CN104630871B - A kind of etching process method of low pressure hard Fabrication of High Specific Capacitance aluminum electric pole foil - Google Patents
A kind of etching process method of low pressure hard Fabrication of High Specific Capacitance aluminum electric pole foil Download PDFInfo
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Abstract
The present invention relates to a kind of etching process method of low pressure hard Fabrication of High Specific Capacitance aluminum electric pole foil, belong to aluminium foil manufacturing technology field.This method determines frequency power with the constant-current type of PWM control technologies and provides electrochemical corrosion power, the corrosion process of low pressure aluminum electric pole foil is divided into three different technology conditions to complete, it is the new pitting corrosion of burn into depth reaming burn into of layouting respectively, aluminium foil more than after three corrosion, it can obtain within etching extent 10mg every square centimeter, specific volume reaches Fabrication of High Specific Capacitance, the low pressure corroding electrode paper tinsels of performance brilliance more than 75 μ F/cm2.
Description
Technical field
The present invention relates to a kind of etching process method of aluminum electric pole foil, and in particular to a kind of low pressure hard Fabrication of High Specific Capacitance aluminium electrode
The etching process method of paper tinsel, belongs to aluminium foil manufacturing technology field.
Background technology
In electrolytic capacitor family, aluminium electrolutic capacitor is superior, cheap, the widely used basis member of performance
Part, is worldwide greatly developed over nearly 20 years, in large quantities applied to household electrical appliance, computer, communication, industry control
In system, electric automobile, electric locomotive and military and aerospace equipment.For over ten years, the output sustainable growth of global capacitor, and
Aluminium electrolutic capacitor maintains the status that it accounts for whole three/the last mono- of capacitor market, and its annual growth is stably held in 4-
6%.Electrode foil is the main raw material(s) of aluminium electrolutic capacitor, is technology content and added value highest part, electrode foil manufacturing industry
State of development directly influence the development of aluminium electrolutic capacitor industry.Japan is the maximum production of global capacitor aluminium pole paper tinsel
And consumption market, more than the 75% of global yield was once reached during Japanese aluminium electrolutic capacitor yield highest, at present Japan's aluminium electroloysis
The yield of capacitor still reaches world wide production more than 40%, and existing most of yield is transferred to China's Mainland, thus, with aluminium electroloysis
The electrode foil of capacitor synchronized development has the very big market space.Miniaturization, chip type aluminium electrolutic capacitor are to give priority to
One of product, therefore Fabrication of High Specific Capacitance low-field electrode paper tinsel be low-voltage foil from now on development priority.
The capacity of capacitor is directly proportional to the dielectric constant and electrode area S of medium, is inversely proportional with electrode spacing d.
The medium of aluminium electrolutic capacitor is aluminum oxide film layer, and dielectric constant and electrode spacing d are secured via the film layer, therefore it holds
The size of amount derives from electrode area S size.The manufacturing process of electrode foil for aluminum electrolytic capacitors is divided into corrosion process
And formation process, corrosion process is to expand electrode area S among these, and formation process is superficial growth aluminum oxidation film.Low pressure
The corrosion process of aluminum electric pole foil is mainly aluminium foil in the corrosive liquid based on hydrochloric acid, applies alternating current and carries out part
Electrochemical corrosion, forms the surface of cavernous body, realizes largest surface area.
The corrosion process of low pressure aluminum electric pole foil generally comprises three technical elements：One is the power supply spy for participating in electrochemical reaction
Property, two be raw material light foil-like state, three be corrosion electrochemistry reaction technological parameter.The caustic solution of low pressure aluminum electric pole foil
Since the sixties in last century, switched to exchange galvano-cautery by direct current corrosion, to now with two kinds of corrosion technologies：One is power frequency
Power supply, hard light paper tinsel, the process of highly acidity normal temperature；Another is frequency conversion（10—35Hz）Power supply, soft smooth paper tinsel, Low acid are low
The process of temperature.
