 ~ 25 DEG C, and mass percent is in the sulphuric acid soln of 15 ~ 25%, and to apply current density be 5 ~ 20mAcm
-2anodic current carries out anodic oxidation 10 ~ 60s;
Described phosphoric acid anodizing treatment condition are for aluminium foil is placed in temperature is 20 ~ 25 DEG C, and mass percent is in the phosphoric acid solution of 10 ~ 15%, and to apply current density be 5 ~ 20mAcm
-2anodic current carries out anodic oxidation 10 ~ 60s;
Described chromic acid anodizing treatment condition are for aluminium foil is placed in temperature is 35 ± 2 DEG C, and mass percent is in the chromic acid solution of 3.5 ~ 5%, and to apply current density be 5 ~ 20mAcm
-2anodic current carries out anodic oxidation 10 ~ 60s;
Described oxalic acid anodizing treatment condition are for aluminium foil is placed in temperature is 15 ~ 20 DEG C, and mass percent is in the oxalic acid solution of 4 ~ 6%, and to apply current density be 5 ~ 25mAcm
-2anodic current carries out anodic oxidation 10 ~ 60s;
Describedly by the technical qualification that the mesohigh aluminium foil after anodic oxidation treatment soaks in the basic solution dissolving in ZnO or SnO be: temperature is 30 ~ 50 DEG C, be 1 ~ 10%NaOH containing mass percent, or KOH, or NaOH and KOH, and dissolve in the basic solution that mass percent is 0.01 ~ 1%ZnO or SnO, soak time is 20 ~ 120s.
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CN103774197A (en) * | 2014-01-06 | 2014-05-07 | 广西贺州市桂东电子科技有限责任公司 | Medium and high-pressure etched foil post-treatment method |
CN103774193B (en) * | 2014-01-06 | 2016-09-21 | 广西贺州市桂东电子科技有限责任公司 | A kind of method of mesohigh electric aluminum foil surface electro-deposition disperse zinc nucleus |
CN104357886B (en) * | 2014-10-30 | 2017-10-17 | 广西贺州桂海铝业科技有限公司 | The method that mesohigh anode deposits disperse tin, zinc nucleus with high-purity aluminum foil surface chemistry |
CN104733181B (en) * | 2015-02-16 | 2017-06-06 | 广西正润新材料科技有限公司 | Mesohigh anode deposits the method and device of disperse tin, zinc nucleus with high-purity aluminum foil surface spray |
CN111593356A (en) * | 2020-04-13 | 2020-08-28 | 江苏中基复合材料有限公司 | Production process and application of multistage corona-treated aluminum foil |
CN116329501B (en) * | 2023-03-17 | 2023-10-27 | 广西广投正润新材料科技有限公司 | Molten pre-tin penetration treatment method for medium-high voltage anode aluminum foil for aluminum electrolytic capacitor |
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