CN103451713A - Corrosion pretreatment method for anode oxidation deposited zinc/tin crystal nucleus of middle-high voltage electronic aluminum foil - Google Patents
Corrosion pretreatment method for anode oxidation deposited zinc/tin crystal nucleus of middle-high voltage electronic aluminum foil Download PDFInfo
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Abstract
The invention discloses a corrosion pretreatment method for anode oxidation deposited zinc/tin crystal nucleus of a middle-high voltage electronic aluminum foil. The corrosion pretreatment method comprises the following steps of: carrying out anodic oxidation treatment on the middle-high voltage electronic aluminum foil in sulfuric acid, phosphoric acid, chromic acid or oxalic acid, so as to generate an oxidation film with micropores; then soaking the middle-high voltage electronic aluminum foil which is subjected to the anodic oxidation treatment in an alkali solution dissolved with ZnO or SnO, so as to corrode and thin the porous aluminum oxide film to expose active aluminum at the bottom of the micropores, and carrying out replacement reaction between the active aluminum and a zinc acid radical or a tin acid radical, so as to generate the zinc crystal nucleus or the tin crystal nucleus. In the process that the aluminum foil is corroded, the zinc crystal nucleus or the tin crystal nucleus can guide the aluminum foil to generate micropores, and the possibility that the micropores are combined is reduced; the aluminum foil can be prevented from being corroded and thinned because of an Al2O3 film, and the specific capacitance and the fracture resistance of the middle-high voltage electronic aluminum foil are improved.
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
Constantly dwindle the development with High Density Packaging for what adapt to the 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 enlarge its specific surface area, to improve than electric capacity, 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, sends out pitting corrosion, the aftertreatment of reaming burn into.The high-pressure aluminium foil surface forms equally distributed high-density, the rational Tunnel-hole of size (aperture, hole length) is the key that obtains 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 distribution, density and the pit growth of initial pit.The ununiformity of surface tissue causes surperficial pit skewness, and the pit size differs greatly, very unfavorable to the specific surface area that improves 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, can effectively improve the homogeneity of sending out hole, improve the ratio electric capacity of aluminium foil.Therefore, rationally, effectively pretreatment technology is to improve etched foil than one of gordian technique of electric capacity.Existing preconditioning technique comprises: acid, alkali soak pre-treatment, electrolysis pretreatment and electroless plating metal etc.China Patent Publication No. is that 101425392A has invented the bismuth-containing that adds 0.001～0.025% in the treatment solution of alkali, acid, mixed base or mixing acid or the compound of indium, or the pretreatment technology of its mixture, has improved the ratio electric capacity of aluminium foil.China Patent Publication No. is that 101976612A has invented with 0.15～0.6mol/L NaOH+0.01～1%ZnO mixing solutions and cleans and pretreatment fluid as aluminium foil, has the aluminium foil of raising than the effect of electric capacity.Although above patented technology technique is simple, industrial production is easy to realization, and it is limited that it improves effect than electric capacity.China Patent Publication No. is that 1993786A has utilized the shielding film technological invention and prepares organic microballoon of one deck arranging rule at aluminium foil surface, during aluminium foil corrosion, guides it to form the orderly Tunnel-hole of high-density, can significantly improve the specific volume of aluminium foil.This technology is because the flow process complexity is loaded down with trivial details, and controlling factor is more, also rests at present the laboratory study stage, 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 be under the prerequisite of holding anode aluminium foil physical strength and buckling performance, improve Tunnel-hole and send out the hole homogeneity, reduce and the hole probability, thereby improve its specific surface area and static 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: the 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 that dissolves in ZnO or SnO, make the Properties of Porous Alumina Membranes corrosion thinning, the micropore bottom is exposed active aluminum and zincic acid root or stannate radicle generation replacement(metathesis)reaction and is generated 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 to temperature is 15～25 ℃, and in the sulphuric acid soln that mass percent is 15～25%, and to apply current density be 5～20mA cm
-2anodic current carries out anodic oxidation 10～60s.
Described phosphoric acid anodizing treatment condition are for aluminium foil is placed in to temperature is 20～25 ℃, and in the phosphoric acid solution that mass percent is 10～15%, and to apply current density be 5～20mA cm
-2anodic current carries out anodic oxidation 10～60s.
Described chromic acid anodizing treatment condition are for aluminium foil is placed in to temperature is 35 ± 2 ℃, and in the chromic acid solution that mass percent is 3.5～5%, and to apply current density be 5～20mA cm
-2anodic current carries out anodic oxidation 10～60s.
