CN101029411A - Electrochemical corrosive process of anode aluminum foil - Google Patents
Electrochemical corrosive process of anode aluminum foil Download PDFInfo
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- CN101029411A CN101029411A CN 200610124290 CN200610124290A CN101029411A CN 101029411 A CN101029411 A CN 101029411A CN 200610124290 CN200610124290 CN 200610124290 CN 200610124290 A CN200610124290 A CN 200610124290A CN 101029411 A CN101029411 A CN 101029411A
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Abstract
An electrochemical corrosion technology for anode aluminum foils consists of two DC electrochemical corrosion processes. The first electrochemical corrosion process is carried out in mixed solution containing sulfuric acid, chlorine ion and aluminum ion; the second electrochemical corrosion process is carried out in hydrochloric acid solution added by inorganic phosphoric acid or inorganic phosphate or mixtures. It has homogenous appearance, large capacity ratio, excellent mechanical strength and water-proof performance.
Description
Technical field
The invention belongs to the manufacture method of a kind of medium-high voltage aluminum electrolytic capacitor with anode aluminium foil.
Background technology
Along with the develop rapidly of electronic technology, the volume trend toward miniaturization of complete electronic set also continues always, also is required to want corresponding dwindling as the volume of the aluminium electrolutic capacitor of one of most important components and parts of various complete machines.Wherein, the significant effects factor of restriction aluminium electrolutic capacitor volume-diminished is exactly the core starting material---the ratio electric capacity of anode aluminium foil.
Chinese patent CN85101035 discloses a kind of extending corrosion method of high voltage anode aluminum foil, this patent corrosion process does not for the second time apply direct current, and the mixed solution that adopts nitric acid and aluminum nitrate carries out the pure chemistry corrosion because nitric acid is more serious to degrading of aluminium foil surface, the anode aluminium foil of producing with this method is lower than electric capacity, and the autocatalytic characteristics during owing to nitric acid reaction, the process controllability of corrosion process is relatively poor for the second time.
Chinese patent CN1292434A discloses a kind of extending corrosion method of mesohigh anode aluminium foil, and this patent is introduced cupric ion and complex compound thereof in the second time in the pure chemistry corrosive electrolytic solution, in order to improve expansion face corrosive speed of response.But this method might cause metallic copper to be adsorbed in aluminium foil surface, causes follow-up cleaning to remove the metal impurities difficulty, product is reduced service life after making Waste Acid From Hua Cheng Foil and capacitor.
The Japanese Patent spy opens 2002-246274 and discloses a kind of method that improves the anode aluminium foil specific volume, and the anode aluminium foil that uses this method to produce has the corrosion hole of dendritic structure, has improved specific volume thereby improved area expanding rate.But also because the singularity of this pore space structure cause it to be not suitable for high-pressure aluminum electrolytic capacitor, and the aluminium foil physical strength is relatively poor.
Japanese Patent Laid-Open 2005-203530 discloses the caustic solution that improves anode aluminium foil specific volume and intensity, but technological process and plant equipment complexity, investment is big and operational administrative is inconvenient.
Summary of the invention
The objective of the invention is to overcome the deficiency of current medium-high voltage aluminum electrolytic capacitor, propose a kind of electrochemical corrosive process of anode aluminium foil with anodic aluminum corrosion expansion surface technology.
