CN102878961A - Method for detecting surface topography of aluminum electrode foil of electrolytic capacitor - Google Patents
Method for detecting surface topography of aluminum electrode foil of electrolytic capacitor Download PDFInfo
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Abstract
The invention relates to a method for detecting the surface topography of the aluminum electrode foil of an electrolytic capacitor, comprising the steps that mechanical polish-grinding and solution polishing is conducted by alkaline solution and/or acid polishing slurry, after a polish-formed foil is obtained, the foil is put under an electron microscope to be photographed, and an electron microscope image displaying micro holes and an alumina membrane structure are obtained. By using the detecting method of the invention, clear intuitive photos of the micro topography of the electrode foil can be completely obtained, a direct basis for analyzing the influencing factors of the specific volume of the electrode foil accurately and quantitatively is provided, and therefore, reliable experimental data and guidance are provided for deeply researching and developing the technology of the electrolytic capacitor and process control on actual production lines.
Description
Technical field
The present invention relates to the aluminium electrolutic capacitor manufacturing technology, more particularly, the present invention relates to a kind of detection and manufacture method of aluminium electrolutic capacitor aluminium matter electrode foil.
Background technology
The production of the aluminium matter electrode foil that aluminium electrolutic capacitor is used, successively mainly be divided into corrosion and change into two large operations by operation: corrosion process makes first high-purity aluminum foil make etched foil through a series of electrochemical treatment in specific solution, the etched foil surface forms the micro-rough structure that comprises a large amount of fine holes and raceway groove, thereby make the aluminium foil specific surface area obtain greatly to improve, the difformity of these holes and raceway groove and combination thereof and distribute on variation etc. can cause the micro-rough structure of different situations, have influence on and follow-uply change into the specific surface area of middle aluminum oxide film and compare electric capacity; Formation process also is to use a series of electrochemical process for treating to form fine and close aluminum oxide film at the aluminium foil surface through the corrosion extended surface namely to form Waste Acid From Hua Cheng Foil.The pellumina on electrode foil surface in the aluminium electrolutic capacitor, as actuating medium in the aluminium electrolutic capacitor, its micro-rough structure and effective surface area have determined the specific surface area of electrode foil and then have determined the specific volume of electrode foil, electrode foil surface this layer pellumina also all plays an important role for withstand voltage some electrical propertiess such as grade of capacitor.And the static capacity under the electrode foil unit area is specific volume, the topmost performance index of electrode foil, industry all competitively strives for making the larger electrode foil of specific surface area, to obtain under the specific voltage more the electrolytic condenser of Fabrication of High Specific Capacitance, to reduce the capacitor volume, to improve its electric property.
In fact, in shop production line day-to-day operation process, because starting material batch aspect, equipment state aspect, control instrument accuracy aspect, environmental factor aspect, various different variations all may occur, these independents variable change micro-rough structure and the effective surface area that all may have influence on etched foil and Waste Acid From Hua Cheng Foil product multi-form variation occur, thereby so that comparatively specific surface area and the specific volume of macroscopic view produce some erratic variations.
Owing to causing the specific surface area of macroscopic view, the independent variable form that specific volume changes is all not identical with mechanism, therefore, same specific volume may have different micro-rough structures, perhaps, different specific volumes may have same or analogous micro-rough structure, only has the micro-rough structure that observes etched foil and Waste Acid From Hua Cheng Foil product more vividly, could instruct exactly and adjust corrosion and the practical operation of formation workshop production line, improve product at specific volume, the hit rate of the quality index aspect such as withstand voltage, thereby increase production efficiency, reduce production costs, therefore, in the production and research and development of electrode foil, for the low reason of analyzing electrode paper tinsel specific volume, often need to carry out to the microscopic appearance of electrode foil comprehensively accurately observation, thereby provide useful guidance for the technology controlling and process on the actual production line.
Since the electrode foil surface adhesion shelters such as one deck aluminium bits impurity, need to suitably process micro-rough structure and the hole pattern that just can observe it to sample.Traditional observation procedure has ultra-thin section observation method, electropolishing observation method, chemical dissolution observation method.
