CN103187176B - A kind of etching process of anode aluminum foil of electrolytic capacitor - Google Patents
A kind of etching process of anode aluminum foil of electrolytic capacitor Download PDFInfo
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- CN103187176B CN103187176B CN201310093975.9A CN201310093975A CN103187176B CN 103187176 B CN103187176 B CN 103187176B CN 201310093975 A CN201310093975 A CN 201310093975A CN 103187176 B CN103187176 B CN 103187176B
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Abstract
The present invention relates to a kind of method for manufacturing electrode foil, refer in particular to the manufacture method of anode foil for aluminum electrolytic capacitor.Manufacture method of the present invention comprises pre-treatment, communication pre-corrosion, middle chemical treatment, final exchange corrosion, reprocessing five steps, and in AC corrosion process, take ultrasonic wave added corrosion, aluminium foil surface etch pit can be realized be evenly distributed, when supersonic frequency is 40HZ, adopt the aluminium anode foil that this process is formed, than the anode foils adopting traditional corrosion chemical synthesizing method to obtain, ratio capacitance is improved largely, under the prerequisite obtaining Fabrication of High Specific Capacitance, electrode foil has good mechanical strength simultaneously, present invention process method is applicable to the production of various low-voltage aluminum electrolytic capacitor anode foils, technique is simple, easy to operate, cost is low, easy control, large-scale industrial production can be realized.
Description
Technical field
The present invention relates to a kind of aluminum foil corrosion technique method, particularly a kind of etching process of anode aluminum foil of electrolytic capacitor.
Background technology
Along with developing rapidly of electronic industry, the sharply expansion of the produce markets such as computer, communication products and household electrical appliances, also sharply rises to the demand of aluminium electrolytic capacitor.At present, aluminium electrolytic capacitor development trend is miniaturization, chip type, high temperature resistant and long-life, and therefore Fabrication of High Specific Capacitance electrode foil manufacturing technology becomes the key manufacturing high-quality aluminum electrolytic capacitor.Electrode foil is through the electronic product that special corrosion chemical synthesis technology is produced, and its production difficulty is large, (Fabrication of High Specific Capacitance and high strength) with high content of technology, for a long time dependence on import always.Corrosion is the preceding working procedure that Waste Acid From Hua Cheng Foil manufactures.Etched foil specific volume is basis and the key of Waste Acid From Hua Cheng Foil specific volume.Therefore can etching process technology determine the electrode foil that obtain Fabrication of High Specific Capacitance.In corrosion process, often there will be the uneven phenomenon of corrosion, local corrosion is excessive, causes etched foil specific volume not high, various hydraulic performance decline, therefore the etching process of the electrode foil technology paid close attention to of Shi Ge manufacturer always.
Summary of the invention
Technical problem to be solved by this invention is: in prior art, in the corrosion process of aluminium foil, often there will be the phenomenon that corrosion is uneven.
For solving this technical problem, technical scheme provided by the invention is:
The invention provides a kind of etching process of anode aluminum foil of electrolytic capacitor, basic step comprises, pre-treatment, communication pre-corrosion, middle chemical treatment, final exchange corrosion, reprocessing five steps, wherein, in communication pre-corrosion and these two steps of final exchange corrosion, with the addition of ultrasonic wave added means.