Former corrosion technology is also referred to as power frequency corrosion technology, and its feature shows as that there is provided the electricity of electrochemical corrosion power
Source is power frequency supply, i.e., directly with adjustable variable-pressure device by civil power become low-voltage and high-current, frequency it is constant（50Hz）Friendship
Flow electricity output；In terms of raw material light paper tinsel just can be used after being cold rolled to paillon foil using hard light paper tinsel, i.e. aluminium sheet；In technique
It is highly acidity hydrochloric acid in terms of parameter（20wt%）For main body corrosive liquid, corrode in two times（Cloth spot corrosion and deep erosions）Come
Into, during each fluid temperature it is general at 36 DEG C or so.
Latter corrosion technology is also referred to as converter technique, and its feature is shown as, and power supply used is low-frequency variable-frequency power sources,
It will first be changed into 10-35Hz exchange electricity output behind commercial power rectification again, participate in electrochemical reaction；Raw material light paper tinsel is medium-soft state
Aluminium foil, i.e., form cold rolling good hard light paper tinsel in vacuum, 300 DEG C or so lower annealing a few hours；Corrosive liquid is low with 10wt%
Acidity hydrochloric acid is cryogenic conditions typically at 20 DEG C or so of main body, temperature, point multistage（Ten grades or so）, according to per one-level state
Corrosion process is completed from different supply frequency and temperature.
In power frequency corrosion technology, used power frequency supply is although simple in construction, but there is also control accuracy it is very poor, hand over
The problem of wave distortion is big is flowed, also because wave distortion, causes product electrode aluminium foil to be not readily available higher specific volume.And becoming
In frequency corrosion technology, use the equipment investment of variable-frequency power sources big, high to use environment requirement, cause the cost of product also high.
In addition, in multistage corrosion process, before every grade of supply frequency selection, height setting of current density size, temperature etc. are required
Closely, the process condition range being applicable is narrow for the cooperation of rear class.In the environment of the keen competition of market, too high sets
Standby expense input is that unadvisable and follow-up maintenance cost is also quite huge, but the production of power frequency supply and corrosion technology
Product also have a small amount of Existential Space in stability and the advanced demand for being difficult to meet client only in cost.
Chinese invention " electrolytic capacitor low impedance anode aluminum foil erosion method and its chemical processing fluid ", application number
200610201482.2 disclosing a kind of method for preparing Low ESR anode aluminum foil of electrolytic capacitor, chemical attack is used.
The content of the invention
It is an object of the invention to provide a kind of etching process method of low pressure hard Fabrication of High Specific Capacitance aluminum electric pole foil, with PWM controls
The constant-current type of technology determines frequency power and provides electrochemical corrosion power, and the corrosion process of low pressure aluminum electric pole foil is divided into three different process
Condition is completed, and can obtain the remarkable product of Fabrication of High Specific Capacitance, performance.
To realize the purpose of foregoing invention, the technical scheme that the present invention takes is as follows：
A kind of etching process method of low pressure hard Fabrication of High Specific Capacitance aluminum electric pole foil, comprises the following steps：
（1）Cloth spot corrosion：First the aluminium foil after oil removal treatment is soaked 30 ~ 60 seconds in corrosive liquid of layouting, then
0.3A/cm2 current densities are imposed, 12 ~ 20 seconds action time, temperature maintains 35 ~ 45 DEG C；
（2）Depth reaming is corroded：In step（1）Cloth spot corrosion carries out deep erosions on the basis of producing spot corrosion, along with
The expansion corrosion of pit, temperature maintains 30 ~ 35 DEG C, average 0.15A/cm2 current densities, action time is imposed in power-up procedures
300 ~ 400 seconds；
（3）New pitting corrosion：In step（2）Under depth reaming corrosiveness, the pit of formation has certain aperture and depth
On the basis of, then corroded with larger current density, a large amount of new bore are produced, the electrode foil compared with Fabrication of High Specific Capacitance is obtained；
（4）Post processing：Aluminium foil more than after three corrosion, is cleaned, is dried, obtained every in a conventional manner
Square centimeter etching extent 10mg within, specific volume reach more than 75 μ F/cm2, the low pressure corroding electrode paper tinsel of function admirable.