The ultra-thin section observation method: be that sample is placed resin, after constant temperature solidifies 36 hours, use ultramicrotome to excise 5～10 microns along the direction of vertical cross-section, for subsequent use; Then sample is placed to observe under the transmission electron microscope and detect.The method sample preparation time is longer, and because the aluminium quality is soft, and most of microscopic appearance can be distorted in cutting-off process, the picture distortion that obtains is serious.
Electropolishing observation method: be not have not place the polishing fluid that forms with phosphoric acid and chrome green electropolishing 90～180 seconds under 80 temperature about spending through the etched foil that changes into; Next soak in dilute sulfuric acid and remove electrolysate, then deionized water is cleaned for subsequent use.Sample placed under the scanning electron microscope observe, can photograph clearly surface hole defect photo (Fig. 1).What the method observed is the surface topography of etched foil, and obviously, electrode foil only change into form pellumina after its micro-rough structure just specific storage is had practical significance.For the mesohigh electrode foil, electrode foil can change a lot at the hole pattern (aperture) on Waste Acid From Hua Cheng Foil surface, and therefore, the method adopts the surface topography of etched foil to analyze the specific volume characteristic that changes into the electrode foil surface, cause distortion larger, can not be suitable for.
The chemical dissolution observation method: the electrode foil of selecting to have changed into is cut into suitable size, be attached on the plastic sheet with resin, sample is placed sodium radio-phosphate,P-32 solution, soaked under the normal temperature 30～60 minutes, until the base aluminum of electrode foil is fully dissolved, the plastic sheet that will stick again layer oxide film takes out, clean with deionized water, behind the oven dry sample, place under the scanning electron microscope and observe, can photograph the internal surface shape (Fig. 2) of oxide film.The method is with the simultaneously stripping of microscopic appearance of different aspects, and the photo stereoscopic sensation is stronger, but can't see the hole internal diameter, can not accurately observe the microscopic appearance of electrode foil comprehensively, more is difficult to microscopic appearance is carried out the accurately analysis of quantification.
Summary of the invention
Above-mentioned shortcoming for prior art, the objective of the invention is to provide a kind of detection method of electrolytic condenser surface of aluminum electrode foil pattern, it has following advantage: the clear and intuitive photo that can obtain more all sidedly electric pole foil microscopic appearance, for accurately quantitatively analyzing electrode paper tinsel specific volume influence factor direct basis is provided, thereby provide reliable experimental data and guidance for the technology controlling and process on further investigation exploitation electrolytic condenser technology and the actual production line.
For this reason, the detection method of a kind of electrolytic condenser surface of aluminum electrode foil pattern of technical solution of the present invention; Comprise the steps:
X1) have the Waste Acid From Hua Cheng Foil of pellumina to changing into gained, use flint glass paper dip in water rough polishing Waste Acid From Hua Cheng Foil paper tinsel face to produce a kind of towards polishing scratch, obtain the rough polishing Waste Acid From Hua Cheng Foil;
X2) stagger rough polishing Waste Acid From Hua Cheng Foil surface polishing scratch towards, dip in water fine polishing paper tinsel face to rough polishing polishing scratch with fine sandpaper and all disappear, obtain the fine polishing Waste Acid From Hua Cheng Foil;
X3) stagger fine polishing Waste Acid From Hua Cheng Foil surface polishing scratch towards, have the flannelette essence of abrasive pastes to throw the paper tinsel face with surface-coated, to visual paper tinsel face polishing scratch disappear, the flour milling smooth without foul till, obtain essence and throw Waste Acid From Hua Cheng Foil;
X4) adopt alkaline solution and/or acid polishing slurry that the gained essence is thrown Waste Acid From Hua Cheng Foil and carry out the solution polishing, obtain polishing Waste Acid From Hua Cheng Foil;
X5) will polish Waste Acid From Hua Cheng Foil washing oven dry, and place under the Electronic Speculum and take pictures, obtain showing the Electronic Speculum picture of Micro porosity and pellumina structure.
