CN111307851A - Self-resetting type electrode foil three-dimensional morphology characterization method - Google Patents
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Abstract
The invention discloses a self-resetting type three-dimensional shape characterization method of an electrode foil. The method can economically and efficiently obtain the three-dimensional morphology characteristics of the low-voltage foil sponge holes, has high information precision, and has important significance for quantitatively evaluating the low-voltage foil sponge holes.
Description
Technical Field
The invention relates to a three-dimensional appearance characterization method of an electrode foil, which comprises formation, mechanical polishing, electrolytic erosion (or chemical erosion) and appearance characterization.
Background
At present, aluminum electrode foil is the main component material of a capacitor, and the production process of the aluminum electrode foil is mainly divided into two parts of corrosion and formation. The etching process is to form high-density holes on the surface of the optical foil to improve the effective surface area of the foil, thereby improving the specific volume performance of the electrode foil. The formation process is to form an oxide film on the surface of the etched foil to meet the pressure resistance requirement. From the viewpoint of nominal voltage, the electrode foil can be divided into low-voltage foil and medium-voltage foil, and the holes formed on the surfaces of the low-voltage foil and the medium-voltage foil are sponge holes and tunnel holes respectively. The characteristics of the surface pores, whether low or medium pressure foils, are the main factors affecting their specific volume, including the size, distribution, density, shape, etc. of the pores. Therefore, accurately acquiring the morphological characteristics of the holes on the surface of the electrode foil is a key step for evaluating the performance and quality of the electrode foil, is an important method for guiding the improvement of the existing electrode foil production process from a microscopic level, and is an important basis for researching and developing a new process.
For medium and high voltage foil, tunnel holes formed by corrosion are relatively independent, the shapes of the holes are relatively regular, and the distribution condition and related information of the holes can be clearly obtained by observing the surface of the foil by using a Scanning Electron Microscope (SEM). For low-voltage foil, sponge holes formed by corrosion are staggered, and the shapes of the holes are complex and irregular. In optical or electronic optical systems, topographical features deep in the hole cannot be clearly observed, since the depth of the hole severely affects the capture of optical or electronic signals. The imaging characteristic enables the position of the tunnel hole to be an obvious low signal intensity area, and the hole area and the non-hole area are easily distinguished; the single-hole depth of the sponge hole is usually shallow, the difference between the signal intensity of the hole area and the signal intensity of the non-hole area is relatively small, the proportion of the non-hole area is small, and experimenters are difficult to judge and count the hole distribution condition in the same plane. In order to make up for the defect that the sponge pore morphology is difficult to quantitatively evaluate in a microscopic representation mode, main manufacturers at home and abroad begin to evaluate the pore size and the pore volume by using a mercury intrusion detector testing method, but the testing method has extremely low efficiency and is difficult to meet the testing requirements of research and production. Therefore, an efficient characterization method and a statistical method for the three-dimensional morphology of the sponge holes are urgently to be established.
The latest literature and patent search results show that the resin replica technology can effectively represent the three-dimensional morphology of the hole. The basic process is as follows: and immersing the surface of the foil into resin, immersing the resin into the holes in a pressurizing mode, and chemically eroding away the aluminum foil after the resin is solidified. Although the method can clearly display the three-dimensional appearance of the sponge holes, the sample preparation process is complicated, the simulation degree of the resin replica has a large relation with the pressurizing parameter, the resin wettability and the resin fluidity, and the display result of the resin replica is difficult to ensure to be completely the same as the real appearance of the holes. In addition, before SEM observation, the resin replica needs additional carbon spraying or gold spraying treatment because of non-conductivity, so that the sample preparation cost is high, and the resin replica is not suitable for large-scale use. .
Disclosure of Invention
Aiming at the defects in the prior art, the technical problem to be solved by the invention is to complete the characterization of the appearance of the sponge holes on the surface of the low-pressure foil in a more economical and efficient manner.
Fig. 1 to 5 show a self-healing type three-dimensional topography characterization method for electrode foil, comprising the following steps: firstly, carrying out formation treatment on an electrode foil, then mechanically polishing one side surface of the electrode foil to a residual core layer by using sand paper, then carrying out electrolytic erosion or chemical erosion until all exposed pure aluminum is dissolved, and finally observing the appearance of one side of a residual oxide layer close to the residual core layer under a scanning electron microscope or an optical microscope.
