CN110208304B - Method for analyzing microscopic morphology of porous oxide film on surface layer of aluminum foil - Google Patents
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Abstract
The invention relates to an analysis method for the microscopic morphology of a porous oxide film on the surface layer of an aluminum foil. A method for analyzing the microscopic morphology of a porous oxide film on the surface layer of an aluminum foil comprises the following steps: carrying out high-temperature melting treatment on the formation pretreatment aluminum foil sample, wherein a certain included angle is formed between the formation pretreatment aluminum foil sample and the bottom of a heating container in the treatment process, aluminum liquid flows to the lower part under the action of gravity, and after cooling, aluminum is separated from aluminum oxide to obtain a porous oxide film; and (3) placing the porous oxide film in a scanning electron microscope or an electronic lens for analysis to obtain micro-morphology parameters. According to the method for analyzing the micro-morphology of the porous oxide film on the surface layer of the aluminum foil, the aluminum foil with the acid and alkali resistant aluminum oxide film on the surface is melted at high temperature, the aluminum oxide film is stripped, and the micro-morphology parameters are further analyzed to provide data support for researching a formation mechanism. And the stripping process is simple and easy to control, and the method is suitable for analyzing the microscopic morphology of the surface porous oxide film to perform basic research.
Description
Technical Field
The invention particularly relates to an analysis method for the microscopic morphology of a porous oxide film on an aluminum foil surface layer.
Background
In the industry, an aluminum foil formation pretreatment (boiling water boiling or anodic oxidation) is carried out to generate a porous oxide film with the pore diameter of 5-200nm and the thickness of 30-800nm, and after formation, the porous oxide film is partially converted into a compact oxide film to be used as a dielectric film of an electrolytic capacitor. The porous oxide film is closely related to the quality index of the formed foil.
In the prior art, an alkaline etching method is adopted to strip an oxide film on the surface of an aluminum foil, and then a scanning electron microscope or an electronic lens is used for analysis, so that the micro-morphology parameters of the oxide film can be obtained. However, there are the following problems: since amorphous alumina and crystalline alumina are both dissolved in alkali liquor, and crystalline aluminum oxyhydroxide is alkali-resistant and acid-resistant, the alkaline etching method is only effective for films containing crystalline aluminum oxyhydroxide, i.e., the alkaline etching method cannot strip films of amorphous alumina and crystalline alumina. Therefore, the aluminum foil (mainly containing crystalline aluminum hydroxide) after formation can only be stripped into an oxide film on the surface of the aluminum foil by an alkaline etching method; and then analyzing by a scanning electron microscope or an electronic lens to obtain the micro-morphology parameters. The porous alumina film on the surface of the aluminum foil before formation treatment comprises amorphous alumina, wherein the aperture of the micropores is 5-200nm, and the thickness is about 30-2000 nm; the oxide film is dissolved at the same time regardless of the dissolution of aluminum by the acid solution or the alkali solution, and the effect of peeling off the oxide film is not achieved.
In view of the above, the present invention provides a novel method for analyzing the microstructure of a porous oxide film on an aluminum foil surface.
Disclosure of Invention
The invention aims to provide an analysis method for the micro-morphology of a porous oxide film on the surface layer of an aluminum foil, which is suitable for the aluminum foil before formation, solves the problems that the porous alumina is not acid-base-resistant and is not easy to peel, improves the analysis accuracy of the micro-morphology, and provides data support for researching a formation mechanism.
In order to realize the purpose, the adopted technical scheme is as follows:
a method for analyzing the microscopic morphology of a porous oxide film on the surface layer of an aluminum foil comprises the following steps:
carrying out high-temperature melting treatment on the formation pretreatment aluminum foil sample, wherein a certain included angle is formed between the formation pretreatment aluminum foil sample and the bottom of a heating container in the treatment process, aluminum liquid flows to the lower part under the action of gravity, and after cooling, aluminum is separated from aluminum oxide to obtain a porous oxide film;
and (3) placing the porous oxide film in a scanning electron microscope or an electronic lens for analysis to obtain micro-morphology parameters.
Furthermore, the width of the aluminum foil sample before formation treatment is 0.5-1.5cm, and the length is 2.5-5.0 cm.
Furthermore, the long edge of the formation pretreatment aluminum foil sample is vertical to the bottom of the heating container.
Still further, in the high-temperature melting treatment process: and fixing the formation pretreatment aluminum foil sample by using a ceramic chip, and keeping the formation pretreatment aluminum foil sample vertical to the bottom of the heating container.
Further, the temperature of the high-temperature melting treatment is 700-.
Furthermore, in the analysis process, the aperture of the micropores of the porous oxide film is larger than 50nm and is analyzed by a scanning electron microscope; for example, the pore diameter of the micropores of the porous oxide film is less than 50nm and is analyzed by an electron lens.