The electrochemical corrosive process of anode aluminium foil of the present invention may further comprise the steps:
For the first time electrochemical corrosion extended surface is to carry out in the mixed solution that contains sulfuric acid and chlorion, and the electric current that is applied on the aluminium foil is direct current.The mass percent of sulfuric acid is 20%～40% in the mixed solution, and the mass percent of chlorion is 1.5%～7.5%, and solution temperature is 60 ℃～90 ℃, and the current density that is applied on the aluminium foil is 0.20A/cm
2～0.80A/cm
2Wherein, when sulfuric acid concentration is lower than 20%, can make the corrosion hole density deficiency of aluminium foil surface, descend than electric capacity; When sulfuric acid concentration is higher than 40%, can make the corrosion hole of aluminium foil surface overstocked, cause surface deterioration, also can make than electric capacity to descend.When chlorine ion concentration was lower than 1.5%, the corrosion hole density deficiency of aluminium foil surface descended than electric capacity; When chlorine ion concentration was higher than 7.5%, the corrosion hole density of aluminium foil surface also became on the low side, descend than electric capacity, and mechanical strength was bad.When solution temperature is lower than 60 ℃, can make the corrosion hole density step-down of aluminium foil surface, descend than electric capacity, and physical strength is bad; When solution temperature was higher than 90 ℃, the corrosion hole density of aluminium foil surface was overstocked, causes surface deterioration, descends than electric capacity.When current density is lower than 0.20A/cm
2The time, corrosion hole density deficiency, more on the low side than electric capacity; When current density is higher than 0.80A/cm
2The time, the corrosion hole density of aluminium foil surface is overstocked, causes surface deterioration, descends than electric capacity.
For the second time electrochemical corrosion extended surface is to carry out in the hydrochloric acid solution that adds inorganic phosphate or inorganic phosphate or both mixtures, and the electric current that is applied on the aluminium foil is direct current.The mass percent of chlorion is 2.0%～10.0% in the mixing solutions, and the current density that is applied on the aluminium foil is 0.05A/cm
2～0.30A/cm
2, solution temperature is 70 ℃～95 ℃, and inorganic phosphate that is added or phosphoric acid salt mass percent are 0.01%～1%, and wherein, when the concentration of chlorion was lower than 2.0%, speed of response is too slow, and was more on the low side than electric capacity, and production efficiency is also on the low side; When the concentration of chlorion was higher than 10.0%, speed of response was too fast, and aluminium foil surface degrades seriously, and is also more on the low side than electric capacity.When aluminum ions concentration was lower than 2.0%, aluminium foil surface degrades seriously, and was more on the low side than electric capacity; When temperature was lower than 70 ℃, speed of response is too slow, and was more on the low side than electric capacity, and production efficiency is also on the low side; When temperature was higher than 95 ℃, speed of response was too fast, and aluminium foil surface degrades seriously, and is more on the low side than electric capacity.When the inorganic phosphate that adds or phosphate concn are lower than 0.01%; can not play the protection aluminium foil surface; aluminium foil surface degrades seriously; it is more on the low side than electric capacity: when inorganic phosphate or its salinity are higher than 1%; because protection excessively; the reasonable process that the corrosion hole enlarges is obstructed, and also can make specific volume on the low side.
In addition, industrial chemicals wide material sources used in the present invention, for the first time the chlorion in the electrochemical corrosion extended surface mixed solution can hydrochloric acid or muriatic mode add.Inorganic phosphate in for the second time electrochemical corrosion extended surface mixed solution or phosphate can be one or more in phosphoric acid, ammonium dihydrogen phosphate (ADP), calgon, the sodium polyphosphate etc.
The present invention compared with prior art has following advantage and effect:
1, reduces than electric capacity raising, deviation: contrast in detail visible embodiment.
2, mechanical strength improves: contrast in detail visible embodiment.
3, even, the high conformity of outward appearance visual inspection.
4, water-tolerant, it is unattenuated to store the longer time specific volume than original technology.