Described oxalic acid anodizing treatment condition are for aluminium foil is placed in to temperature is 15～20 ℃, and in the oxalic acid solution that mass percent is 4～6%, and to apply current density be 5～25mA cm
-2anodic current carries out anodic oxidation 10～60s.
The described technical qualification that mesohigh aluminium foil after anodic oxidation treatment is soaked in the basic solution that dissolves in ZnO or SnO are: temperature is 30～50 ℃, containing mass percent is 1～10%NaOH, 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 outstanding technological merit of the present invention is:
The aluminium foil process is at sulphuric acid soln, or phosphoric acid solution, or chromic acid solution, or, after the oxalic acid solution Anodic Oxidation, at aluminium foil surface, generates the micropore oxide film.This film has unique structure, nestles up the metallic aluminium surface and has the blocking layer that one deck is quite thin.Aluminium foil after anodic oxidation is placed in to the basic solution that dissolves in ZnO or SnO to be soaked, anode oxide film generation uniform dissolution, the micropore bottom occurs to dissolve exposes active aluminum, with the zincic acid root be transformed in alkaline solution or stannate radicle generation replacement(metathesis)reaction, generates zinc nucleus or tin nucleus.When entering in etchant solution, aluminium foil corrodes while sending out hole, the Zn nucleus on surface or Sn nucleus and aluminium form the microbattery of a large amount of and disperse, eliminate or weakened because aluminium foil surface greasy dirt, impurity, heat oxide film cause and sent out the inhomogeneous impact in hole, zinc nucleus or tin nucleus, as an evenly hole of active site guiding aluminium foil, reduce and the 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, with respect to traditional acid, alkali, mixing acid or mixed base dipping pretreatment technique, pit is more evenly distributed, and the static specific volume improves more remarkable.
Embodiment
The invention will be further described by the following examples.
In the galvanic corrosion of anode aluminium foil, adopting purity is 99.99%, and thickness is 120 μ m, the aluminium foil that the cubic texture occupation rate is greater than 95%.Technical process of the present invention is: anodic oxidation+alkali cleaning pre-treatment, a pitting corrosion, the aftertreatment of reaming burn into.Its concrete steps are as follows:
(1) anodic oxidation+alkali cleaning pre-treatment: the mesohigh electric aluminum foil, in sulphuric acid soln, or in phosphoric acid solution, or in chromic acid solution, or is carried out to 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 that dissolves in ZnO or SnO, make the Properties of Porous Alumina Membranes corrosion thinning, the micropore bottom is exposed active aluminum and zincic acid root or stannate radicle generation replacement(metathesis)reaction and is generated zinc nucleus or tin nucleus, finally with deionized water, aluminium foil is rinsed well.
(2) send out pitting corrosion: it is 65～80 ℃ that pretreated aluminium foil is placed on to temperature, and containing mass percent is in the mixing solutions of 1%～10% hydrochloric acid and 20%～40% sulfuric acid, and applying current density is 400～1000mA cm
-2direct current send out pitting corrosion 50～180s.
(3) reaming corrosion: sending out the complete aluminium foil in hole, to be placed on temperature be in 65～80 ℃ of reaming corrosive fluids, the corrosive fluid main component is 1%～10%(mass percent) hydrochloric acid or 3%～10%(mass percent) salpeter solution, applying current density is 50～200mA cm
-2direct current carry out reaming corrosion 400～1000s.
(4) aftertreatment: by secondary chambering, to be placed on temperature be 65～70 ℃ to complete aluminium foil, in the salpeter solution that to contain mass percent be 0.13%～10%, soaks 30～180s.
Last basis " the electron trade standard SJ/T11140-1997 of the People's Republic of China (PRC): electrode foil for aluminum electrolytic capacitors " is carried out 520V and is changed into.
Comparative Examples
Adopt traditional mixing acid pretreatment technology, pretreatment fluid used is 1M HCl+7M H
2sO
4, temperature is 80 ℃, aluminium foil is directly soaked in pretreatment fluid to 120s, then carries out above-mentioned send out pitting corrosion, the aftertreatment of reaming burn into and 520V and change into processing.
Embodiment 1
It is 20 ℃ that aluminium foil is placed in to temperature, the H that mass percent is 20%
2sO
4in solution, applying current density is 5mA cm
-2anodic current carries out anodic oxidation 30s, and then aluminium foil is placed in to temperature is 40 ℃, soak 30s in the mixing solutions that mass percent is 5%NaOH and 0.05%ZnO, then carry out identical with Comparative Examples pitting corrosion, the aftertreatment of reaming burn into and the 520V of sending out and change into processing.