Although micro-rough structure and the surface topography of etched foil have influence on electrolytic capacitor paper tinsel specific surface area and specific volume, but only consider when changing into and just really tamp electrode foil surface microscopic coarse structure after forming pellumina, make it setting, micro-rough structure after the electrode foil setting just real contrast table area, have reality and directly impact and meaning than electric capacity, the present invention expressly adopts the afterwards Waste Acid From Hua Cheng Foil of gained with pellumina making of taking a sample of the stage of changing into; Has the compound top layer of pellumina that has formalized for Waste Acid From Hua Cheng Foil, this a series of micro-rough textural element of shallow-layer raceway groove under pellumina is compound and the hole of depth, and, for crystalline aluminum oxide film strength and the extremely strong acid-alkali-corrosive-resisting ability that is equivalent to pottery, the problem that direct dissolving is not fallen, the inventive method is developed just right mechanical grinding polishing operation, aluminium oxide coverture with sand papering removal top layer is that " shell " layer grinds off first, expose the material that the inside aluminium oxide and aluminium are mingled with, use the chemical solution rubbing down: chemical solution is shelters such as the aluminium of suitable thickness bits impurity again, the shallow-layer pellumina cleans, dissolve away, remove, make Waste Acid From Hua Cheng Foil have fully comprehensively shallow have deeply expose its top layer, the pattern directly perceived of a series of micro-rough structures such as the shallow-layer raceway groove under pellumina is compound and depth hole; The result is exactly: the SEM that has observed a large amount of tubulose aluminium oxide structure features that forefathers have no is Electronic Speculum pattern photo.Thereafter Fig. 3 and Fig. 4,5,6 electromicroscopic photograph be as seen from this instructions: Waste Acid From Hua Cheng Foil electromicroscopic photograph of the present invention, the clear mini-type tubular pore space structure that has represented electrode foil surface alumina oxide film formation, internal diameter and the more comprehensive micro-rough structure such as external diameter and shallow-layer raceway groove of electrode foil hole have been highlighted, and, can directly read the μ m level size of these micromechanisms on the electromicroscopic photograph; These data can be calculated the statistical data of these micromechanisms through Computer Processing; And when capacitor was worked, alumina tube was the pith in the dielectric material, and its inside pipe wall is negative pole, and the pipe outer wall is anodal.Do not have destroyed residual structure and appearance structure minutia and quantized data after these rubbing downs, all very valuable for the structural factor of analyzing electrode paper tinsel specific surface area, specific volume, for analyze and adjust previous etched foil technique, thereafter chemical synthesis technology can both provide important and abundant detailed information, and provides brand-new and solid reliable experimental data and guidance for further investigation exploitation electrolytic condenser technology.
For further improving the inventive method for predictability, prediction planning property, promptness and the accuracy of technology controlling and process on the actual production line, optimize technology controlling and process on the actual production line, the inventive method also comprises following improvement:
Also comprise step X0 before the described step X1) namely: simulation changes into the chemical synthesis technology of production line, the etched foil that makes on the electroetching production line is simulated change into, and makes corresponding Waste Acid From Hua Cheng Foil; Then, the gained Waste Acid From Hua Cheng Foil is carried out respectively described X1) to X5) detecting step, take pictures respectively until obtain showing the Electronic Speculum picture of gained Micro porosity and pellumina structure.
Be the Operating Guideline of further raising the inventive method for technology controlling and process on the actual production line, the practical application of fully expanding quantized data, the inventive method also comprises following improvement:
Also comprise step X6 after the described step X5) namely: hole and pellumina structure on the gained Waste Acid From Hua Cheng Foil Electronic Speculum picture are measured contrast, and then measure correlation data according to each batch and adjust each batch etched foil and change into accordingly production technology.
