CN110208304A - A kind of analysis method of aluminium foil surface layer porous oxide film microscopic appearance - Google Patents
A kind of analysis method of aluminium foil surface layer porous oxide film microscopic appearance Download PDFInfo
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- CN110208304A CN110208304A CN201910520669.6A CN201910520669A CN110208304A CN 110208304 A CN110208304 A CN 110208304A CN 201910520669 A CN201910520669 A CN 201910520669A CN 110208304 A CN110208304 A CN 110208304A
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- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B15/00—Measuring arrangements characterised by the use of electromagnetic waves or particle radiation, e.g. by the use of microwaves, X-rays, gamma rays or electrons
- G01B15/04—Measuring arrangements characterised by the use of electromagnetic waves or particle radiation, e.g. by the use of microwaves, X-rays, gamma rays or electrons for measuring contours or curvatures
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
- G01N23/04—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/2005—Preparation of powder samples therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
Abstract
The present invention is a kind of analysis method of aluminium foil surface layer porous oxide film microscopic appearance.A kind of analysis method of aluminium foil surface layer porous oxide film microscopic appearance, the following steps are included: chemical conversion pre-treatment aluminium foil print is carried out high-temperature digestion processing, chemical conversion pre-treatment aluminium foil print described in treatment process forms an angle with heating container bottom shape, under the effect of gravity, molten aluminum flows to the lower part, after cooling, aluminium is separated with aluminium oxide, obtains porous oxide film；The porous oxide film is placed in scanning electron microscope or electron lens is analyzed, obtains microscopic appearance parameter.A kind of analysis method of aluminium foil surface layer porous oxide film microscopic appearance of the present invention, high-temperature digestion is passed through with not acid and alkali-resistance type aluminum oxide film aluminium foil to surface, pellumina is removed, further analysis obtains microscopic appearance parameter, provides data for research chemical conversion mechanism and supports.And stripping process is simple, and it is easily controllable, suitable for the analysis of surface layer porous oxide film microscopic appearance, carry out basic research.
Description
Technical field
Present invention relates particularly to a kind of analysis methods of aluminium foil surface layer porous oxide film microscopic appearance.
Background technique
(boiling water boiling or anodic oxidation) is handled before aluminium foil is melted into industry, generating aperture is 5-200nm, 30-800nm thick
Porous oxide film, after being melted into, this layer of porous oxide film is partially converted into dense oxidation film, makees electrolytic capacitor dielectric film.
This layer of porous oxide film and Waste Acid From Hua Cheng Foil quality index are maintained close ties with.
In the prior art, it takes alkaline etching method to remove aluminium foil surface oxidation film, then is analyzed with scanning electron microscope or electron lens,
It can get oxidation film microscopic appearance parameter.But there is problems in that since amorphous alumina, crystalline aluminum oxide are dissolved in
In lye, crystal type aluminum oxyhydroxide is alkaline-resisting acidproof, therefore alkaline etching method is only effective to the film comprising crystal type aluminum oxyhydroxide, i.e.,
Alkaline etching method can not remove the film of amorphous alumina, crystalline aluminum oxide.Therefore, (crystallization can only be mainly contained to aluminium foil after chemical conversion
Type aluminum oxyhydroxide) take alkaline etching method removing chemical conversion aluminium foil surface oxidation film；It is analyzed, is obtained with scanning electron microscope or electron lens again
Microscopic appearance parameter.Chemical conversion pre-treatment aluminium foil surface porous aluminas film component is amorphous alumina, and wherein micropore size is
5-200nm, thickness are about 30-2000nm；Ineffective acid solution or lye dissolve aluminium, can dissolve oxidation film simultaneously, stripping is not achieved
Effect from oxidation film.
In view of this, the invention reside in provide a kind of analysis method of new aluminium foil surface layer porous oxide film microscopic appearance.
Summary of the invention
The purpose of the present invention is to provide a kind of analysis method of aluminium foil surface layer porous oxide film microscopic appearance, it is suitable for changing
At preceding aluminium foil, solve the problems, such as porous aluminas not acid and alkali-resistance, be not easily stripped, Morphology analysis accuracy is improved, for research
It is melted into mechanism and data support is provided.