Compared with the prior art, the invention has the advantages that:
1. the invention adopts high temperature to melt aluminum, the sample wafer is vertically placed, and the aluminum liquid flows to the lower end under the action of gravity, thereby achieving the purpose of separating aluminum from aluminum oxide; and (4) analyzing the separated alumina film under an electron microscope to obtain the micro-morphology parameters.
2. The high-temperature stripping process of the oxide film is simple and easy to operate. The used materials can be purchased in the market; scanning electron microscopy or electron lens analysis is the same as the general approach.
3. The method can analyze the appearance of the acid and alkali resistant alumina film, and has important significance for researching the formation mechanism of the aluminum foil and improving the quality of the formed foil product.
Drawings
FIG. 1 is an SEM image of a porous oxide film on the surface of an aluminum foil in example 1;
FIG. 2 is an SEM photograph of a porous oxide film on the surface of an aluminum foil in example 1;
FIG. 3 is an SEM image of a porous oxide film on the surface of an aluminum foil in example 2;
FIG. 4 is an SEM image of a porous oxide film on the surface of an aluminum foil in example 2.
Detailed Description
In order to further illustrate the method for analyzing the micro-morphology of the porous oxide film on the surface of the aluminum foil according to the present invention, the following embodiments, structures, features and effects thereof will be described in detail. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
The method for analyzing the micro-morphology of the porous oxide film on the surface layer of the aluminum foil according to the present invention will be described in detail with reference to the following embodiments and fig. 1 to 4:
the technical scheme of the invention is as follows:
and (2) carrying out high-temperature melting treatment on the formation pretreatment aluminum foil sample, wherein a certain included angle is formed between the formation pretreatment aluminum foil sample and the bottom of the heating container in the treatment process, the aluminum liquid flows to the lower part under the action of gravity, and after cooling, the aluminum is separated from the aluminum oxide to obtain the porous oxide film. (for the purpose of peeling off the porous oxide film)
And (3) placing the porous oxide film in a scanning electron microscope or an electronic lens for analysis to obtain micro-morphology parameters.
Preferably, the aluminum foil sample wafer before the formation treatment has a width of 0.5-1.5cm and a length of 2.5-5.0 cm.
Preferably, the long side of the aluminum foil sample subjected to the formation pretreatment is perpendicular to the bottom of the heating container. Is beneficial to the flow of aluminum liquid and enhances the separation effect with aluminum oxide
More preferably, in the high-temperature melting treatment process: and fixing the formation pretreatment aluminum foil sample by using a ceramic chip, and keeping the formation pretreatment aluminum foil sample vertical to the bottom of the heating container.
Preferably, the temperature of the high-temperature melting treatment is 700-100 ℃, and the time is 10-60min, so that the aluminum foil can be quickly and fully melted into the pre-treated aluminum foil sample.
Preferably, in the analysis process, the aperture of the micropores of the porous oxide film is larger than 50nm and is analyzed by a scanning electron microscope; for example, the pore diameter of the micropores of the porous oxide film is less than 50nm and is analyzed by an electron lens.
The pre-chemical conversion treatment aluminum foil in the present invention refers to an aluminum foil before chemical conversion treatment.
Example 1.
The specific operation steps are as follows:
taking the aluminum foil raw material subjected to sulfuric acid anodic oxidation treatment as the formation pretreatment aluminum foil, wherein the pore diameter of the surface porous alumina micropores is 5-20nm, and the thickness is about 600-700 nm.
(1) Cutting the pre-formation treatment aluminum foil into pre-formation treatment aluminum foil sample pieces with the width of 1.5cm and the length of 5.0cm, which are called sample pieces for short.
(2) Placing the sample in a clean crucible, fixing the sample by using two ceramic plates, and keeping the sample vertically standing in the crucible, wherein the long edge of the formed pre-treatment aluminum foil sample is vertical to the bottom of the heating container.
(3) And (3) placing the crucible with the sample wafer in a muffle furnace, and treating for 30min at the temperature of 700-.
(4) And taking out the oxide film for later use after cooling.
(5) The separated porous oxide film was analyzed by placing it in an electron lens to obtain a microscopic morphology SEM photograph, fig. 1-2. As can be seen from FIGS. 1-2, the microscopic morphology is highly accurate.
The invention relates to an analysis method for the microscopic morphology of a porous oxide film on the surface layer of an aluminum foil. The aluminum foil with the surface provided with the acid and alkali resistant aluminum oxide film is subjected to high temperature melting, the aluminum oxide film is peeled, and the microstructure parameters are further analyzed, so that the problems that the porous aluminum oxide is not acid and alkali resistant and is not easy to peel are solved, and the analysis accuracy of the microstructure is improved.
Example 2.
The specific operation steps are as follows:
taking phosphoric acid for anodic oxidation treatment of aluminum foil raw material, wherein the pore diameter of the surface layer porous alumina micropores is 70-80nm, and the thickness is about 1500-2000 nm.
(1) The aluminum foil was cut into sample pieces having a width of 0.5cm and a length of 2.5 cm.