For the washing of further giving full play to polishing solution, decontamination, clear stain, dissolving, aobviously really act on, improve rubbing down efficient and to the comprehensive effect of announcement of micro-rough structure, the inventive method also comprises following improvement:
Described step X4) electrolytic polishing liquid in is that weight ratio is absolute ethyl alcohol: perchloric acid=1～2: 4～1 solution.
Described step X4) in, the current density of electropolishing is 0.05～1.0A/cm
2, the electropolishing time is 5～60 seconds.
The described electropolishing time is 10-50 second; Described current density 0.05-0.85A/cm
2
Described step X4) in, the alkaline solution wt% that soaks essence throwing Waste Acid From Hua Cheng Foil consists of: the aqueous solution that contains NaOH 1～5, sodium phosphate 0.1～1.0.
Described step X4) in, the temperature that alkaline solution soaks is controlled at 20～40 ℃, and soak time is 10-100 second.
Described soak time is 20-80 second; Described soaking temperature is 25-35 ℃.
For further optimizing the inventive method to mechanical polishing sense of propriety and the efficient of electrode foil, the inventive method also comprises following improvement:
Described step X1) flint glass paper in is 50～400# waterproof abrasive paper, 1-10 minute rough polishing time; Described step X2) fine sandpaper in is 500～5000# waterproof abrasive paper, 2-20 minute fine polishing time; Described step X3) abrasive pastes in are diamond paste, and adamas particle diameter wherein is 0.5～5um, and the smart throwing time is 3-30 minute; Described step X2), X3) direction of fine polishing, grinding all perpendicular to original polishing scratch towards.
The invention will be further described below in conjunction with the drawings and specific embodiments.
Description of drawings
Fig. 1 is the etched foil surface electromicroscopic photograph figure that traditional electropolishing method obtains.
Fig. 2 is the Waste Acid From Hua Cheng Foil inside surface electromicroscopic photograph figure that the traditional chemical dissolution method obtains.
Fig. 3 is the Waste Acid From Hua Cheng Foil surface Electronic Speculum photo-interpretation figure that the inventive method obtains.
Fig. 4 is the Waste Acid From Hua Cheng Foil surface electromicroscopic photograph schematic diagram that the inventive method embodiment 1 obtains.
Fig. 5 is the Waste Acid From Hua Cheng Foil surface electromicroscopic photograph schematic diagram that the inventive method embodiment 2 obtains.
Fig. 6 is the Waste Acid From Hua Cheng Foil surface electromicroscopic photograph schematic diagram that the inventive method embodiment 3 obtains.
Such as Fig. 1, be depicted as the etched foil surface electromicroscopic photograph figure that traditional electropolishing method obtains.Only can see among the figure: black partly is the corrosion hole of blur margin, light-colored part is not distinguish the metallic aluminium of the depth, this method has drawn from and not yet forms the etched foil of pellumina, relatively has compacting pellumina Waste Acid From Hua Cheng Foil, its surface topography not yet formalizes, distortion is larger, is difficult to analyze the specific volume characteristic on etched foil and Waste Acid From Hua Cheng Foil surface.
Such as Fig. 2, be depicted as the Waste Acid From Hua Cheng Foil inside surface electromicroscopic photograph figure that the traditional chemical dissolution method obtains.For having removed the pattern of the pellumina pipe shell that stays after the base aluminum, can't observe all sidedly pellumina tubulose hole and internal-and external diameter thereof, and the basic micro-rough structure such as base aluminum surface seen in the figure.The microscopic appearance that can not comprehensively accurately reflect electrode foil is difficult to microscopic appearance is carried out the accurately analysis of quantification.
Embodiment
Such as Fig. 3, be depicted as the Waste Acid From Hua Cheng Foil surface Electronic Speculum photo-interpretation figure that the inventive method obtains.As seen from Figure 3: with the pipe 1 (dielectric layer of microcapacitor) that the pellumina of hole 3 consists of, its internal diameter, external diameter, periosteum thickness are high-visible; Concave station 2 its clear-cuts of the dissolved rear formation of base aluminum as seen; The hole 3 of tubular inorganic membrane (negative pole of microcapacitor) outline diameter is high-visible on the electrode foil; And the size of these microstructures all is can know tolerance out and statistical treatment under the Electronic Speculum.Obviously, the more comprehensive microscopic appearance that reflects electrode foil of photo that the inventive method obtains clear and intuitively, can for accurately quantitatively analyzing electrode paper tinsel specific volume influence factor direct basis is provided, thereby provide reliable experimental data and guidance for the technology controlling and process on further investigation exploitation electrolytic condenser technology and the actual production line.