To achieve the goals above, used technical solution:
A kind of analysis method of aluminium foil surface layer porous oxide film microscopic appearance, comprising the following steps:
Chemical conversion pre-treatment aluminium foil print is subjected to high-temperature digestion processing, chemical conversion pre-treatment aluminium foil sample described in treatment process
Piece forms an angle with heating container bottom shape, and under the effect of gravity, molten aluminum flows to the lower part, after cooling, aluminium and aluminium oxide point
From obtaining porous oxide film；
The porous oxide film is placed in scanning electron microscope or electron lens is analyzed, obtains microscopic appearance parameter.
Further, the wide 0.5-1.5cm of chemical conversion pre-treatment aluminium foil print, long 2.5-5.0cm.
Further, the long side of the chemical conversion pre-treatment aluminium foil print is vertical with heating container bottom.
Further, in the high-temperature digestion treatment process: using the fixed chemical conversion pre-treatment aluminium of potsherd
Foil sample keeps chemical conversion pre-treatment aluminium foil print vertical with heating container bottom.
Further, the temperature of high-temperature digestion processing is 700-1000 DEG C, time 10-60min.
Further, in the analytic process, porous oxide film micropore size is greater than 50nm and uses scanning electron microscope analysis；
It is analyzed as porous oxide film micropore size is less than 50nm using electron lens.
Compared with prior art, the invention has the beneficial effects that:
1, the present invention uses high-temperature digestion aluminium, and print is disposed vertically, and under the effect of gravity, molten aluminum flows to lower end, from
And achievees the purpose that aluminium and separated with aluminium oxide；The pellumina isolated is placed under Electronic Speculum and is analyzed, can be obtained microscopic appearance
Parameter.
2, high temperature of the invention removing oxidation membrane process is simple, easy to operate.Its material therefor, market are commercially available；
Scanning electron microscope or electron lens analysis are identical as generic way.
3, the present invention can analyze not acid and alkali-resistance pellumina pattern, to research aluminium foil chemical conversion mechanism, promote Waste Acid From Hua Cheng Foil product
Quality is significant.
Detailed description of the invention
Fig. 1 is that the SEM of 1 aluminium foil surface layer porous oxide film of embodiment schemes；
Fig. 2 is that the SEM of 1 aluminium foil surface layer porous oxide film of embodiment schemes；
Fig. 3 is that the SEM of 2 aluminium foil surface layer porous oxide film of embodiment schemes；
Fig. 4 is that the SEM of 2 aluminium foil surface layer porous oxide film of embodiment schemes.
Specific embodiment
In order to which the present invention is further explained, a kind of analysis method of aluminium foil surface layer porous oxide film microscopic appearance, reaches expected
Goal of the invention, in conjunction with the preferred embodiment, to a kind of aluminium foil surface layer porous oxide film microscopic appearance proposed according to the present invention
Analysis method, specific embodiment, structure, feature and its effect, detailed description is as follows.In the following description, different
What " embodiment " or " embodiment " referred to is not necessarily the same embodiment.In addition, special characteristic, knot in one or more embodiments
Structure or feature can be combined by any suitable form.
A kind of aluminium foil surface layer porous oxide film microscopic appearance of the present invention is divided below in conjunction with specific embodiment and Fig. 1-4
Analysis method is further described in detail:
The technical solution of the present invention is as follows:
Chemical conversion pre-treatment aluminium foil print is subjected to high-temperature digestion processing, chemical conversion pre-treatment aluminium foil sample described in treatment process
Piece forms an angle with heating container bottom shape, and under the effect of gravity, molten aluminum flows to the lower part, after cooling, aluminium and aluminium oxide point
From obtaining porous oxide film.(reaching removing porous oxide film purpose)
The porous oxide film is placed in scanning electron microscope or electron lens is analyzed, obtains microscopic appearance parameter.
Preferably, the wide 0.5-1.5cm of chemical conversion pre-treatment aluminium foil print, the long 2.5-5.0cm.