As preferably: the supersonic frequency of ultrasonic wave added means is 40KHz,
If supersonic frequency is too low, corrode insufficient, frequency is too high, and corrosion too much causes weightless excessive, affects the mechanical performance of aluminium foil,
The concrete steps of above-mentioned aluminum foil corrosion technique are:
(1) pre-treatment: aluminium foil being placed in temperature is 20 ~ 30 DEG C, concentration is soak l-2min in the NaOH aqueous solution of 2.0-3.0mo1/l, then repeatedly rinses well with distilled water,
Pre-treatment is mainly used in the preliminary treatment of aluminium foil surface, namely removes the greasy dirt of aluminium foil surface, impurity, and natural oxide film, makes aluminium foil surface even, activation, is conducive to forming equally distributed initial pit;
(2) communication pre-corrosion: also referred to as prime AC corrosion, is placed in hybrid corrosion solution by the aluminium foil after pre-treatment, carries out communication pre-corrosion, and hybrid corrosion solution composition is the AlCl of 3.0mol/l hydrochloric acid, 0.75mol/l sulfuric acid, 0.1mol/l
3solution, whole corrosion process completes under ultrasonic wave added, and supersonic frequency is 40KHz, and etchant solution temperature is 40-50 DEG C, and the pre-etching time is 1-2min,
Wherein, communication pre-corrosion here, use voltage is 220V, current density is 0.2A/cm
2, frequency is the alternating current of 50HZ,
Communication pre-corrosion is the committed step of whole etching process, and its main purpose forms the initial pit with certain depth and aperture at aluminium foil surface,
Initial pit in pre-etching, requires that not only position distribution is even, and requires that pore size and the degree of depth are also evenly distributed, under this high request, this invention takes ultrasonic wave added, by means of the advantage of ultrasonic wave uniqueness, the situation that pit is uneven and undesirable can be improved;
(3) intermediate treatment: by the aluminium foil after communication pre-corrosion, in the hybrid corrosion liquid in step (2), processes 2 ~ 5min at 50 ~ 60 DEG C,
Intermediate treatment object is by chemical method, the corrosion deposited film on removing surface, and activation corrosion hole to a certain extent;
(4) final exchange corrosion: by the aluminium foil after step (3) process, be placed in hybrid corrosion liquid and carry out AC corrosion, hybrid corrosion liquid consists of hydrochloric acid, the sulfuric acid of 0.2mol/l, the 0.2mol/lAlCl of 4.5mol/l
3, 0.4mol/l oxalic acid solution, whole AC corrosion process completes under ultrasonic wave added, and supersonic frequency is 40KHz, and etchant solution temperature is 35 ~ 45 DEG C, and the AC corrosion time is 4-5min,
Wherein, final exchange corrosion here, use voltage is 220V, current density is 0.3A/cm
2, frequency is the alternating current of 50HZ,
Final exchange corrosion object carries out reaming on the basis of initial pit, and under the effect of alternating current, on the one hand under the effect of activation-PASSIVATION MECHANISM, corrosion, towards developing in depth and breadth, keeps certain hole passive area simultaneously, maintains the mechanical strength of etched foil,
Final exchange corrosion etching time is longer, solution concentration skewness, can cause corrosion uneven, the measures such as stirring often will be taked to make corrosion evenly, the present invention replaces mechanical agitation with ultrasonic wave added in final exchange corrosion, make surface corrosion evenly;
(5) reprocessing: by the etched foil after step (4) process, be placed in that temperature is 20 ~ 30 DEG C, Solute mass fraction is the HNO of 3%
3soak 30 seconds in solution, then clean by washed with de-ionized water,
Reprocessing object removes the residual chloride ion of aluminium foil surface and metal impurities.
Beneficial effect of the present invention is: in prime and final exchange corrosion process, take ultrasonic wave added effect, and ultrasonic wave is a kind of mechanical oscillation, usually propagates in elastic fluid in the mode of compressional wave, is a kind of mode of propagation of energy.When ultrasonic wave is propagated in corrosive liquid, due to the interaction of ultrasonic wave and corrosive liquid, make corrosion even.If but supersonic frequency is too low, corrode insufficient; Frequency is too high, and corrosion too much causes weightless excessive, affects the mechanical performance of aluminium foil, and the present invention adopts frequency to be the ultrasonic assistant aluminium foil corrosion of 40KHz, and comprehensive effect effectively can improve specific volume, can ensure again the mechanical strength of etched foil.
Embodiment
Many and the paper tinsel for the Xinjiang of 100 μm, further illustrates the present invention:
Embodiment 1
1, pre-treatment
Solution: 2mol/lNaOH
Temperature: 25 DEG C
Time: 1 minute
2, communication pre-corrosion
Solution: the sulfuric acid+0.1mol/lAlCl of 3.0mol/l hydrochloric acid+0.75mol/l
3
Temperature: 50 DEG C
Alternating current: voltage 220V, current density 0.2A/cm
2, frequency 50HZ
Time: 1 minute
Whole process completes under ultrasonic wave added effect, supersonic frequency 40KHz.