Concrete embodiment:
Below in conjunction with embodiment technical scheme of the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1:
Use aluminium content greater than 99.9%, cube texture is greater than 98% 110 micron thickness specific model electronic light paper tinsels, after suitably paper tinsel surface grease is removed in pre-treatment, carry out twice electrochemistry extended surface corrosion: the mass percent of sulfuric acid is 30% in for the first time electrochemical corrosion solution, chlorion adds in the mode of hydrochloric acid, its mass percent is 4.0%, solution temperature is 75 ℃, and the current density that is applied on the aluminium foil is 0.50A/cm
2The mass percent of for the second time electrochemical corrosion Chlorine in Solution ion is 6.0%, and the phosphoric acid quality percentage that adds is about 0.20%, and solution temperature is 85 ℃, and the current density that is applied on the aluminium foil is 0.10A/cm
2
Embodiment 2:
Use aluminium content greater than 99.9%, cube texture is greater than 98% 110 micron thickness specific model electronic light paper tinsels, after suitably paper tinsel surface grease is removed in pre-treatment, carry out twice electrochemistry extended surface corrosion: the mass percent of sulfuric acid is 30% in for the first time electrochemical corrosion solution, chlorion adds in the mode of ammonium chloride, its mass percent is 5.9%, solution temperature is 75 ℃, and the current density that is applied on the aluminium foil is 0.50A/cm
2The mass percent of for the second time electrochemical corrosion Chlorine in Solution ion is 6.0%, and the ammonium dihydrogen phosphate (ADP) mass percent of adding is about 0.23%, and solution temperature is 85 ℃, and the current density that is applied on the aluminium foil is 0.10A/cm
2
Embodiment 3:
Use aluminium content greater than 99.9%, cube texture is greater than 98% 110 micron thickness specific model electronic light paper tinsels, after suitably paper tinsel surface grease is removed in pre-treatment, carry out twice electrochemistry extended surface corrosion: the mass percent of sulfuric acid is 30% in for the first time electrochemical corrosion solution, chlorion adds in the mode of sodium chloride, its mass percent is 6.4%, solution temperature is 75 ℃, and the current density that is applied on the aluminium foil is 0.50A/cm
2The mass percent of for the second time electrochemical corrosion Chlorine in Solution ion is 6.0%, and the calgon mass percent of adding is about 0.21%, and solution temperature is 85 ℃, and the current density that is applied on the aluminium foil is 0.10A/cm
2
Embodiment 4:
Use aluminium content greater than 99.9%, cube texture is greater than 98% 110 micron thickness specific model electronic light paper tinsels, after suitably paper tinsel surface grease is removed in pre-treatment, carry out twice electrochemistry extended surface corrosion: the mass percent of sulfuric acid is 30% in for the first time electrochemical corrosion solution, chlorion adds in the mode of potassium chloride, its mass percent is 8.2%, solution temperature is 75 ℃, and the current density that is applied on the aluminium foil is 0.50A/cm
2The mass percent of for the second time electrochemical corrosion Chlorine in Solution ion is 6.0%, and the sodium polyphosphate mass percent of adding is about 0.20%, and solution temperature is 85 ℃, and the current density that is applied on the aluminium foil is 0.10A/cm
2
Embodiment 5:
Use aluminium content greater than 99.9%, cube texture is greater than 98% 110 micron thickness specific model electronic light paper tinsels, after suitably paper tinsel surface grease is removed in pre-treatment, carry out twice electrochemistry extended surface corrosion: the mass percent of sulfuric acid is 30% in for the first time electrochemical corrosion solution, chlorion adds in the mode of potassium chloride, its mass percent is 8.2%, solution temperature is 75 ℃, and the current density that is applied on the aluminium foil is 0.50A/cm
2The mass percent of for the second time electrochemical corrosion Chlorine in Solution ion is 6.0%, adds mass percent and is about 0.10% sodium polyphosphate+0.10% phosphoric acid, and solution temperature is 85 ℃, and the current density that is applied on the aluminium foil is 0.10A/cm
2
Aluminium foil after finishing through twice galvanic corrosion expansion face among the foregoing description 1～embodiment 5 is cleaned up in 50% concentrated nitric acid, pure water successively, by electron trade standard " SJ/T11140-1997 electrode foil for aluminum electrolytic capacitors " its 590V is tested than electric capacity and physical strength, the gained result is as shown in table 1.
