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CN109884106A - A kind of analysis method of anodic corrosion foil for fast aluminum electrolytic capacitor - Google Patents

A kind of analysis method of anodic corrosion foil for fast aluminum electrolytic capacitor Download PDF

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Publication number
CN109884106A
CN109884106A CN201910179812.XA CN201910179812A CN109884106A CN 109884106 A CN109884106 A CN 109884106A CN 201910179812 A CN201910179812 A CN 201910179812A CN 109884106 A CN109884106 A CN 109884106A
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CN
China
Prior art keywords
hole
etched foil
analysis method
foil
aluminum electrolysis
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CN201910179812.XA
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Chinese (zh)
Inventor
胥珊娜
王海丽
钟玉洁
王雷
奚运涛
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Xian Shiyou University
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Xian Shiyou University
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Priority to CN201910179812.XA priority Critical patent/CN109884106A/en
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Abstract

A kind of quick aluminum electrolysis capacitor anode etched foil borrosion hole analysis method, electrobrightening is carried out to etched foil using chromium trioxide-phosphoric acid electrolysis, obtain the electron microscopic picture of Micro porosity structure, it is distinguished by image procossing and to form factor, data are handled using circular model or square model, obtain etch pit characteristic parameter.Single hole and simultaneously hole are distinguished using the form factor under control different amplification, achievees the purpose that each characteristic parameter of accurate rapid qualitative analysis etched foil pattern and index.Using average single hole aperture, single hole accounting and the etch pits characteristic parameter such as hole accounting, hair engaging aperture density, rate of corrosion, achieve the purpose that instruct technique adjustment, the method that manually number hole counts than before greatly improves work efficiency and analysis precision.New analysis method is provided for aluminum electrolysis capacitor anode etched foil technique adjustment.

