CN1458658A - Anode aluminium foil etching process for electrolytic capacitor - Google Patents
Anode aluminium foil etching process for electrolytic capacitor Download PDFInfo
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- CN1458658A CN1458658A CN 03126696 CN03126696A CN1458658A CN 1458658 A CN1458658 A CN 1458658A CN 03126696 CN03126696 CN 03126696 CN 03126696 A CN03126696 A CN 03126696A CN 1458658 A CN1458658 A CN 1458658A
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Abstract
The etching process of anode aluminum foil for electrolytic capacitor includes one pre-treatment step. The pretreating solution is solution of alkali, acid or their mixture with Zn and/or Pb compound in 0.0001-1.0 wt% added. Aluminum foil is soaked in the pretreating solution for 10-300 sec, and owing to the separation of Zn and/or Pb, the aluminum foil surface becomes more easy in producing homogeneous spot etching in the fore etching process, and this results in raised area expanding rate, specific capacitance and tensile strength of the aluminum foil.
Description
Technical field
The present invention relates to a kind of corrosion of metals technology, especially relate to a kind of pre-treating method of anode aluminum foil of electrolytic capacitor etching process.
Background technology
Aluminum foil for electrolytic capacitor anode, in order to enlarge its effective surface area, increase the static capacity (specific volume) of unit are, generally carry out chemistry or electrochemical corrosion treatment, it is equally distributed and the etch pit of certain depth is arranged to make its surface form high density, thereby increases the surface area of aluminium foil.The etching process flow process generally comprises following steps: level burn into reprocessing behind pre-treatment, the prime burn into.Pre-treatment is that the light paper tinsel is carried out the various physics of being done before the galvanic corrosion, the processing of chemistry, main effect is greasy dirt, impurity and a natural oxide film of removing aluminium foil surface, adjust the aluminium foil institutional framework, improve its surface state, make even, the activation in its surface, form equally distributed initial voids when being beneficial to the prime corrosion, improve the electric corrosion performance of aluminium foil.Existing research and production reality show that all reasonably pre-treatment can improve light paper tinsel surface state effectively, enlarges the surface area of etched foil significantly, are to improve one of indispensable effective measures of etched foil static specific volume.Existing pre-treating technology is at a certain temperature, with aluminium foil directly in acid or aqueous slkali soaking a few minutes, handle like this and when removing aluminium foil surface greasy dirt and oxide-film, also dissolved the impurity element that the aluminium foil top layer helps sending out the hole, cause the density deficiency and the mechanical strength of corrosion hole skewness, hole to descend.
Summary of the invention
Technical problem to be solved by this invention provides a kind of area expanding rate and static capacity that had both improved anode aluminium foil, does not lose the etching process of the anode aluminum foil of electrolytic capacitor of its mechanical strength simultaneously.
Etching process of the present invention is a pre-treating method of having invented unique anode aluminum foil of electrolytic capacitor etching process, and level was corroded and reprocessing after this anode aluminum foil of electrolytic capacitor etching process comprised pre-treatment, prime burn into.The present invention adds to contain the compound of Zn or Pb or the mixture of above-claimed cpd in the pretreatment liquid of present existing alkali, acid, mixed acid or mixed base, and the percentage by weight that contains Zn or Pb in the pretreatment liquid is 0.0001～1.0%.Above-mentioned pretreatment liquid can be 1～10wt%NaOH solution, 1～10wt%KOH solution, 1～20wt%H
2SO
4Solution, 1～20wt%H
3PO
4Solution, 1～20wt%HNO
3Solution, 1～20wt%HCl solution, 1～20wt%H
3PO
4With the mixed liquor of 0.01～1wt%HF or the mixed liquor of 1～20wt%HCl and 0.01～1wt%HF, but be not limited only to mixed liquor, two or more sour mixed liquor of above-mentioned alkali, acid, two or more alkali.When temperature is 30～90 ℃, aluminium foil soaked 10～300 seconds in above-mentioned pretreatment liquid after, carry out level corrosion and reprocessing behind the common prime burn into again.