Table 1
| The extended surface method | Than electric capacity % | Than capacitance deviation % | Mechanical strength (returning) |
| Embodiment 1 | 105 | 5 | 59 |
| Embodiment 2 | 105 | 5 | 58 |
| Embodiment 3 | 107 | 6 | 52 |
| Embodiment 4 | 110 | 6 | 53 |
| Embodiment 5 | 117 | 6 | 54 |
Claims (2)
1, a kind of electrochemical corrosive process of anode aluminium foil comprises that twice the anodic etching method expands the face process, is characterized in that:
For the first time electrochemical corrosion extended surface is to carry out in the mixed solution that contains sulfuric acid and chlorion, the electric current that is applied on the aluminium foil is direct current, the mass percent of sulfuric acid is 20%～40% in the mixed solution, the mass percent of chlorion is 1.5%～7.5%, solution temperature is 60 ℃～90 ℃, and the current density that is applied on the aluminium foil is 0.20A/cm
2～0.80A/cm
2
The expansion face of galvanic corrosion for the second time is to carry out in the hydrochloric acid soln that adds inorganic phosphate or inorganic phosphate or both mixtures, the electric current that is applied on the aluminium foil is a direct current, the mass percent of chlorion is 2.0%～10.0% in the mixing solutions, and the current density that is applied on the aluminium foil is 0.05A/cm
2～0.30A/cm
2, solution temperature is 70 ℃～95 ℃, inorganic phosphate that is added or phosphoric acid salt mass percent are 0.01%～1%.
2, the electrochemical corrosive process of anode aluminium foil according to claim 1 is characterized in that: inorganic phosphate or phosphoric acid salt that galvanic corrosion is for the second time expanded in the face mixing solutions are one of phosphoric acid, primary ammonium phosphate, Sodium hexametaphosphate 99, sodium polyphosphate or its mixture.
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| CN 200610124290 CN101029411A (en) | 2006-12-19 | 2006-12-19 | Electrochemical corrosive process of anode aluminum foil |
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|---|---|---|---|
| CN 200610124290 CN101029411A (en) | 2006-12-19 | 2006-12-19 | Electrochemical corrosive process of anode aluminum foil |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101964257A (en) * | 2010-11-04 | 2011-02-02 | 南通华冠电子科技有限公司 | Ultrahigh-pressure anode aluminum foil formation method |
| CN101880906B (en) * | 2009-05-04 | 2012-11-07 | 新疆众和股份有限公司 | Anode foil corrosion method for ultra-high voltage aluminum electrolytic capacitor and electrolyte thereof |
| CN103276435A (en) * | 2013-05-21 | 2013-09-04 | 东莞劲胜精密组件股份有限公司 | Micro-nano processing method for aluminum/aluminum alloy surface and aluminum/ aluminum alloy structure |
| CN103928237A (en) * | 2014-04-25 | 2014-07-16 | 南京工业大学 | Hole expanding process for anode foil of medium-high voltage aluminum electrolytic capacitor |
| CN107123549A (en) * | 2017-04-18 | 2017-09-01 | 扬州宏远电子有限公司 | A kind of pre-treating method for improving solid-state capacitor electrode aluminium foil specific volume |
-
2006
- 2006-12-19 CN CN 200610124290 patent/CN101029411A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880906B (en) * | 2009-05-04 | 2012-11-07 | 新疆众和股份有限公司 | Anode foil corrosion method for ultra-high voltage aluminum electrolytic capacitor and electrolyte thereof |
| CN101964257A (en) * | 2010-11-04 | 2011-02-02 | 南通华冠电子科技有限公司 | Ultrahigh-pressure anode aluminum foil formation method |
| CN103276435A (en) * | 2013-05-21 | 2013-09-04 | 东莞劲胜精密组件股份有限公司 | Micro-nano processing method for aluminum/aluminum alloy surface and aluminum/ aluminum alloy structure |
| CN103276435B (en) * | 2013-05-21 | 2014-08-06 | 东莞劲胜精密组件股份有限公司 | Micro-nano processing method for aluminum/aluminum alloy surface and aluminum/ aluminum alloy structure |
| CN103928237A (en) * | 2014-04-25 | 2014-07-16 | 南京工业大学 | Hole expanding process for anode foil of medium-high voltage aluminum electrolytic capacitor |
| CN107123549A (en) * | 2017-04-18 | 2017-09-01 | 扬州宏远电子有限公司 | A kind of pre-treating method for improving solid-state capacitor electrode aluminium foil specific volume |
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