Embodiment 2
It is 20 ℃ that aluminium foil is placed in to temperature, the H that mass percent is 20%
2sO
4in solution, applying current density is 10mA cm
-2anodic current carries out anodic oxidation 30s, and then aluminium foil is placed in to temperature is 40 ℃, soak 30s in the mixing solutions that mass percent is 5%NaOH and 0.05%ZnO, then carry out identical with Comparative Examples pitting corrosion, the aftertreatment of reaming burn into and the 520V of sending out and change into processing.
Embodiment 3
It is 20 ℃ that aluminium foil is placed in to temperature, the H that mass percent is 20%
2sO
4in solution, applying current density is 10mA cm
-2anodic current carries out anodic oxidation 10s, and then aluminium foil is placed in to temperature is 40 ℃, soak 30s in the mixing solutions that mass percent is 5%NaOH and 0.1%ZnO, then carry out identical with Comparative Examples pitting corrosion, the aftertreatment of reaming burn into and the 520V of sending out and change into processing.
Embodiment 4
It is 20 ℃ that aluminium foil is placed in to temperature, the H that mass percent is 20%
2sO
4in solution, applying current density is 10mA cm
-2anodic current carries out anodic oxidation 30s, and then aluminium foil is placed in to temperature is 40 ℃, soak 30s in the mixing solutions that mass percent is 5%NaOH and 0.1%ZnO, then carry out identical with Comparative Examples pitting corrosion, the aftertreatment of reaming burn into and the 520V of sending out and change into processing.
Embodiment 5
It is 20 ℃ that aluminium foil is placed in to temperature, the H that mass percent is 20%
2sO
4in solution, applying current density is 10mA cm
-2anodic current carries out anodic oxidation 50s, and then aluminium foil is placed in to temperature is 40 ℃, soak 30s in the mixing solutions that mass percent is 5%NaOH and 0.1%ZnO, then carry out identical with Comparative Examples pitting corrosion, the aftertreatment of reaming burn into and the 520V of sending out and change into processing.
Embodiment 6
It is 20 ℃ that aluminium foil is placed in to temperature, the H that mass percent is 20%
2sO
4in solution, applying current density is 10mA cm
-2anodic current carries out anodic oxidation 30s, and then aluminium foil is placed in to temperature is 40 ℃, in the mixing solutions that mass percent is 5%KOH and 0.1%ZnO, soaks 30s, then carries out send out pitting corrosion, reaming burn into aftertreatment and the 520V identical with Comparative Examples and change into processing.
Embodiment 7
It is 20 ℃ that aluminium foil is placed in to temperature, the H that mass percent is 20%
2sO
4in solution, applying current density is 10mA cm
-2anodic current carries out anodic oxidation 30s, and then aluminium foil is placed in to temperature is 40 ℃, mass percent is 2.5%NaOH, in the mixing solutions of 2.5%KOH and 0.1%ZnO, soaks 30s, then carries out identical with Comparative Examples pitting corrosion, the aftertreatment of reaming burn into and the 520V of sending out and change into processing.
Embodiment 8
It is 20 ℃ that aluminium foil is placed in to temperature, the H that mass percent is 20%
2sO
4in solution, applying current density is 10mA cm
-2anodic current carries out anodic oxidation 30s, and then aluminium foil is placed in to temperature is 40 ℃, soak 30s in the mixing solutions that mass percent is 5%NaOH and 0.05%SnO, then carry out identical with Comparative Examples pitting corrosion, the aftertreatment of reaming burn into and the 520V of sending out and change into processing.
Embodiment 9
It is 20 ℃ that aluminium foil is placed in to temperature, the H that mass percent is 20%
2sO
4in solution, applying current density is 10mA cm
-2anodic current carries out anodic oxidation 30s, and then aluminium foil is placed in to temperature is 40 ℃, soak 30s in the mixing solutions that mass percent is 5%NaOH and 0.1%SnO, then carry out identical with Comparative Examples pitting corrosion, the aftertreatment of reaming burn into and the 520V of sending out and change into processing.
Embodiment 10
It is 20 ℃ that aluminium foil is placed in to temperature, the H that mass percent is 15%
3pO
4in solution, applying current density is 10mA cm
-2anodic current carries out anodic oxidation 30s, and then aluminium foil is placed in to temperature is 40 ℃, soak 30s in the mixing solutions that mass percent is 5%NaOH and 0.1%ZnO, then carry out identical with Comparative Examples pitting corrosion, the aftertreatment of reaming burn into and the 520V of sending out and change into processing.