The pretreatment liquid treatment temperature is lower than 25 ℃, and aluminium foil surface is not reaction generation almost, the effect that does not have; And surpassing 95 ℃, undue dissolving, the effect that does not also have take place in aluminium foil surface.The pretreatment liquid temperature ranges that the present invention suits is 30～90 ℃, specifically decides according to the composition and the concentration of pretreatment liquid.
The pretreatment liquid processing time is lower than 5 seconds, and aluminium foil surface is not reaction generation almost, the effect that does not reach; But surpass 360 seconds, undue dissolving, the effect that does not also reach take place in aluminium foil surface.The pretreatment liquid processing time that the present invention suits specifically decides according to the Pressure, Concentration, Temperature of pretreatment liquid for being generally 10～300 seconds.
The invention has the beneficial effects as follows that owing to added the compound that contains Zn or Pb or the mixture of two kinds of compounds in the pretreatment liquid, when aluminium foil was carried out pre-treatment, aluminium foil surface was separated out because of Zn or Pb's, helped when prime is corroded the even spot corrosion of easier generation; Improved the corrosion area expanding rate of aluminium foil, than static capacity, and keep its excellent mechanical intensity.
Embodiment
The invention will be further described below in conjunction with embodiment.In this anode aluminum foil of electrolytic capacitor etching process, used aluminium foil be in homemade high-purity aluminum foil, aluminium content 〉=99.99wt% is through vacuum furnace (24 hours annealing in process of 550 ℃ of insulations of vacuum degree≤1.3pa), annealing paper tinsel [100] face occupation rate 〉=95%; The prime corrosive liquid is 30wt%H
2SO
4+ 3wt%HCl, back level corrosive liquid is 3wt%HCl+1.0wt%AlCl
3, treatment fluid is 5wt%HNO
3, again through cleaning, drying.
Comparative Examples the 1,2, the 3rd, three concrete schemes of existing pre-treating technology, used pretreatment liquid all is common alkali or the acid solutions that do not have to add the mixture of the compound contain Zn or Pb or two kinds of compounds, when 40～80 ℃ of temperature, aluminium foil was directly soaked 60～150 seconds in pretreatment liquid, level is corroded and reprocessing the 375V of aluminium foil after carrying out common prime burn into again
fStatic capacity is 0.75～0.81 μ F/cm
2, tensile strength is 20.2～21.4N/cm.
Embodiment 1 is to be after 40 ℃, concentration are to soak 120 seconds in the pretreatment liquid of 5.0wt%NaOH+0.005wt%ZnO with aluminium foil in temperature, carries out level corrosion and reprocessing behind the common prime burn into again.
Embodiment 2 be with aluminium foil be 802 in temperature, concentration is 5.0wt%H
2SO
4Soak in the pretreatment liquid of+0.005wt%PbO after 120 seconds, carry out level corrosion and reprocessing behind the common prime burn into again.
Embodiment 3 is to be that 70 ℃, concentration are 5.0wt%H with aluminium foil in temperature
3PO
4Soak in the pretreatment liquid of+0.005wt%ZnO after 120 seconds, carry out level corrosion and reprocessing behind the common prime burn into again.
Embodiment 4 is to be that 70 ℃, concentration are 5.0wt%H with aluminium foil in temperature
3PO
4Soak in the pretreatment liquid of+0.005wt%ZnO+0.005wt%PbO after 120 seconds, carry out level corrosion and reprocessing behind the common prime burn into again.
Embodiment 5 is to be that 70 ℃, concentration are 5.0wt%H with aluminium foil in temperature
3PO
4Soak in the pretreatment liquid of+0.1wt%HF+0.005wt%ZnO after 120 seconds, carry out level corrosion and reprocessing behind the common prime burn into again.