The electric current by PWM control technologies constant-current type, determine frequency 50Hz power supplys and provide；
The main body of described corrosive liquid of layouting is made up of 18wt% hydrochloric acid, 0.8wt% sulfuric acid；
Described depth reaming corrosive liquid be by 20wt% hydrochloric acid, 1.2wt% sulfuric acid, 6g/L oxalic acid, 300mg/L thiocarbamides,
150mg/L iron chloride is constituted；
Described new bore corrosive liquid is formulated with cloth spot corrosion, and temperature maintains 25 ~ 35 DEG C, imposes 0.27A/cm2 electric currents
Density, 110 ~ 130 seconds action time.
Variable-frequency power sources：Variable-frequency power sources is address general at home, more precisely, it should be alternating electromotive force frequency conversion
Device, i.e. Ac power Frequency Converter are general to be called with abbreviation AFC.Suitable for the corrosion of low pressure aluminum electric pole foil
Variable-frequency power sources have output frequency low（10-35Hz）And continuously adjustabe, high current（3000A or so）, therefore involve great expense.
PWM：Pulse width modulation, English name Pulse Width Modulation.
Etching extent：The part that aluminium foil participates in electrochemical reaction and is corroded, removes, i.e. unit light paper tinsel weight subtracts completion
Weight after corrosion process.
The beneficial effects of the invention are as follows：Using PWM control technologies constant-current type surely frequency（50Hz）Power supply, can be solved into very well
The problem of in terms of sheet, precision, properties of product；In etching process, hard light paper tinsel, highly acidity, normal temperature are chosen（30 DEG C of left sides
It is right）, in three times corrode, the low pressure aluminum electric pole foil that product is stable, performance specific volume is high can be obtained；Three corrosion are burn into of layouting
Depth reaming is corroded and new pitting corrosion, can efficiently solve that specific volume in power frequency corrosion technology is high, in frequency conversion corrosion technology because
Multistage cooperation and the problems such as the small technique scope of application；In whole etching extent, cloth spot corrosion accounts for 1-5%, depth reaming corrosion
50-70% is accounted for, and new pitting corrosion accounts for 25-35%.Under less equipment investment, relatively low operation and maintenance cost, with reference to corrosion work
Skill is changed, minimal thickness electrode foil specific volume, high thickness electrode foil and frequency conversion corrosion skill as frequency conversion corrosion technology in can obtaining
Effect of the art close to specific volume.
Brief description of the drawings
Fig. 1 is process chart.
Embodiment
The present invention is described in further details below by example, these examples are only used for illustrating the present invention, do not limit
The scope of the present invention processed.
Embodiment 1
A kind of etching process method of low pressure hard Fabrication of High Specific Capacitance aluminum electric pole foil, comprises the following steps：
1. cloth spot corrosion：Domestic 95 μm of hard light paper tinsels after oil removal treatment are first soaked 45 in corrosive liquid of layouting
Second, then impose 0.3A/cm2 current densities, 16 seconds action time, the composition main body of corrosive liquid of layouting be 18wt% hydrochloric acid,
0.8wt% sulfuric acid, temperature maintains 40 DEG C；
2. depth reaming is corroded：Deep erosions are carried out on the basis of preceding working procedure produces spot corrosion, along with the expansion of pit
Big corrosion, the composition main body of corrosive liquid is 20wt% hydrochloric acid, 1.2wt% sulfuric acid, also add 6g/L oxalic acid, 300mg/L thiocarbamides,
150mg/L iron chloride, temperature maintains 33 DEG C, and average 0.15A/cm2 current densities, action time 360 are imposed in power-up procedures
Second；
3. new pitting corrosion：Under preceding working procedure effect, the pit of formation has on the basis of certain aperture and depth, then with
Larger current density is corroded, and is produced a large amount of new bore, is obtained the electrode foil compared with Fabrication of High Specific Capacitance, is equally formulated with " cloth spot corrosion "
Liquid, temperature maintains 30 DEG C, imposes 0.27A/cm2 current densities, 120 seconds action time；
4. the aluminium foil more than after three corrosion, is cleaned according to conventional post processing mode, is dried, can be obtained
Within etching extent 10mg every square centimeter, specific volume reach more than 75 μ F/cm2, the low pressure corroding electrode paper tinsel of function admirable.