3, intermediate treatment
Solution: the sulfuric acid+0.1mol/lAlCl of 3.0mol/l hydrochloric acid+0.75mol/l
3
Temperature: 50 DEG C
Time: 2 minutes
4, final exchange corrosion
Solution: the sulfuric acid+0.2mol/lAlCl of 4.5mol/l hydrochloric acid+0.2mol/
3+ 0.4mol/l oxalic acid
Temperature: 45 DEG C
Alternating current: voltage 220V, current density 0.3A/cm
2, frequency 50HZ
Time: 4 minutes
Whole process completes under ultrasonic wave added effect, supersonic frequency 40KHz.
5, reprocessing
Solution: mass fraction is 3%HNO
3
Time: 30 seconds
Temperature: room temperature
It is after immersion completes, clean by washed with de-ionized water,
The present invention changes into condition
Adopt WWL-LDX11 precision linear DC current regulator power supply, formation voltage V
fefor 20V, current density is 0.25A/cm
2, temperature is 85 DEG C, and foil samples, as anode, is placed in the ammonium adipate aqueous solution (ammonium adipate 150g, pure water 850g) that mass fraction is 15%, and form groove as negative electrode, oxidization time is 10min.
Embodiment 2
1, pre-treatment
Solution: 2.5mol/lNaOH
Temperature: 25 DEG C
Time: 2 minutes
2, communication pre-corrosion
Solution: the sulfuric acid+0.1mol/lAlCl of 3.0mol/l hydrochloric acid+0.75mol/l
3
Temperature: 45 DEG C
Alternating current: voltage 220V, current density 0.2A/cm
2, frequency 50HZ
Time: 1.5 minutes
Whole process completes under ultrasonic wave added effect, supersonic frequency 40KHz.
3, intermediate treatment
Solution: the sulfuric acid+0.1mol/lAlCl of 3.0mol/l hydrochloric acid+0.75mol/l
3
Temperature: 55 DEG C
Time: 5 minutes
4, final exchange corrosion
Solution: the sulfuric acid+0.2mol/lAlCl of 4.5mol/l hydrochloric acid+0.2mol/
3+ 0.4mol/l oxalic acid
Temperature: 40 DEG C
Alternating current: voltage 220V, current density 0.3A/cm
2, frequency 50HZ
Time: 4.5 minutes
Whole process completes under ultrasonic wave added effect, supersonic frequency 40KHz.
5, reprocessing
Solution: mass fraction is 3%HNO
3
Time: 30 seconds
Temperature: room temperature
It is after immersion completes, clean by washed with de-ionized water,
The present invention changes into condition
Adopt WWL-LDX11 precision linear DC current regulator power supply, formation voltage V
fefor 20V, current density is 0.25A/cm
2, temperature is 85 DEG C, and foil samples, as anode, is placed in the ammonium adipate aqueous solution (ammonium adipate 150g, pure water 850g) that mass fraction is 15%, and form groove as negative electrode, oxidization time is 10min.
Embodiment 3
1, pre-treatment
Solution: 3mol/lNaOH
Temperature: 25 DEG C
Time: 1 minute
2, communication pre-corrosion
Solution: the sulfuric acid+0.1mol/lAlCl of 3.0mol/l hydrochloric acid+0.75mol/l
3
Temperature: 40 DEG C
Alternating current: voltage 220V, current density 0.2A/cm
2, frequency 50HZ
Time: 2 minutes
Whole process completes under ultrasonic wave added effect, supersonic frequency 40KHz.