The present invention forms a sufficiently thick oxide layer on the inner surface of the sponge pores by chemical conversion treatment (as shown in fig. 1 and 2), and the oxide layer is formed by self-growth on the foil surface, so the present invention is called self-replication. Compared with other replica technologies such as resin and the like, the self-replication in the holes can ensure that the morphology of the holes is closer to the actual morphology of the holes, and distortion or misjudgment caused by insufficient pressure or other interference factors (such as capillary force and the like) is avoided. After the oxide layer is formed in the sponge holes, the hole layer on one side of the foil (as shown in fig. 3) needs to be removed by mechanical polishing, i.e., the residual core layer is exposed to the air, so as to prepare for removing pure aluminum. It should be noted that mechanical polishing is not suitable for grinding the entire foil surface to the residual core layer, but should be carried out by grinding a small portion of the foil in the central region, since the remaining oxide layer is very brittle after the pure aluminum has been completely etched away, and the surrounding non-etched region is required to provide support. The pure aluminum can be removed by electrolytic etching or chemical etching, and electrolytic etching is recommended because electrolytic etching is significantly superior to chemical etching in both etching efficiency and etching effect. When electrolytic etching is carried out, a mixed solution of perchloric acid and alcohol is recommended to be used as an etching solution, and the proportion of perchloric acid is not more than 30% so as to prevent excessive etching or damage to an oxide layer. The electrolytic corrosion voltage can be selected from 5-40V, and the recommended voltage range is 18-22V; the maximum temperature of electrolytic corrosion is not more than 20 ℃ to prevent the corrosion rate from being too fast and even damaging the appearance of the oxide layer. Under the recommended electrolytic etching parameter conditions, the oxide layer area where pure aluminum is completely etched away can be obtained after 5-10 min of electrolytic etching (as shown in fig. 4 and 5). And fully soaking and cleaning the electrolytically eroded sample in pure water, soaking the sample in alcohol for a period of time, and then drying the surface of the foil by using a blower or drying the foil in a drying box. Since the area eroded to the oxide layer is brittle, a part of the unetched area needs to be left when the metallographic sample is cut, as shown in fig. 5.
Finally, the residual oxide layer becomes a self-healing material of the sponge hole, and the oxide layer close to one side of the residual core layer is directly observed under SEM, wherein the appearance of the oxide is the entity expression form of the sponge hole.
The invention is further improved in that: the electrode foil can be a corrosion foil or a formed foil; the method is mainly used for the appearance characterization of low-voltage foils and is also suitable for medium-high voltage foils.
The invention is further improved in that: before the electrode foil is subjected to formation treatment, the electrode foil is soaked in boiling water for pretreatment.
The invention is further improved in that: the formation treatment adopts a mixed solution of 80-120 g/L boric acid and 1-5 g/L ammonium dihydrogen phosphate, the formation voltage is 80-150V, the formation temperature is 70-90 ℃, and the formation time is 10-20 min.
The invention is further improved in that: the sand paper used for mechanical polishing is 1200-2000 # water-grinding sand paper.
The invention is further improved in that: the electrolytic erosion adopts a mixed solution of 5% -15% perchloric acid and alcohol, the voltage of the electrolytic erosion is 15-30V, and the electrolytic erosion temperature is-30-10 ℃.
The invention is further improved in that: the chemical erosion adopts a mixed solution of 4-9 g/L sodium hydroxide and 3-10 g/L sodium phosphate, the maximum weight ratio of the sodium hydroxide to the sodium phosphate is 3:1, the minimum weight ratio of the sodium hydroxide to the sodium phosphate is 1:1, and the chemical erosion temperature is 10-30 ℃.
Compared with the prior art, the invention has the following advantages:
the three-dimensional morphology characteristics of the low-voltage foil holes are obtained economically and efficiently, the information accuracy is high, and the method is an important basis for quantitatively evaluating the characteristics of the low-voltage foil sponge holes. Specifically, the following points are mainly defined. 1) The self-replicating technology of the invention utilizes the thickened oxide film on the surface of the hole, has high conformity between the appearance of the oxide film and the real shape of the hole, and is more reliable than appearance information obtained by other replicating technologies. 2) The sample preparation period is short, the whole process of the invention can be completed within 1 hour, and other renaturation techniques usually require 8 hours or even longer, because the resin renaturation and other techniques have to take longer solidification time as the cost in order to obtain good fluidity of the resin. 3) The method has the advantages of low oxygen production cost, no obvious consumable material in the sample preparation process, long-term use of the formation solution and the electrolytic corrosion solution, and no need of additional treatment such as carbon spraying or gold spraying in SEM observation. Drawings
FIG. 1 is a schematic cross-sectional view of an untreated low-pressure foil.
Fig. 2 is a schematic cross-sectional view of a low-pressure foil after a formation process.
FIG. 3 is a schematic cross-sectional view of a low-pressure foil after mechanical polishing.
FIG. 4 is a schematic cross-sectional view of a low-voltage foil after electrolytic etching.
FIG. 5 is a schematic view of the surface of a low-voltage foil after electrolytic etching.
Reference numbers in the figures: 1-pure aluminum residual core layer, 2-hole layer in the area of the hole, 3-oxide or oxide layer after chemical conversion treatment, 4-area for grinding and erosion, 5-area without grinding and erosion, and 6-cutting line for preparing metallographic samples.