Embodiment 2
A kind of etching process method of low pressure hard Fabrication of High Specific Capacitance aluminum electric pole foil, comprises the following steps：
1. cloth spot corrosion：Domestic 95 μm of hard light paper tinsels after oil removal treatment are first soaked 30 in corrosive liquid of layouting
Second, then impose 0.3A/cm2 current densities, 12 seconds action time, the composition main body of corrosive liquid of layouting be 18wt% hydrochloric acid,
0.8wt% sulfuric acid, temperature maintains 35 DEG C；
2. depth reaming is corroded：Deep erosions are carried out on the basis of preceding working procedure produces spot corrosion, along with the expansion of pit
Big corrosion, the composition main body of corrosive liquid is 20wt% hydrochloric acid, 1.2wt% sulfuric acid, also add 6g/L oxalic acid, 300mg/L thiocarbamides,
150mg/L iron chloride, temperature maintains 30 DEG C, and average 0.15A/cm2 current densities, action time 300 are imposed in power-up procedures
Second；
3. new pitting corrosion：Under preceding working procedure effect, the pit of formation has on the basis of certain aperture and depth, then with
Larger current density is corroded, and is produced a large amount of new bore, is obtained the electrode foil compared with Fabrication of High Specific Capacitance, is equally formulated with " cloth spot corrosion "
Liquid, temperature maintains 25 DEG C, imposes 0.27A/cm2 current densities, 110 seconds action time；
4. post processing：Aluminium foil more than after three corrosion, is cleaned, is dried, can be obtained in a conventional manner
Within etching extent 10mg every square centimeter, specific volume reach more than 75 μ F/cm2, the low pressure corroding electrode paper tinsel of function admirable.
Embodiment 3
A kind of etching process method of low pressure hard Fabrication of High Specific Capacitance aluminum electric pole foil, comprises the following steps：
1. cloth spot corrosion：Domestic 95 μm of hard light paper tinsels after oil removal treatment are first soaked 60 in corrosive liquid of layouting
Second, then impose 0.3A/cm2 current densities, 20 seconds action time, the composition main body of corrosive liquid of layouting be 18wt% hydrochloric acid,
0.8wt% sulfuric acid, temperature maintains 45 DEG C；
2. depth reaming is corroded：Deep erosions are carried out on the basis of preceding working procedure produces spot corrosion, along with the expansion of pit
Big corrosion, the composition main body of corrosive liquid is 20wt% hydrochloric acid, 1.2wt% sulfuric acid, also add 6g/L oxalic acid, 300mg/L thiocarbamides,
150mg/L iron chloride, temperature maintains 35 DEG C, and average 0.15A/cm2 current densities, action time 400 are imposed in power-up procedures
Second；
3. new pitting corrosion：Under preceding working procedure effect, the pit of formation has on the basis of certain aperture and depth, then with
Larger current density is corroded, and is produced a large amount of new bore, is obtained the electrode foil compared with Fabrication of High Specific Capacitance, is equally formulated with " cloth spot corrosion "
Liquid, temperature maintains 35 DEG C, imposes 0.27A/cm2 current densities, 130 seconds action time；
4. post processing：Aluminium foil more than after three corrosion, is cleaned, is dried, can be obtained in a conventional manner
Within etching extent 10mg every square centimeter, specific volume reach more than 75 μ F/cm2, the low pressure corroding electrode paper tinsel of function admirable.