Embodiment 6 is to be after 70 ℃, concentration are to soak 120 seconds in the pretreatment liquid of 5.0wt%HCl+0.1wt%HF+0.005wt%ZnO+0.005wt%PbO with aluminium foil in temperature, carries out level corrosion and reprocessing behind the common prime burn into again.
Embodiment 1～6th, and part specific embodiments of the present invention after handling through pre-treating technology of the present invention, is carried out level corrosion and reprocessing behind the common prime burn into, the 375V of aluminium foil again
fStatic capacity is 0.90～0.96 μ F/cm
2, tensile strength is 22.1～24.0N/cm, the performance of aluminium foil is significantly improved.
Table 1 is that the detailed numerical value of Comparative Examples and static capacity that embodiment surveys and tensile strength compares.375V in the table 1
fCapacity is meant the static capacity after 375 volts of voltages change into.
Table 1:
Annotate: the capacity among Comparative Examples, the embodiment, tensile strength values are the data according to electronics industry standard SJ/T11140-1997 test promulgated by the ministries or commissions of the Central Government.
| Sample | Pretreatment liquid | Temperature (℃) | Time (second) | ??375V fCapacity (μ F/cm 2) | Tension (N/cm) | |
| Main component | Adding ingredient | |||||
| Comparative Examples 1 | ??5.0wt％NaOH | ????40 | ????60 | ????0.80 | ??21.4 | |
| Comparative Examples 2 | ??5.0wt％H 2SO 4 | ????80 | ??120 | ????0.81 | ??20.2 | |
| Comparative Examples 3 | ??5.0wt％H 3PO 4 | ????70 | ??120 | ????0.75 | ??20.5 | |
| Embodiment 1 | ??5.0wt％NaOH | ??0.005wt％ZnO | ????40 | ??120 | ????0.96 | ??23.1 |
| Embodiment 2 | ??5.0wt％H 2SO 4 | ??0.005wt％PbO | ????80 | ??120 | ????0.92 | ??23.7 |
| Embodiment 3 | ??5.0wt％H 3PO 4 | ??0.005wt％ZnO | ????70 | ??120 | ????0.90 | ??24.0 |
| Embodiment 4 | ??5.0wt％H 3PO 4 | ??0.005wt％ZnO ??+0.005wt％PbO | ????70 | ????120 | ????0.91 | ??22.5 |
| Embodiment 5 | ??5.0wt％H 3PO 4??+0.1wt％HF | ??0.005wt％ZnO | ????70 | ??120 | ????0.93 | ??22.7 |
| Embodiment 6 | ??5.0wt％HCl ??+0.1wt％HF | ??0.005wt％ZnO ??+0.005wt％PbO | ????70 | ??120 | ????0.92 | ??22.1 |
The bulking value that data in the table 1 demonstrate among the embodiment has fully had significant raising than the bulking value in the Comparative Examples, and tensile strength also obviously improves.
Claims (9)
1, a kind of anode aluminum foil of electrolytic capacitor etching process, comprise pre-treatment, it is characterized in that adding contains the compound of Zn or Pb or the mixture of above-claimed cpd in the pretreatment liquid of described pre-treatment, the percentage by weight that contains Zn or Pb in the described pretreatment liquid is 0.0001～1.0wt%.
2, anode aluminum foil of electrolytic capacitor etching process according to claim 1, the percentage by weight that it is characterized in that containing in the described pretreatment liquid Zn or Pb is 0.001～0.025wt%.
3, anode aluminum foil of electrolytic capacitor etching process according to claim 1 and 2 is characterized in that described pretreatment liquid treatment temperature is 30～90 ℃, and the described pretreatment liquid processing time is 10～300 seconds.
4, anode aluminum foil of electrolytic capacitor etching process according to claim 1 and 2 is characterized in that: described pretreatment liquid is NaOH solution, KOH solution, H
2SO
4Solution, H
3PO
4Solution, HNO
3Solution, HCl solution, H
3PO
4With the mixed liquor of HF or the mixed liquor of HCl and HF.