3, intermediate treatment
Solution: the sulfuric acid+0.1mol/lAlCl of 3.0mol/l hydrochloric acid+0.75mol/l
3
Temperature: 60 DEG C
Time: 3 minutes
4, final exchange corrosion
Solution: the sulfuric acid+0.2mol/lAlCl of 4.5mol/l hydrochloric acid+0.2mol/
3+ 0.4mol/l oxalic acid
Temperature: 35 DEG C
Alternating current: voltage 220V, current density 0.3A/cm
2, frequency 50HZ
Time: 5 minutes
Whole process completes under ultrasonic wave added effect, supersonic frequency 40KHz.
5, reprocessing
Solution: mass fraction is 3%HNO
3
Time: 30 seconds
Temperature: room temperature
It is after immersion completes, clean by washed with de-ionized water,
The present invention changes into condition
Adopt WWL-LDX11 precision linear DC current regulator power supply, formation voltage V
fefor 20V, current density is 0.25A/cm
2, temperature is 85 DEG C, and foil samples, as anode, is placed in the ammonium adipate aqueous solution (ammonium adipate 150g, pure water 850g) that mass fraction is 15%, and form groove as negative electrode, oxidization time is 10min.
Comparative example 1:
The present embodiment is at communication pre-corrosion and final exchange corrosion, and in these two steps, do not adopt any supplementary means (do not adopt ultrasonic wave added means, also do not adopt mechanical agitation means), all the other experiment conditions are all identical with embodiment 1.
Comparative example 2:
The present embodiment is at communication pre-corrosion and final exchange corrosion, and in these two steps, do not adopt ultrasonic wave added means, but have employed mechanical agitation means, stir speed (S.S.) 200r/min, all the other experiment conditions are all identical with embodiment 1.
Comparative example 3:
The present embodiment is at communication pre-corrosion and final exchange corrosion, and in these two steps, the ultrasonic wave added means of employing, supersonic frequency is 30KHz, and all the other experiment conditions are all identical with embodiment 1.
Comparative example 4:
The present embodiment is at communication pre-corrosion and final exchange corrosion, and in these two steps, the ultrasonic wave added means of employing, supersonic frequency is 35KHz, and all the other experiment conditions are all identical with embodiment 1.
Comparative example 5:
The present embodiment is at communication pre-corrosion and final exchange corrosion, and in these two steps, the ultrasonic wave added means of employing, supersonic frequency is 45KHz, and all the other experiment conditions are all identical with embodiment 1.
Comparative example 6:
The present embodiment is at communication pre-corrosion and final exchange corrosion, and in these two steps, the ultrasonic wave added means of employing, supersonic frequency is 50KHz, and all the other experiment conditions are all identical with embodiment 1.
Respectively performance test is carried out to the Waste Acid From Hua Cheng Foil of each embodiment above, the specific volume of main test aluminium foil and tensile strength, aluminium foil after changing into is cut into the sample of 1cm × 5cm, respectively by specific volume and the tensile strength of JK2911LCR digital electric bridge and WDW-10 electronic universal tester test aluminium foil
Specific volume determination step is as follows: using anode foils as positive pole, stainless steel electrode is as negative pole, be placed in constant temperature and measure groove, in groove, solution is ammonium adipate solution (ammonium adipate 150g, pure water 850g), connect with the mains, from JK2911LCR digital electric bridge, read capacitance value can (unit are specific volume need divided by 5);
Load on clamp of stretching tester by test film during tensile strength test, rate of extension remains on 10 ± 1mm/min, and measure pulling force during fracture, single pass test repeats 5 times and averages.
Test result is listed in the following table:
Above result display: by taking ultrasonic wave added in aluminium foil corrosion process, when ultrasonic frequency is 40HZ, aluminium foil obtains best ratio capacitance and tensile strength.