Description

A kind of quick aluminum electrolysis capacitor anode etched foil borrosion hole analysis method
Technical field
The present invention relates to the technical fields to aluminium electrolutic capacitor analysis measurement, and in particular to a kind of quick alminium electrolytic condenser Device anodic attack foil borrosion hole analysis method.
Background technique
Anode foils are the key raw materials of aluminium electrolutic capacitor, thus the manufacturing technology of anode foils is largely fixed The technical level of aluminium electrolutic capacitor.It is increasingly minimized and integrated requirement to meet electronic product, needs to realize aluminium The high specific capacitance of electrolytic capacitor electrode foil.The production of the aluminum electrode foil of aluminium electrolutic capacitor is successively led by process It is divided into two big processes of corrosion and chemical conversion.Corrosion process make etched foil surface formed include a large amount of longitudinal fine tunnel holes and The heterogeneous microstructure of lateral channel, so that aluminium foil specific surface area is greatly improved, the different shape of hole, distribution shape State, hair engaging aperture density and hole size etc. influence whether the specific surface area and specific capacitance of aluminum oxide film in subsequent chemical conversion.State at present Inside and outside most common aluminum electrolysis capacitor anode etched foil borrosion hole has ultra-thin section observation method, electrobrightening observation method, chemical solution Solve observation method.Such as " method for making sample of measuring aluminium electrolysis capacitor electric pole foil microscopic appearance " (CN 101210863A), be by Etched foil is placed in the polishing fluid formed with phosphoric acid and chrome green at a temperature of 70-90 DEG C, current density 0.1A/cm2- Deionized water cleaning, drying is used after 0.5A/cm2 electrobrightening 90-180 seconds.Sample is placed under scanning electron microscope and is observed, can be clapped Clearly surface hole defect photo is taken the photograph, and carries out Manual analysis.The shortcomings that the method, is: (1) according to maximum current density 0.5A/ Cm2, electrobrightening 90-180 seconds at a temperature of 90 DEG C, average single thickness thinning of surveying is 8-15 μm (see figure one), is only capable of reflection table Layer borrosion hole growing state cannot reflect etched foil entirety pitting pattern and distribution, analysis result distortion;(2) Manual analysis hole Photo, working efficiency is low, error is big.
Another detection method of surface topography of aluminum electrode foil of electrolytic capacitor.Such as " electrolytic capacitor aluminum electric pole foil table The detection method of face pattern " (CN 102878961A), has the Waste Acid From Hua Cheng Foil of pellumina to chemical conversion gained, and grinding, polishing obtain Essence throws Waste Acid From Hua Cheng Foil;Waste Acid From Hua Cheng Foil is thrown to gained essence using alkaline solution or acid polishing slurry and carries out solution polishing, obtains polishing chemical conversion Foil;Polishing Waste Acid From Hua Cheng Foil washing is dried, is placed under Electronic Speculum and takes pictures, obtain the electron microscope of display Micro porosity and pellumina structure Piece.The disadvantages of this method are: (1) analyzes Waste Acid From Hua Cheng Foil hole and pellumina structure, not to decision aluminium electricity electrolytic capacitor The major influence factors of device capacity-etched foil carries out service system analysis, cannot instruct the process modification of corrosion process;(2) right Hair engaging aperture density, single hole aperture, single hole accounting and the hole accounting for influencing capacity are not analyzed comprehensively.
Summary of the invention
In order to overcome the above-mentioned prior art, the object of the present invention is to provide a kind of quick aluminum electrolysis capacitor anode etched foils Borrosion hole analysis method, can obtain the clear and intuitive photo that etched foil prolongs depth direction microscopic appearance, can accurate rapid qualitative Each characteristic parameter of etched foil pattern and index are analyzed, provides direct basis for specific volume of electrode foil influence factor, thus deeply to grind The technology controlling and process studied carefully on exploitation electrolytic capacitor technology and actual production line provides reliable experimental data and guidance.
To achieve the goals above, the technical solution adopted by the present invention is that:
A kind of quick aluminum electrolysis capacitor anode etched foil borrosion hole analysis method, comprising the following steps:
1) there is the etched foil of complicated Tunnel-hole to corrosion gained, use the phosphoric acid and mass fraction 10- of mass fraction 70-90% 30% chromium trioxide matches solution, carries out electrobrightening, and clean drying with pure water, control polish temperature for 65 DEG C -80 DEG C, Time 1-5 minute and current density (0.1-0.3A/cm2), the series polishing foil from a surface to sandwich layer is obtained, and measure etched foil Thickness;
2) it is placed under Electronic Speculum and carries out the positive and negative electron microscopic picture taken pictures, obtain showing Micro porosity structure under 1000 times and 2000 times, It is distinguished by image procossing and to form factor;
3) picture processing is carried out by public image processing software Image J, by controlling different amplification, i.e., 1000 Times, the form factor under 2000 times be that 0.7-0.98 distinguishes single hole and simultaneously hole;
4) initial data is analyzed for single hole, using circular model (area=1/4 × π × aperture2) or square model (area=hole Diameter2) data are handled, obtain average single hole aperture, single hole accounting;
Initial data is analyzed for simultaneously hole, data processing is carried out and obtains simultaneously hole accounting;Calculate whole hair engaging aperture density, rate of corrosion.
The public image processing software is Image J.
The phosphoric acid and chromic anhydride proportion are phosphoric acid 70-90% mass fraction, chromium trioxide 10-30% mass fraction.
Control polish temperature, time and the current density is polish temperature (65 DEG C -80 DEG C), time (1-5 minutes) And current density (0.1-0.3A/cm2).
5, a kind of quick aluminum electrolysis capacitor anode etched foil borrosion hole analysis method according to claim 1, it is special Sign is that the same amplification factor and form factor are respectively as follows: amplification factor (1000 times, 2000 times), form factor (0.7- 0.98).
The beneficial effects of the present invention are:
1, the invention is prolonged etched foil and is analyzed under depth direction different amplification, carries out to the distribution of whole borrosion hole and feature Analysis comprehensively.
2, Manual analysis is compared, analytic process is high-efficient, resultant error is small.
3, the characteristic parameter for enriching characterization etched foil, is more advantageous to and instructs technique adjustment.
4, it can achieve quickly analysis and obtain the purpose along depth direction different layers deep etch foil borrosion hole characteristic parameter.
5, it avoids manually visualizing the error that identification generates.
6, using average single hole aperture, single hole accounting and the etch pits characteristic parameter such as hole accounting, hair engaging aperture density, rate of corrosion, Achieve the purpose that instruct technique adjustment.
Detailed description of the invention
Fig. 1 is that the embodiment of the present invention is etched foil electrobrightening depth schematic diagram.
Fig. 2 is electrobrightening 2min aluminium foil borrosion hole image (a) under 1000 times of scanning electron microscope, is handled with image processing software Single hole image (b) afterwards, with image processing software, treated and hole image (c).
Fig. 3 is electrobrightening 2min aluminium foil borrosion hole image (a) under 2000 times of scanning electron microscope, is handled with image processing software Single hole image (b) afterwards, with image processing software, treated and hole image (c).
Fig. 4 be certain domestic etched foil and 2000 times of pore analysis data comparison figures of certain import etched foil.
Specific embodiment
The present invention is further discussed below with reference to embodiments.
Using the above method, the embodiment of the present invention 1 is as follows:
Certain aluminum electrolysis capacitor anode etched foil, 120 μm of etched foil thickness specification, 0.78 μ F/cm2 of capacity, bending 50 is returned, and is resisted Tensile strength 25.9.
Etched foil is cut into the strip sample of 2cm × 8cm first, wherein the part bottom 2cm × 2cm enters concentration In temperature phosphoric acid-chromic anhydride proportion solution, applying current density respectively is 0.2A/cm2Electric current 1min-5min(correspond to etched foil Thickness thinning is shown in Fig. 1) electrobrightening is carried out, sample must be polished after cleaning.Then paillon front and back sides are carried out under scanning electron microscope Observation, and obtain 1000 times and 2000 times of stereoscan photographs.
Then data processing is carried out to picture using Image J PaintShop, then progress scale setting first is selected It takes effective coverage to carry out image threshold setting, and is set that (wherein 1000 times of picture form factors are set as to form factor 0.8,0.9) 2000 times of picture form factors are set as.Single hole and simultaneously hole picture is shown in Fig. 2 and Fig. 3 after processing.Single hole is obtained simultaneously And the simultaneously area data in hole, data are post-processed using square hole model or circular hole model, obtain corroded area accounting, single hole Accounting, single hole average pore size, hair engaging aperture density and the characteristic parameters such as hole accounting.Fig. 4 show certain domestic etched foil and certain import is rotten Lose foil pore analysis data comparison figure.To complete the analysis of aluminum electrolysis capacitor anode etched foil characteristic parameter.