Embodiment 4
A kind of etching process method of low pressure hard Fabrication of High Specific Capacitance aluminum electric pole foil, comprises the following steps：
1. cloth spot corrosion：Domestic 95 μm of hard light paper tinsels after oil removal treatment are first soaked 40 in corrosive liquid of layouting
Second, then impose 0.3A/cm2 current densities, 14 seconds action time, the composition main body of corrosive liquid of layouting be 18wt% hydrochloric acid,
0.8wt% sulfuric acid, temperature maintains 38 DEG C；
2. depth reaming is corroded：Deep erosions are carried out on the basis of preceding working procedure produces spot corrosion, along with the expansion of pit
Big corrosion, the composition main body of corrosive liquid is 20wt% hydrochloric acid, 1.2wt% sulfuric acid, also add 6g/L oxalic acid, 300mg/L thiocarbamides,
150mg/L iron chloride, temperature maintains 32 DEG C, and average 0.15A/cm2 current densities, action time 330 are imposed in power-up procedures
Second；
3. new pitting corrosion：Under preceding working procedure effect, the pit of formation has on the basis of certain aperture and depth, then with
Larger current density is corroded, and is produced a large amount of new bore, is obtained the electrode foil compared with Fabrication of High Specific Capacitance, is equally formulated with " cloth spot corrosion "
Liquid, temperature maintains 28 DEG C, imposes 0.27A/cm2 current densities, 115 seconds action time；
4. post processing：Aluminium foil more than after three corrosion, the aluminium foil more than after three corrosion, more than
Three times corrosion after aluminium foil, cleaned, dried in a conventional manner, can obtain etching extent 10mg every square centimeter with
Interior, specific volume reaches more than 75 μ F/cm2, the low pressure corroding electrode paper tinsel of function admirable.
Embodiment 5
A kind of etching process method of low pressure hard Fabrication of High Specific Capacitance aluminum electric pole foil, comprises the following steps：
1. cloth spot corrosion：Domestic 95 μm of hard light paper tinsels after oil removal treatment are first soaked 50 in corrosive liquid of layouting
Second, then impose 0.3A/cm2 current densities, 18 seconds action time, the composition main body of corrosive liquid of layouting be 18wt% hydrochloric acid,
0.8wt% sulfuric acid, temperature maintains 42 DEG C；
2. depth reaming is corroded：Deep erosions are carried out on the basis of preceding working procedure produces spot corrosion, along with the expansion of pit
Big corrosion, the composition main body of corrosive liquid is 20wt% hydrochloric acid, 1.2wt% sulfuric acid, also add 6g/L oxalic acid, 300mg/L thiocarbamides,
150mg/L iron chloride, temperature maintains 34 DEG C, and average 0.15A/cm2 current densities, action time 380 are imposed in power-up procedures
Second；
3. new pitting corrosion：Under preceding working procedure effect, the pit of formation has on the basis of certain aperture and depth, then with
Larger current density is corroded, and is produced a large amount of new bore, is obtained the electrode foil compared with Fabrication of High Specific Capacitance, is equally formulated with " cloth spot corrosion "
Liquid, temperature maintains 33 DEG C, imposes 0.27A/cm2 current densities, 125 seconds action time；
4. post processing：Aluminium foil more than after three corrosion, is cleaned, is dried, can be obtained in a conventional manner
Within etching extent 10mg every square centimeter, specific volume reach more than 75 μ F/cm2, the low pressure corroding electrode paper tinsel of function admirable.
The etching extent of each step should make adjustment according to light paper tinsel thickness and application purpose, to reach optimum efficiency.