Embodiment 11
It is 35 ℃ that aluminium foil is placed in to temperature, the H that mass percent is 4%
2crO
4in solution, applying current density is 10mA cm
-2anodic current carries out anodic oxidation 30s, and then aluminium foil is placed in to temperature is 40 ℃, soak 30s in the mixing solutions that mass percent is 5%NaOH and 0.1%ZnO, then carry out identical with Comparative Examples pitting corrosion, the aftertreatment of reaming burn into and the 520V of sending out and change into processing.
Embodiment 12
It is 20 ℃ that aluminium foil is placed in to temperature, the H that mass percent is 5%
2c
2o
4in solution, applying current density is 10mA cm
-2anodic current carries out anodic oxidation 30s, and then aluminium foil is placed in to temperature is 40 ℃, soak 30s in the mixing solutions that mass percent is 5%NaOH and 0.1%ZnO, then carry out identical with Comparative Examples pitting corrosion, the aftertreatment of reaming burn into and the 520V of sending out and change into processing.
Table 1 Comparative Examples 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: the 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 that dissolves in ZnO or SnO, make the Properties of Porous Alumina Membranes corrosion thinning, the micropore bottom is exposed active aluminum and zincic acid root or stannate radicle generation replacement(metathesis)reaction and is generated 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 to temperature is 15～25 ℃, and in the sulphuric acid soln that mass percent is 15～25%, and to apply current density be 5～20mA cm
-2anodic current carries out anodic oxidation 10～60s;
Described phosphoric acid anodizing treatment condition are for aluminium foil is placed in to temperature is 20～25 ℃, and in the phosphoric acid solution that mass percent is 10～15%, and to apply current density be 5～20mA cm
-2anodic current carries out anodic oxidation 10～60s;
Described chromic acid anodizing treatment condition are for aluminium foil is placed in to temperature is 35 ± 2 ℃, and in the chromic acid solution that mass percent is 3.5～5%, and to apply current density be 5～20mA cm
-2anodic current carries out anodic oxidation 10～60s;
Described oxalic acid anodizing treatment condition are for aluminium foil is placed in to temperature is 15～20 ℃, and in the oxalic acid solution that mass percent is 4～6%, and to apply current density be 5～25mA cm
-2anodic current carries out anodic oxidation 10～60s;
The described technical qualification that mesohigh aluminium foil after anodic oxidation treatment is soaked in the basic solution that dissolves in ZnO or SnO are: temperature is 30～50 ℃, containing mass percent is 1～10%NaOH, 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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Cited By (6)
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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 |
| CN103774193A (en) * | 2014-01-06 | 2014-05-07 | 广西贺州市桂东电子科技有限责任公司 | Method for electrolytic-depositing dispersed zinc crystal nucleuses on surface of medium-high voltage electronic aluminum foil |
| CN104357886A (en) * | 2014-10-30 | 2015-02-18 | 广西贺州桂海铝业科技有限公司 | Method for chemically depositing diffused tin-zinc crystal nucleus on surface of high-purity aluminum foil for medium/high-voltage positive electrode |
| CN104733181A (en) * | 2015-02-16 | 2015-06-24 | 广西贺州桂海铝业科技有限公司 | Method and device for depositing disperse tin and zinc crystal nucleuses on surface of highly pure aluminum foil for medium and high voltage anodes in mist spraying mode |
| 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 |
| CN116329501A (en) * | 2023-03-17 | 2023-06-27 | 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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| 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 |
| CN103774193A (en) * | 2014-01-06 | 2014-05-07 | 广西贺州市桂东电子科技有限责任公司 | Method for electrolytic-depositing dispersed zinc crystal nucleuses on surface of medium-high voltage electronic aluminum foil |
| 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 |
| CN104357886A (en) * | 2014-10-30 | 2015-02-18 | 广西贺州桂海铝业科技有限公司 | Method for chemically depositing diffused tin-zinc crystal nucleus on surface of high-purity aluminum foil for medium/high-voltage positive electrode |
| 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 |
| CN104733181A (en) * | 2015-02-16 | 2015-06-24 | 广西贺州桂海铝业科技有限公司 | Method and device for depositing disperse tin and zinc crystal nucleuses on surface of highly pure aluminum foil for medium and high voltage anodes in mist spraying mode |
| 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 |
| CN116329501A (en) * | 2023-03-17 | 2023-06-27 | 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 |
| 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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