Detailed Description
Example 1:
firstly, soaking a low-pressure corrosion foil in boiling pure water for pre-formation treatment for 5 min; then, carrying out chemical conversion treatment in 100g/L boric acid solution, adding 5g/L ammonium dihydrogen phosphate, setting the voltage at 100V, and carrying out chemical conversion treatment for 5min after reaching the pressure. The formed foil is directly polished on sand paper by hand, and observation is carried out once every 10 times of grinding until the middle part of the foil presents a residual core layer area with the diameter of about 1cm, and the residual core layer area presents a metallic silver color. Electrolytic etching is carried out on the polished foil, the electrolytic etching temperature is controlled below 10 ℃, the concentration of perchloric acid in electrolytic etching liquid is recommended to be below 10% (preferably about 8%), the voltage is preferably about 20V, the initial electrolysis time can be set to be 5min, and then the stepping time is 1min until a gray black oxidation area with the diameter not less than 5mm appears in the polishing area. Washing with flowing pure water for 1min, immersing the sample in alcohol, and blow-drying with blower. For SEM observation, the voltage should be as small as possible to reduce the charging effect, and 5kV is recommended.
Example 2:
firstly, soaking a low-pressure corrosion foil in boiling pure water for pre-formation treatment for 20 min; then, carrying out chemical conversion treatment in 200g/L boric acid solution, adding 2g/L ammonium dihydrogen phosphate, setting the voltage at 100V, and carrying out chemical conversion treatment for 15min after reaching the pressure. The formed foil is directly polished on sand paper by hand, and observation is carried out once every 10 times of grinding until the middle part of the foil presents a residual core layer area with the diameter of about 1cm, and the residual core layer area presents a metallic silver color. Electrolytic etching is carried out on the polished foil, the electrolytic etching temperature is controlled below 10 ℃, the concentration of perchloric acid in electrolytic etching liquid is recommended to be below 10% (preferably about 8%), the voltage is preferably about 20V, the initial electrolysis time can be set to be 5min, and then the stepping time is 1min until a gray black oxidation area with the diameter not less than 5mm appears in the polishing area. Washing with flowing pure water for 1min, immersing the sample in alcohol, and blow-drying with blower. For SEM observation, the voltage should be as small as possible to reduce the charging effect, and 5kV is recommended.
Example 3:
firstly, carrying out secondary formation treatment on the low-voltage formed foil in 100g/L boric acid solution, adding 5g of ammonium dihydrogen phosphate, setting the voltage at 100V, and carrying out formation treatment for 5min after reaching the voltage. The formed foil is directly polished on sand paper by hand, and observation is carried out once every 10 times of grinding until the middle part of the foil presents a residual core layer area with the diameter of about 1cm, and the residual core layer area presents a metallic silver color. Electrolytic etching is carried out on the polished foil, the electrolytic etching temperature is controlled below 10 ℃, the concentration of perchloric acid in electrolytic etching liquid is recommended to be below 10% (preferably about 8%), the voltage is preferably about 20V, the initial electrolysis time can be set to be 5min, and then the stepping time is 1min until a gray black oxidation area with the diameter not less than 5mm appears in the polishing area. Washing with flowing pure water for 1min, immersing the sample in alcohol, and blow-drying with blower. For SEM observation, the voltage should be as small as possible to reduce the charging effect, and 5kV is recommended.
Example 4:
firstly, carrying out secondary formation treatment on the low-voltage formed foil in 200g/L boric acid solution, adding 2g of ammonium dihydrogen phosphate, setting the voltage at 100V, and carrying out formation treatment for 15min after reaching the voltage. The formed foil is directly polished on sand paper by hand, and observation is carried out once every 10 times of grinding until the middle part of the foil presents a residual core layer area with the diameter of about 1cm, and the residual core layer area presents a metallic silver color. Electrolytic etching is carried out on the polished foil, the electrolytic etching temperature is controlled below 10 ℃, the concentration of perchloric acid in electrolytic etching liquid is recommended to be below 10% (preferably about 8%), the voltage is preferably about 20V, the initial electrolysis time can be set to be 5min, and then the stepping time is 1min until a gray black oxidation area with the diameter not less than 5mm appears in the polishing area. Washing with flowing pure water for 1min, immersing the sample in alcohol, and blow-drying with blower. For SEM observation, the voltage should be as small as possible to reduce the charging effect, and 5kV is recommended.
According to the embodiment, effective morphological information of holes on the surface of the etched foil or the formed foil can be obtained, and the strength and the corrosion degree of the oxide film can be adversely affected after relevant parameters are changed. The parameters referred to in the examples are recommended usage parameters.