Claims (2)
1. a kind of etching process method of low pressure hard Fabrication of High Specific Capacitance aluminum electric pole foil, it is characterised in that：Comprise the following steps：
（1）Cloth spot corrosion：First the aluminium foil after oil removal treatment is soaked 30 ~ 60 seconds in corrosive liquid of layouting, then imposed
0.3A/cm2 current densities, 12 ~ 20 seconds action time, temperature maintains 35 ~ 45 DEG C；
（2）Depth reaming is corroded：In step（1）Cloth spot corrosion carries out deep erosions on the basis of producing spot corrosion, along with pit
Expansion corrosion, temperature maintains 30 ~ 35 DEG C, imposes average 0.15A/cm2 current densities in power-up procedures, action time 300 ~
400 seconds；
（3）New pitting corrosion：In step（2）Under depth reaming corrosiveness, the pit of formation has the base of certain aperture and depth
On plinth, then corroded with larger current density, produce a large amount of new bore, obtain the electrode foil compared with Fabrication of High Specific Capacitance；
（4）Post processing：Aluminium foil more than after three corrosion, is cleaned, is dried, obtained at every square in a conventional manner
Centimetre etching extent 10mg within, specific volume reach more than 75 μ F/cm2, the low pressure corroding electrode paper tinsel of function admirable；
The electric current by PWM control technologies constant-current type, determine frequency 50Hz power supplys and provide.
2. a kind of etching process method of low pressure hard Fabrication of High Specific Capacitance aluminum electric pole foil according to claim 1, it is characterised in that：
Step（1）The main body of described corrosive liquid of layouting is made up of 18wt% hydrochloric acid, 0.8wt% sulfuric acid；
Step（2）Described depth reaming corrosive liquid is by 20wt% hydrochloric acid, 1.2wt% sulfuric acid, 6g/L oxalic acid, 300mg/L sulphur
Urea, 150mg/L iron chloride are constituted；
Step（3）The corrosive liquid formula of described new pitting corrosion is with cloth spot corrosion, and temperature maintains 25 ~ 35 DEG C, imposes
0.27A/cm2 current densities, 110 ~ 130 seconds action time.
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| CN108977875A (en) * | 2018-07-04 | 2018-12-11 | 山西沃特海默新材料科技股份有限公司 | A kind of the electrochemical corrosion preparation method and its micropore copper foil of micropore battery copper foil |
| 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 |
| CN111519239B (en) * | 2020-05-18 | 2021-12-07 | 南通海星电子股份有限公司 | Etching method for ultrahigh-pressure etched foil |
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| US4474657A (en) * | 1983-12-20 | 1984-10-02 | North American Philips Corporation | Single step electro chemical etch process for high volt aluminum anode foil |
| US4518471A (en) * | 1984-08-29 | 1985-05-21 | North American Philips Corporation | Two step electrochemical etch process for high volt aluminum anode foil |
| CN1090687C (en) * | 1999-06-25 | 2002-09-11 | 四川大学 | Low-pressure anode aluminium foil face-expanding erosion method |
| CN100511517C (en) * | 2005-06-06 | 2009-07-08 | 肇庆华锋电子铝箔有限公司 | Variable frequency corrosion method of low-voltage anode foil for electrolytic capacitor |
| CN101211696B (en) * | 2006-12-30 | 2011-06-22 | 新疆众和股份有限公司 | Electrolytic capacitor low impedance anode aluminum foil erosion method and its chemical processing fluid |
| CN101275269B (en) * | 2008-04-22 | 2010-09-22 | 日丰（清远）电子有限公司 | Etching Process of Aluminum Foil for Electrolytic Capacitor |
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Address after: 526060 Duanzhou Industrial City, Duanzhou District, Zhaoqing City, Guangdong Province Co-patentee after: Zhaoqing Gaoyao Huafeng Electronic aluminium foil Co., Ltd. Patentee after: Guangdong Huafeng New Energy Technology Co., Ltd. Address before: 526060 Duanzhou Industrial City, Duanzhou Road, Zhaoqing City, Guangdong Province Co-patentee before: Zhaoqing Gaoyao Huafeng Electronic aluminium foil Co., Ltd. Patentee before: Zhaoqing Huafeng Electronic Aluminum Foil Co., Ltd. |
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