Claims (1)
1. the etching process of an anode aluminum foil of electrolytic capacitor, it is characterized in that: described etching process comprises five steps, be respectively pre-treatment, communication pre-corrosion, middle chemical treatment, final exchange corrosion and reprocessing, wherein, in communication pre-corrosion and these two steps of final exchange corrosion, with the addition of ultrasonic wave added means
The concrete steps of described technique are
(1) pre-treatment: aluminium foil being placed in temperature is 20 ~ 30 DEG C, concentration is soak l-2min in the NaOH aqueous solution of 2.0-3.0mo1/l, then repeatedly rinses well with distilled water;
(2) communication pre-corrosion: the aluminium foil after pre-treatment is placed in hybrid corrosion solution, carries out communication pre-corrosion, and hybrid corrosion solution composition is the AlCl of 3.0mol/l hydrochloric acid, 0.75mol/l sulfuric acid, 0.1mol/l
3solution, whole corrosion process completes under ultrasonic wave added, and supersonic frequency is 40KHz, and etchant solution temperature is 40-50 DEG C, and the pre-etching time is 1-2min,
Described communication pre-corrosion, use voltage is 220V, current density is 0.2A/cm
2, frequency is the alternating current of 50HZ;
(3) intermediate treatment: by the aluminium foil after communication pre-corrosion, in the hybrid corrosion liquid in step (2), processes 2 ~ 5min at 50 ~ 60 DEG C;
(4) final exchange corrosion: by the aluminium foil after step (3) process, be placed in hybrid corrosion liquid and carry out AC corrosion, hybrid corrosion liquid consists of hydrochloric acid, the sulfuric acid of 0.2mol/l, the 0.2mol/lAlCl of 4.5mol/l
3, 0.4mol/l oxalic acid solution, whole AC corrosion process completes under ultrasonic wave added, and supersonic frequency is 40KHz, and etchant solution temperature is 35 ~ 45 DEG C, and the AC corrosion time is 4-5min,
Described final exchange corrosion, use voltage is 220V, current density is 0.3A/cm
2, frequency is the alternating current of 50HZ;
(5) reprocessing: by the etched foil after step (4) process, be placed in that temperature is 20 ~ 30 DEG C, Solute mass fraction is the HNO of 3%
3soak 30 seconds in solution, then clean by washed with de-ionized water.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105420803A (en) * | 2015-11-27 | 2016-03-23 | 广西贺州市桂东电子科技有限责任公司 | Method for ultrasonic-assisted corrosion of middle-high voltage anode aluminum foil |
| CN105401209B (en) * | 2015-12-09 | 2018-03-30 | 广西贺州市桂东电子科技有限责任公司 | A kind of method of mesohigh anodic aluminum corrosion processing |
| CN105551805B (en) * | 2016-01-18 | 2018-01-12 | 南通海星电子股份有限公司 | The middle processing method of medium-high voltage aluminum electrolytic capacitor electrode foil |
| CN105862116A (en) * | 2016-04-10 | 2016-08-17 | 江苏荣生电子有限公司 | Method for manufacturing energy storage foil by utilizing ultrasonic treatment |
| CN106001111A (en) * | 2016-05-18 | 2016-10-12 | 北京科技大学 | Micro-forming rolling technology preparing high-specific-volume aluminum foil electrode |
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| CN109628979A (en) * | 2018-12-20 | 2019-04-16 | 宝兴县华锋储能材料有限公司 | A kind of manufacturing method of extremely low pressure Fabrication of High Specific Capacitance Waste Acid From Hua Cheng Foil |
| CN110048126B (en) * | 2019-03-24 | 2020-10-16 | 藤县加裕电子科技有限公司 | Manufacturing process of aluminum foil and positive current collector |
| CN110257893A (en) * | 2019-05-29 | 2019-09-20 | 安徽省临泉县康悦电子科技有限公司 | A kind of aluminum foil corrosion technique |
| CN110783110A (en) * | 2019-11-07 | 2020-02-11 | 南通海星电子股份有限公司 | Method for manufacturing electrode foil for solid-state capacitor |
| CN111508713A (en) * | 2020-03-11 | 2020-08-07 | 恒扬（韶关）工业有限公司 | Low-voltage aluminum foil corrosion process for aluminum electrolytic capacitor |
| CN112981516B (en) * | 2021-02-03 | 2022-04-05 | 广州金立电子有限公司 | Anode aluminum foil corrosion method for aluminum electrolytic capacitor |
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