Embodiment 1
Such as Fig. 4, be depicted as the aluminum electrolysis capacitor formed foil surface electromicroscopic photograph schematic diagram that the inventive method embodiment 1 obtains.This embodiment changes into the mesohigh electrode foil to what change into that the production line up-sampling gets off, and order proceeds as follows:
A, cut out the print of lower 10mm*110mm from aluminum electric pole foil;
B, rough polishing: use 400# waterproof abrasive paper to dip in water rough polishing mill 8 minutes;
C, fine polishing: dipped in water fine polishing mill 15 minutes with 2000# waterproof abrasive paper;
D, essence are thrown: with the flannelette rubbing down that is coated with 0.5um particle diameter diamond paste, the time is 25 minutes;
The polishing of e, alkaline solution: put into 5% NaOH and the alkaline solution mixed solution of 7 ‰ sodium phosphates after the good sample of will polish is clean and soak, temperature conditions is 30 ℃, and soak time is 60 seconds, cleans up post-drying, and is for subsequent use;
F, detection: sample placed to take pictures under the Electronic Speculum obtain Fig. 4.
Embodiment 2
Such as Fig. 5, be depicted as the aluminum electrolysis capacitor formed foil surface electromicroscopic photograph schematic diagram that the inventive method embodiment 2 obtains.This embodiment changes into the mesohigh electrode foil to what simulation changed into that production line makes, proceeds as follows:
A, cut out the print of lower 10mm*110mm from aluminum electric pole foil;
B, rough polishing: use 400# waterproof abrasive paper to dip in the water rough polishing 8 minutes;
C, fine polishing: dipped in water fine polishing mill 15 minutes with 2000# waterproof abrasive paper;
D, essence are thrown: with the flannelette rubbing down that is coated with 0.5um particle diameter diamond paste, the time is 25 minutes;
E, electrolytic solution polishing, electrolytic polishing liquid is absolute ethyl alcohol: perchloric acid=1: 4, current density are 0.1A/cm
2, the electropolishing time is 20 seconds, cleaning, drying is for subsequent use;
F, detection: sample placed to take pictures under the Electronic Speculum obtain Fig. 5.
Embodiment 3
Such as Fig. 6, be depicted as the Waste Acid From Hua Cheng Foil surface electromicroscopic photograph schematic diagram that the inventive method embodiment 3 obtains.This embodiment changes into the aluminium electrolutic capacitor that production line makes to simulation and has changed into the mesohigh electrode foil, proceeds as follows:
A, cut out the print of lower 10mm*110mm from aluminum electric pole foil;
B, rough polishing: use 400# waterproof abrasive paper to dip in the water rough polishing 8 minutes;
C, fine polishing: dipped in water fine polishing mill 15 minutes with 2000# waterproof abrasive paper;
D, essence are thrown: with the flannelette rubbing down that is coated with 0.5um particle diameter diamond paste, the time is 25 minutes;
The polishing of e, dual solution: put into 5% NaOH and the alkaline solution mixed solution of 7 ‰ sodium phosphates after the sample that at first polishing is good is cleaned and soak, temperature conditions is 30 ℃, and soak time is 60 seconds; And then carrying out electropolishing, electrolytic polishing liquid is absolute ethyl alcohol: perchloric acid=1: 4, current density are 0.1A/cm
2, the electropolishing time is 20 seconds, cleaning, drying is for subsequent use;
F, detection: sample placed to take pictures under the Electronic Speculum obtain Fig. 6.