(2) And placing the sample into a clean crucible, fixing the sample by using two ceramic plates, and keeping the sample vertically standing in the crucible, wherein the long edge of the formed pre-treatment aluminum foil sample is vertical to the bottom of the heating container.
(3) And (3) placing the crucible with the sample wafer in a muffle furnace, and treating for 60min at 830-840 ℃.
(4) And taking out the oxide film for later use after cooling.
(5) The separated porous oxide film is analyzed by a scanning electron microscope to obtain a microscopic morphology SEM picture, which is shown in FIGS. 3-4. As can be seen from FIGS. 3-4, the microscopic morphology is highly accurate.
The invention relates to an analysis method for the microscopic morphology of a porous oxide film on the surface layer of an aluminum foil. The aluminum foil with the surface provided with the acid and alkali resistant aluminum oxide film is subjected to high temperature melting, the aluminum oxide film is peeled, and the microstructure parameters are further analyzed, so that the problems that the porous aluminum oxide is not acid and alkali resistant and is not easy to peel are solved, and the analysis accuracy of the microstructure is improved.
Example 3.
The specific operation steps are as follows:
taking phosphoric acid for anodic oxidation treatment of aluminum foil raw material, wherein the pore diameter of the surface layer porous alumina micropores is 70-80nm, and the thickness is about 1500-2000 nm.
(1) The aluminum foil was cut into sample pieces having a width of 1.0cm and a length of 4.0 cm.
(2) And placing the sample into a clean crucible, fixing the sample by using two ceramic plates, and keeping the sample vertically standing in the crucible, wherein the long edge of the formed pre-treatment aluminum foil sample is vertical to the bottom of the heating container.
(3) The crucible with the sample wafer is placed in a muffle furnace for 10min at 1000 ℃.
(4) And taking out the oxide film for later use after cooling.
(5) The separated porous oxide film is placed in a scanning electron microscope for analysis, and the micro-morphology is good and the accuracy is high.
The invention relates to an analysis method for the microscopic morphology of a porous oxide film on the surface layer of an aluminum foil. The aluminum foil with the surface provided with the acid and alkali resistant aluminum oxide film is subjected to high temperature melting, the aluminum oxide film is peeled, and the microstructure parameters are further analyzed, so that the problems that the porous aluminum oxide is not acid and alkali resistant and is not easy to peel are solved, and the analysis accuracy of the microstructure is improved.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (5)
1. The method for analyzing the microscopic morphology of the porous oxide film on the surface layer of the aluminum foil is characterized by comprising the following steps of:
carrying out high-temperature melting treatment on the formation pretreatment aluminum foil sample, wherein a certain included angle is formed between the formation pretreatment aluminum foil sample and the bottom of a heating container in the treatment process, aluminum liquid flows to the lower part under the action of gravity, and after cooling, aluminum is separated from aluminum oxide to obtain a porous oxide film;
analyzing the porous oxide film by adopting a scanning electron microscope or an electronic lens to obtain a microscopic morphology;
wherein the temperature of the high-temperature melting treatment is 700-1000 ℃, and the time is 10-60min.
2. The analytical method according to claim 1,
the width of the aluminum foil sample before formation treatment is 0.5-1.5cm, and the length is 2.5-5.0 cm.
3. The analytical method according to claim 1,
the long edge of the formation pretreatment aluminum foil sample is vertical to the bottom of the heating container.
4. The analytical method according to claim 3,
in the high-temperature melting treatment process: and fixing the formation pretreatment aluminum foil sample by using a ceramic chip, and keeping the formation pretreatment aluminum foil sample vertical to the bottom of the heating container.
5. The analytical method according to claim 1,
in the analysis process, the aperture of the micropores of the porous oxide film is larger than 50nm and is analyzed by a scanning electron microscope; the pore diameter of the micropores of the porous oxide film is less than 50nm and is analyzed by an electron lens.
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| CN100436654C (en) * | 2005-01-28 | 2008-11-26 | 厦门大学 | Porous aluminium oxide template preparing method and its apparatus |
| CN101210337B (en) * | 2006-12-29 | 2010-08-25 | 新疆众和股份有限公司 | Method for stripping oxide film of nano aluminum anode |
| CN101211697B (en) * | 2006-12-30 | 2011-06-22 | 新疆众和股份有限公司 | Electrolytic capacitor aluminum foil oxidation film stripping liquid and microscopic appearance measurement method |
| CN101603193A (en) * | 2009-07-10 | 2009-12-16 | 中国科学院电工研究所 | A kind of method of peeling anodic aluminum oxide film |
| CN102891012A (en) * | 2012-09-14 | 2013-01-23 | 朱健雄 | Method for manufacturing amorphous oxidation film aluminum foil |
| CN104404597A (en) * | 2014-11-10 | 2015-03-11 | 常毅 | Preparation method of porous alpha-alumina membrane |
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