Claims (5)

1. a kind of quick aluminum electrolysis capacitor anode etched foil borrosion hole analysis method, which comprises the following steps:
1) there is the etched foil of complicated Tunnel-hole to corrosion gained, use the phosphoric acid and mass fraction 10- of mass fraction 70-90% 30% chromium trioxide matches solution, carries out electrobrightening, and clean drying with pure water, control polish temperature for 65 DEG C -80 DEG C, Time 1-5 minute and current density (0.1-0.3A/cm2), the series polishing foil from a surface to sandwich layer is obtained, and measure etched foil Thickness;
2) it is placed under Electronic Speculum and carries out the positive and negative electron microscopic picture taken pictures, obtain showing Micro porosity structure under 1000 times and 2000 times, It is distinguished by image procossing and to form factor;
3) picture processing is carried out by public image processing software Image J, by controlling different amplification, i.e., 1000 Times, the form factor under 2000 times be that 0.7-0.98 distinguishes single hole and simultaneously hole;
4) initial data is analyzed for single hole, using circular model (area=1/4 × π × aperture2) or square model (area=hole Diameter2) data are handled, obtain average single hole aperture, single hole accounting;
Initial data is analyzed for simultaneously hole, data processing is carried out and obtains simultaneously hole accounting;Calculate whole hair engaging aperture density, rate of corrosion.
2. a kind of quick aluminum electrolysis capacitor anode etched foil borrosion hole analysis method according to claim 1, feature exist In the public image processing software is Image J.
3. a kind of quick aluminum electrolysis capacitor anode etched foil borrosion hole analysis method according to claim 1, feature exist In the phosphoric acid and chromic anhydride proportion are phosphoric acid 70-90% mass fraction, chromium trioxide 10-30% mass fraction.
4. a kind of quick aluminum electrolysis capacitor anode etched foil borrosion hole analysis method according to claim 1, feature exist In control polish temperature, time and the current density are polish temperature (65 DEG C -80 DEG C), time (1-5 minutes) and electric current Density (0.1-0.3A/cm2).
5. a kind of quick aluminum electrolysis capacitor anode etched foil borrosion hole analysis method according to claim 1, feature exist In the same amplification factor and form factor are respectively as follows: amplification factor (1000 times, 2000 times), form factor (0.7- 0.98).
CN201910179812.XA 2019-03-11 2019-03-11 A kind of analysis method of anodic corrosion foil for fast aluminum electrolytic capacitor Pending CN109884106A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111276333A (en) * 2020-03-27 2020-06-12 乳源瑶族自治县东阳光化成箔有限公司 Calculation method for evaluating energy consumption of corrosion foil formation
CN111814831A (en) * 2020-06-10 2020-10-23 东莞东阳光科研发有限公司 Method for measuring specific value of corrosion foil

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB845832A (en) * 1957-11-07 1960-08-24 Philips Electrical Ind Ltd Improvements in or relating to methods of manufacturing perforated shear plates for dry-shaving apparatus
CN101210863A (en) * 2006-12-29 2008-07-02 新疆众和股份有限公司 Sample preparation method for measuring aluminium electrolysis capacitor electric pole foil microscopic appearance

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB845832A (en) * 1957-11-07 1960-08-24 Philips Electrical Ind Ltd Improvements in or relating to methods of manufacturing perforated shear plates for dry-shaving apparatus
CN101210863A (en) * 2006-12-29 2008-07-02 新疆众和股份有限公司 Sample preparation method for measuring aluminium electrolysis capacitor electric pole foil microscopic appearance

Non-Patent Citations (3)

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Title
李文勇 等: "基于形状因子和分割点定位的粘连害虫图像分割方法", 《农业工程学报》 *
洪涛 等: "中高压阳极铝箔微观形貌的分析方法 ", 《电子元件与材料》 *
陈浩 等: "基于几何形状特征的剩余油形态识别 ", 《微型机与应用》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111276333A (en) * 2020-03-27 2020-06-12 乳源瑶族自治县东阳光化成箔有限公司 Calculation method for evaluating energy consumption of corrosion foil formation
CN111276333B (en) * 2020-03-27 2021-10-01 乳源瑶族自治县东阳光化成箔有限公司 Calculation method for evaluating energy consumption of corrosion foil formation
CN111814831A (en) * 2020-06-10 2020-10-23 东莞东阳光科研发有限公司 Method for measuring specific value of corrosion foil

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Application publication date: 20190614

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