Facts have proved, the electrode foil and the photo thereof that adopt the traditional detection technology to obtain, or do not have the etched foil surface of pellumina, or can't see " the Waste Acid From Hua Cheng Foil inside surface " of pore internal diameter.Classic method all can't directly observe the many-sided micro-rough structure of complete electrode foil pellumina and (comprise positive pole, medium, negative pole), if and can not observe etched foil and the vivid micro-rough structure of Waste Acid From Hua Cheng Foil product, just can only be by rule of thumb or phenomenon make indirect inferences, estimate the micro-rough structure of etched foil and Waste Acid From Hua Cheng Foil product, when detecting specific volume when on the low side, the technician can (hole be few to specific volume factor on the low side, hole is many, hole is large, hole is little, size is divided inhomogeneous, distributed number is inhomogeneous etc., these all can make effective surface area descend, cause specific volume to descend) infer, the technician need to see the photo of etched foil hole, the variation of hole diameter after the imagination changes into: which hole is with blocked, which hole can merge inefficacy, then determine that how adjusting controlled process conditions is revised, obviously, its larger blindness can cause the follow-up specific volume that changes into acquisition on the low side, has caused the order index to be difficult to hit.
The Waste Acid From Hua Cheng Foil surface topography that adopts the inventive method to obtain, can clearly represent comprehensively and intuitively change into the electrode foil surface never by many micro-rough CONSTRUCTED SPECIFICATION such as the mini-type tubular capacitor of a large amount of parallel connections of mistake directly perceived and chases to what tamped at last setting by pellumina, internal diameter that especially can clear observation mesohigh electrode foil hole and the interface of external diameter; In production control, replace classic method with the inventive method, can avoid fully to after corroding, change into rear micro-rough structure and make blindness and infer, and then can predict exactly and in time eliminate each stage to all deterioration factors such as the technique of micro-rough dysplasia impact, raw material, environment, parameter drifts.
For example, because can intuitively and compare the mini-type tubular capacitor aperture, just can utilize tubular condenser specific volume formula
[in the formula: Cap is electric capacity; ε
oBe permittivity of vacuum; ε is the anodic alumina films relative dielectric constant; S is the anodic alumina films surface area; D is the thickness (=E of anodic alumina films
aK); E
aFor forming voltage; K is that pellumina forms constant; L is the Tunnel-hole degree of depth; Ci be i hole girth, i=1,2 ... n; N is pore quantity.] Optimization Technology is as follows: the girth Ci by hole or the quantity n of hole compensate or increase specific volume.Like this, order regulation is withstand voltage higher finished product can followingly solve because the rule of CU=constant (U is for forming voltage and general and the positive correlation of capacitor rated insulation voltage) causes the also problem of corresponding increase of the corresponding decline of its specific volume C meeting, pellumina thickness d:
The higher finished product of U due to the order proof voltage, pellumina thickness d can be corresponding larger, then can adopt diameter than macroscopic void and larger girth Ci do compensation, to keep the high as far as possible specific volume of flat foil area; And the lower finished product of the withstand voltage regulation of order U, though specific volume C is corresponding higher, the pellumina thickness d can be corresponding lower, therefore thereby can adapt to can be by the corresponding large specific volume that further improves of paper tinsel face hole number n value than small holes.
In the reality: the semi-manufacture etched foil can be divided into several specifications, and for example HG is towards the 500V-650V kind; HD is towards 400V-550V kind etc.; The Waste Acid From Hua Cheng Foil finished product then can go to produce according to concrete proof voltage such as the kinds such as 450V, 510V, 630V of order regulation.