5, anode aluminum foil of electrolytic capacitor etching process according to claim 1 and 2 is characterized in that: described pretreatment liquid is an acid solution, and the pretreatment liquid treatment temperature is 60～85 ℃, and the pretreatment liquid processing time is 40～150 seconds.
6, anode aluminum foil of electrolytic capacitor etching process according to claim 1 and 2 is characterized in that: described pretreatment liquid is an alkaline solution, and the pretreatment liquid treatment temperature is 30～50 ℃, and the pretreatment liquid processing time is 40～150 seconds.
7, anode aluminum foil of electrolytic capacitor etching process according to claim 1 and 2 is characterized in that: described pretreatment liquid is the mixed liquor of at least two kinds of alkali or the mixed liquor of at least two kinds of acid.
8, anode aluminum foil of electrolytic capacitor etching process according to claim 1 and 2 is characterized in that: described pretreatment liquid is that concentration is 1～20wt%H
2SO
4Solution, concentration are 1～20wt%HNO
3Solution, concentration are that 1～20wt%HCl solution, concentration are 1～20wt%H
3PO
4Solution, concentration are 1～20wt%H
3PO
4With the mixed liquor of 0.01～1wt%HF, mixed liquor, the concentration that concentration is 1～20wt%HCl and 0.01～1wt%HF be that 1～10wt%NaOH solution or concentration are 1～10wt%KOH solution.
9, anode aluminum foil of electrolytic capacitor etching process according to claim 1 and 2 is characterized in that: described pretreatment liquid is that concentration is 4～9wt%H
2SO
4Solution, concentration are 3～7wt%H
3PO
4Solution, concentration are 2～9wt%HNO
3Solution, concentration are that 4～10wt%HCl solution, concentration are 3～7wt%H
3PO
4With the mixed liquor of 0.01～1wt%HF, mixed liquor, the concentration that concentration is 4～10wt%HCl and 0.1～1wt%HF be that 1～7wt%NaOH solution or concentration are 1～7wt%KOH solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031266967A CN1333415C (en) | 2003-05-26 | 2003-05-26 | Anode aluminium foil etching process for electrolytic capacitor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031266967A CN1333415C (en) | 2003-05-26 | 2003-05-26 | Anode aluminium foil etching process for electrolytic capacitor |
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| CN1458658A true CN1458658A (en) | 2003-11-26 |
| CN1333415C CN1333415C (en) | 2007-08-22 |
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| CN101976612A (en) * | 2010-11-04 | 2011-02-16 | 南通华冠电子科技有限公司 | Pretreatment method for aluminum foil corrosion |
| CN101425392B (en) * | 2008-07-29 | 2011-06-15 | 东莞市东阳光电容器有限公司 | Pre-treating process for high-voltage aluminum foil corrosion |
| CN102971898A (en) * | 2011-02-10 | 2013-03-13 | 昭和电工株式会社 | Current collector |
| CN103198925A (en) * | 2013-04-28 | 2013-07-10 | 广西贺州市桂东电子科技有限责任公司 | Method for controlling distribution of mesohigh electronic aluminum foil etching holes |
| CN103451713A (en) * | 2013-08-28 | 2013-12-18 | 广西贺州市桂东电子科技有限责任公司 | Corrosion pretreatment method for anode oxidation deposited zinc/tin crystal nucleus of middle-high voltage electronic aluminum foil |
| CN104616898A (en) * | 2014-12-31 | 2015-05-13 | 东莞市长安东阳光铝业研发有限公司 | Method for improving hole production performance of aluminum foil through additional annealing treatment |
| CN109537040A (en) * | 2018-12-31 | 2019-03-29 | 陈建君 | The process of mesohigh Fabrication of High Specific Capacitance aluminium foil corrosion |