The applicant further states that the present invention is described in the above embodiments to explain the implementation method and device structure of the present invention, but the present invention is not limited to the above embodiments, i.e. it is not meant to imply that the present invention must rely on the above methods and structures to implement the present invention. It should be understood by those skilled in the art that any modifications to the present invention, the implementation of alternative equivalent substitutions and additions of steps, the selection of specific modes, etc., are within the scope and disclosure of the present invention.
The present invention is not limited to the above embodiments, and all the ways of achieving the objects of the present invention by using the structure and the method similar to the present invention are within the protection scope of the present invention.
Claims (7)
1. A self-resetting type electrode foil three-dimensional morphology characterization method is characterized by comprising the following steps: firstly, carrying out formation treatment on an electrode foil, then mechanically polishing one side surface of the electrode foil to a residual core layer by using sand paper, then carrying out electrolytic erosion or chemical erosion until all exposed pure aluminum is dissolved, and finally observing the appearance of one side of a residual oxide layer close to the residual core layer under a scanning electron microscope or an optical microscope.
2. The method for characterizing the three-dimensional morphology of the self-replicating electrode foil according to claim 1, wherein: the electrode foil is a corrosion foil or a formation foil.
3. The method for characterizing the three-dimensional morphology of the self-replicating electrode foil according to claim 1, wherein: before the electrode foil is subjected to formation treatment, the electrode foil is soaked in boiling water for pretreatment.
4. The method for characterizing the three-dimensional morphology of the self-replicating electrode foil according to claim 1, wherein: the formation treatment adopts a mixed solution of 10-500 g/L boric acid and 0-100 g/L ammonium dihydrogen phosphate, the formation voltage is 30-300V, the formation temperature is 50-100 ℃, and the formation time is 2-30 min.
5. The method for characterizing the three-dimensional morphology of the self-replicating electrode foil according to claim 1, wherein: the sand paper used for mechanical polishing is No. 60-5000 water-milled sand paper, dry-milled sand paper, sponge sand paper or dust-free net sand paper.
6. The method for characterizing the three-dimensional morphology of the self-replicating electrode foil according to claim 1, wherein: the electrolytic erosion adopts a mixed solution of 1-30% perchloric acid and alcohol, the voltage of the electrolytic erosion is 5-40V, and the electrolytic polishing temperature is-30-20 ℃.
7. The method for characterizing the three-dimensional morphology of the self-replicating electrode foil according to claim 1, wherein: the chemical erosion adopts a mixed solution of 1-100 g/L sodium hydroxide and 1-20 g/L sodium phosphate, the maximum weight ratio of the sodium hydroxide to the sodium phosphate is 20:1, the minimum weight ratio of the sodium hydroxide to the sodium phosphate is 1:1, and the chemical erosion temperature is-30-90 ℃.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060076243A1 (en) * | 2004-10-12 | 2006-04-13 | Tatsuji Aoyama | Electrode foil for electrolytic capacitor and method for manufacturing the same |
| 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 |
| CN101707142A (en) * | 2009-11-18 | 2010-05-12 | 横店集团东磁股份有限公司 | Formation method for increasing hydration-proof performance of electrode foil for aluminum electrolytic capacitor |
| CN101818378A (en) * | 2010-04-26 | 2010-09-01 | 江苏林洋新能源有限公司 | Velvet manufacturing solution of monocrystalline silicon additive |
| CN102878961A (en) * | 2012-09-08 | 2013-01-16 | 乳源瑶族自治县东阳光化成箔有限公司 | Method for detecting surface topography of aluminum electrode foil of electrolytic capacitor |
| CN109461586A (en) * | 2018-10-10 | 2019-03-12 | 乳源瑶族自治县东阳光化成箔有限公司 | A kind of preparation method reducing aluminium electrolutic capacitor low-field electrode foil leakage current |
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2020
- 2020-03-25 CN CN202010218729.1A patent/CN111307851A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060076243A1 (en) * | 2004-10-12 | 2006-04-13 | Tatsuji Aoyama | Electrode foil for electrolytic capacitor and method for manufacturing the same |
| 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 |
| CN101707142A (en) * | 2009-11-18 | 2010-05-12 | 横店集团东磁股份有限公司 | Formation method for increasing hydration-proof performance of electrode foil for aluminum electrolytic capacitor |
| CN101818378A (en) * | 2010-04-26 | 2010-09-01 | 江苏林洋新能源有限公司 | Velvet manufacturing solution of monocrystalline silicon additive |
| CN102878961A (en) * | 2012-09-08 | 2013-01-16 | 乳源瑶族自治县东阳光化成箔有限公司 | Method for detecting surface topography of aluminum electrode foil of electrolytic capacitor |
| CN109461586A (en) * | 2018-10-10 | 2019-03-12 | 乳源瑶族自治县东阳光化成箔有限公司 | A kind of preparation method reducing aluminium electrolutic capacitor low-field electrode foil leakage current |
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