Seem same etched foil product early stage, and Waste Acid From Hua Cheng Foil hole form but may have difference thereafter; For example the embodiment of the present application 3 Waste Acid From Hua Cheng Foils are taken the photograph to such an extent that Fig. 6 shows that the miniature tube hole is large and dredges, and embodiment 2 Waste Acid From Hua Cheng Foils are taken the photograph to such an extent that Fig. 5 shows that the miniature tube hole is little and many, but the two can reach same specific volume when test etched foil specific volume, all is divided into equal high level HG14 class.When classic method can not microscopic appearance photo intuitively of the present invention, just may be the front etched foil of Fig. 6 embodiment 3 for the production of the 510V kind, and the front etched foil of Fig. 5 embodiment 2 for the production of the 630V kind; Can to dredge be that n is too little because the miniature pore internal diameter of pellumina distributed number excessive, hole be crossed after then the former changes into, difficult on the larger n value acquisition enough augment and do not reach the Fabrication of High Specific Capacitance of expection; Meeting was too small because of the miniature pore internal diameter of pellumina after the latter changed into, girth Ci too large, hole is too little for the pellumina thickness d, difficult from larger Ci value acquisition adequate remedy, do not reach equally the expection Fabrication of High Specific Capacitance, cause the two specific volume all on the low side, actual can only more low-grade HB13-510V and the HB13-630V finished product of output, cause order not hit.Intuitively hole pattern photo, minimizing blindness, realization accurately feed intake probability, raising finished product specific volume and order hit rate thereby effective reduction makes a mistake because of energy behind employing the present invention.
Facts have proved, the inventive method can improve the accuracy rate that etched foil feeds intake, improve the validity that chemical synthesis technology is adjusted, the output capacity that especially can make the above Fabrication of High Specific Capacitance etched foil of 600V-0.58uf brings up to 94% from 90%, and the hit rate that can make etched foil change into different voltage specification capacitor products by order brings up to 97% from 93%.And with the specific volume theoretical limit of photo morphology prediction electrode foil of the present invention, comparable original raising 23% provides great theoretical enlightenment for catching up with and surpassing some advanced enterprises product quality.
Claims (10)
1. the detection method of an electrolytic condenser surface of aluminum electrode foil pattern comprises the steps:
X1) have the Waste Acid From Hua Cheng Foil of pellumina to changing into gained, use flint glass paper dip in water rough polishing Waste Acid From Hua Cheng Foil paper tinsel face to produce a kind of towards polishing scratch, obtain the rough polishing Waste Acid From Hua Cheng Foil;
X2) stagger rough polishing Waste Acid From Hua Cheng Foil surface polishing scratch towards, dip in water fine polishing paper tinsel face to rough polishing polishing scratch with fine sandpaper and all disappear, obtain the fine polishing Waste Acid From Hua Cheng Foil;
X3) stagger fine polishing Waste Acid From Hua Cheng Foil surface polishing scratch towards, have the flannelette essence of abrasive pastes to throw the paper tinsel face with surface-coated, to visual paper tinsel face polishing scratch disappear, the flour milling smooth without foul till, obtain essence and throw Waste Acid From Hua Cheng Foil;
X4) adopt alkaline solution and/or acid polishing slurry that the gained essence is thrown Waste Acid From Hua Cheng Foil and carry out the solution polishing, obtain polishing Waste Acid From Hua Cheng Foil;
X5) will polish Waste Acid From Hua Cheng Foil washing oven dry, and place under the Electronic Speculum and take pictures, obtain showing the Electronic Speculum picture of Micro porosity and pellumina structure.
2. the detection method of electrolytic condenser surface of aluminum electrode foil pattern as claimed in claim 1, it is characterized in that: also comprise step X0 namely before the described step X1: simulation changes into the chemical synthesis technology of production line, the etched foil that makes on the electroetching production line simulated change into, make corresponding Waste Acid From Hua Cheng Foil; Then, the gained Waste Acid From Hua Cheng Foil is carried out respectively the detecting step of described X1 to X5, take pictures respectively until obtain showing the Electronic Speculum picture of gained Micro porosity and pellumina structure.
3. the detection method of electrolytic condenser surface of aluminum electrode foil pattern as claimed in claim 2, it is characterized in that: also comprise step X6 namely after the described step X5: hole and pellumina structure on the gained Waste Acid From Hua Cheng Foil Electronic Speculum picture are measured contrast, and then measure correlation data according to each batch and adjust each batch etched foil and change into accordingly production technology.