| CN110164696A (en) * | 2019-04-12 | 2019-08-23 | 浙江丰川电子科技有限公司 | A kind of electrochemical corrosive process for the production of mesohigh anode foils |
| 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 |
| CN114744208A (en) * | 2022-03-29 | 2022-07-12 | 佛山市中技烯米新材料有限公司 | Current collector etching foil, preparation method thereof, electrode and lithium battery |
Family Cites Families (3)
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| CN1027718C (en) * | 1990-12-11 | 1995-02-22 | 昭和铝株式会社 | Aluminum foil as electrolytic condenser electrodes |
| CN1209496C (en) * | 1998-10-28 | 2005-07-06 | 日本巴卡莱近估股份有限公司 | Composition for metal surface treatment and surface treating liquid and surface treating method |
| JP4071469B2 (en) * | 2001-10-10 | 2008-04-02 | 昭和電工株式会社 | Anode foil for capacitor, method for producing the anode foil, and solid electrolytic capacitor using the anode foil |
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2003
- 2003-05-26 CN CNB031266967A patent/CN1333415C/en not_active Expired - Fee Related
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| CN101425392B (en) * | 2008-07-29 | 2011-06-15 | 东莞市东阳光电容器有限公司 | Pre-treating process for high-voltage aluminum foil corrosion |
| CN101976612A (en) * | 2010-11-04 | 2011-02-16 | 南通华冠电子科技有限公司 | Pretreatment method for aluminum foil corrosion |
| CN102971898A (en) * | 2011-02-10 | 2013-03-13 | 昭和电工株式会社 | Current collector |
| CN102971898B (en) * | 2011-02-10 | 2015-10-07 | 昭和电工株式会社 | Collector body |
| CN103198925B (en) * | 2013-04-28 | 2015-06-17 | 广西贺州市桂东电子科技有限责任公司 | Method for controlling distribution of mesohigh electronic aluminum foil etching holes |
| CN103198925A (en) * | 2013-04-28 | 2013-07-10 | 广西贺州市桂东电子科技有限责任公司 | Method for controlling distribution of mesohigh electronic aluminum foil etching holes |
| CN103451713B (en) * | 2013-08-28 | 2016-01-20 | 广西贺州市桂东电子科技有限责任公司 | The corrosion pretreating method of mesohigh electric aluminum foil anodic oxidation deposition zinc or tin nucleus |
| CN103451713A (en) * | 2013-08-28 | 2013-12-18 | 广西贺州市桂东电子科技有限责任公司 | Corrosion pretreatment method for anode oxidation deposited zinc/tin crystal nucleus of middle-high voltage electronic aluminum foil |
| CN104616898A (en) * | 2014-12-31 | 2015-05-13 | 东莞市长安东阳光铝业研发有限公司 | Method for improving hole production performance of aluminum foil through additional annealing treatment |
| CN104616898B (en) * | 2014-12-31 | 2017-07-07 | 东莞市长安东阳光铝业研发有限公司 | A kind of method that additional annealing treatment improves aluminium foil hair engaging aperture performance |
| CN109537040A (en) * | 2018-12-31 | 2019-03-29 | 陈建君 | The process of mesohigh Fabrication of High Specific Capacitance aluminium foil corrosion |
| CN110164696A (en) * | 2019-04-12 | 2019-08-23 | 浙江丰川电子科技有限公司 | A kind of electrochemical corrosive process for the production of mesohigh anode foils |
| CN110164696B (en) * | 2019-04-12 | 2021-06-22 | 浙江丰川电子环保科技股份有限公司 | Electrochemical corrosion process for producing medium-high voltage anode foil |
| 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 |
| CN114744208A (en) * | 2022-03-29 | 2022-07-12 | 佛山市中技烯米新材料有限公司 | Current collector etching foil, preparation method thereof, electrode and lithium battery |
| CN114744208B (en) * | 2022-03-29 | 2023-02-10 | 佛山市中技烯米新材料有限公司 | Current collector etching foil, preparation method thereof, electrode and lithium battery |
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