4. the detection method of electrolytic condenser surface of aluminum electrode foil pattern as claimed in claim 1, it is characterized in that: the electrolytic polishing liquid among the described step X4 is that weight ratio is absolute ethyl alcohol: perchloric acid=1～2: 4～1 solution.
5. the detection method of electrolytic condenser surface of aluminum electrode foil pattern as claimed in claim 4, it is characterized in that: among the described step X4, the current density of electropolishing is 0.05～1.0A/cm
2, the electropolishing time is 5～60 seconds.
6. the detection method of electrolytic condenser surface of aluminum electrode foil pattern as claimed in claim 5, it is characterized in that: the described electropolishing time is 10-50 second; Described current density 0.05-0.85A/cm
2
7. the detection method of electrolytic condenser surface of aluminum electrode foil pattern as claimed in claim 1 is characterized in that: among the described step X4, soak the alkaline solution wt% that essence throws Waste Acid From Hua Cheng Foil and consist of: the aqueous solution that contains NaOH 1～5, sodium phosphate 0.1～1.0.
8. the detection method of electrolytic condenser surface of aluminum electrode foil pattern as claimed in claim 7, it is characterized in that: among the described step X4, the temperature that alkaline solution soaks is controlled at 20～40 ℃, and soak time is 10-100 second.
9. the detection method of electrolytic condenser surface of aluminum electrode foil pattern as claimed in claim 8, it is characterized in that: described soak time is 20-80 second; Described soaking temperature is 25-35 ℃.
10. the detection method of electrolytic condenser surface of aluminum electrode foil pattern as claimed in claim 1, it is characterized in that: the flint glass paper among the described step X1 is 50～400# waterproof abrasive paper, 1-10 minute rough polishing time; Fine sandpaper among the described step X2 is 500～5000# waterproof abrasive paper, 2-20 minute fine polishing time; Abrasive pastes among the described step X3 are diamond paste, and adamas particle diameter wherein is 0.5～5um, and the smart throwing time is 3-30 minute; Among described step X2, the X3 direction of fine polishing, grinding all perpendicular to original polishing scratch towards.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104165791A (en) * | 2014-08-21 | 2014-11-26 | 厦门厦顺铝箔有限公司 | Ultrathin aluminum foil metallographic phase microscopic structure inspection method |
| CN106568402A (en) * | 2016-11-16 | 2017-04-19 | 上海大学 | Method of testing depth of tiny hole |
| CN111307851A (en) * | 2020-03-25 | 2020-06-19 | 南通海星电子股份有限公司 | Self-resetting type electrode foil three-dimensional morphology characterization method |
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| CN101354326A (en) * | 2008-09-18 | 2009-01-28 | 西部金属材料股份有限公司 | Method for observing tungsten material product microscopic structure |
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| CN1690256A (en) * | 2004-04-20 | 2005-11-02 | 中国科学院理化技术研究所 | Process for preparing aperture-controllable alumina template |
| JP2006196740A (en) * | 2005-01-14 | 2006-07-27 | Matsushita Electric Ind Co Ltd | Method and device for manufacturing of electrode foil for electrolytic capacitor |
| 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 |
| CN101211697A (en) * | 2006-12-30 | 2008-07-02 | 新疆众和股份有限公司 | Electrolytic capacitor aluminum foil oxidation film stripping liquid and microscopic appearance measurement method |
| CN101354326A (en) * | 2008-09-18 | 2009-01-28 | 西部金属材料股份有限公司 | Method for observing tungsten material product microscopic structure |
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| CN104165791A (en) * | 2014-08-21 | 2014-11-26 | 厦门厦顺铝箔有限公司 | Ultrathin aluminum foil metallographic phase microscopic structure inspection method |
| CN106568402A (en) * | 2016-11-16 | 2017-04-19 | 上海大学 | Method of testing depth of tiny hole |
| CN111307851A (en) * | 2020-03-25 | 2020-06-19 | 南通海星电子股份有限公司 | Self-resetting type electrode foil three-dimensional morphology characterization method |
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