Preferably, the long side of the chemical conversion pre-treatment aluminium foil print is vertical with heating container bottom.It is flowed conducive to molten aluminum,
Enhancing and aluminium oxide separating effect
It is further preferred that in the high-temperature digestion treatment process: using the fixed chemical conversion pre-treatment of potsherd
Aluminium foil sample keeps chemical conversion pre-treatment aluminium foil print vertical with heating container bottom.
Preferably, the temperature of high-temperature digestion processing is 700-100 DEG C, time 10-60min, can rapidly sufficiently
Melt chemical conversion pre-treatment foil samples.
Preferably, in the analytic process, porous oxide film micropore size is greater than 50nm and uses scanning electron microscope analysis；Such as
Porous oxide film micropore size is less than 50nm and is analyzed using electron lens.
Heretofore described chemical conversion pre-treatment aluminium foil refers to carrying out the aluminium foil before chemical conversion treatment.
Embodiment 1.
Specific steps are as follows:
Take sulphuric acid anodizing processing aluminium foil raw material as chemical conversion pre-treatment aluminium foil, surface layer porous aluminas micropore size
For 5-20nm, thickness is about 600-700nm.
(1) chemical conversion pre-treatment aluminium foil is cut into the chemical conversion pre-treatment aluminium foil print of wide 1.5cm, long 5.0cm, abbreviation sample
Piece.
(2) print is placed in clean crucible, fixes print with two panels potsherd, print is kept vertically to stand in crucible,
The long side for being wherein melted into pre-treatment aluminium foil print is vertical with heating container bottom.
(3) it will be placed in Muffle furnace equipped with print crucible, 700-1000 DEG C of processing 30min.
(4) oxidation film is taken out after cooling, it is spare.
(5) isolated porous oxide film is placed in electron lens to analyze, can get microscopic appearance SEM photograph, Fig. 1-
2.By Fig. 1-2 it is found that microscopic appearance accuracy is high.
A kind of analysis method of aluminium foil surface layer porous oxide film microscopic appearance of the present invention, is melted into using high-temperature digestion
Aluminium in pre-treatment aluminium foil, under the effect of gravity, molten aluminum flows to the lower part, and after cooling, aluminium is separated with aluminium oxide, separates porous oxygen
Change film.By passing through high-temperature digestion with not acid and alkali-resistance type aluminum oxide film aluminium foil to surface, pellumina is removed, further
Analysis obtains microscopic appearance parameter, solve the problems, such as porous aluminas not acid and alkali-resistance, be not easily stripped, it is quasi- to improve Morphology analysis
True property.
Embodiment 2.
Specific steps are as follows:
Phosphoric acid anodizing is taken to handle aluminium foil raw material, surface layer porous aluminas micropore size is 70-80nm, and thickness is about
1500-2000nm。
(1) aluminium foil is cut into width 0.5cm, length 2.5cm print.
(2) print is fixed print with two panels potsherd, print is kept vertically to stand in crucible as in clean crucible,
The long side for being wherein melted into pre-treatment aluminium foil print is vertical with heating container bottom.
(3) it will be placed in Muffle furnace equipped with print crucible, and handle 60min at 830-840 DEG C.
(4) oxidation film is taken out after cooling, it is spare.
(5) isolated porous oxide film is placed in scanning electron microscope to analyze, can get microscopic appearance SEM photograph, Fig. 3-
4.By Fig. 3-4 it is found that microscopic appearance accuracy is high.
A kind of analysis method of aluminium foil surface layer porous oxide film microscopic appearance of the present invention, is melted into using high-temperature digestion
Aluminium in pre-treatment aluminium foil, under the effect of gravity, molten aluminum flows to the lower part, and after cooling, aluminium is separated with aluminium oxide, separates porous oxygen
Change film.By passing through high-temperature digestion with not acid and alkali-resistance type aluminum oxide film aluminium foil to surface, pellumina is removed, further
Analysis obtains microscopic appearance parameter, solve the problems, such as porous aluminas not acid and alkali-resistance, be not easily stripped, it is quasi- to improve Morphology analysis
True property.
Embodiment 3.
Specific steps are as follows:
Phosphoric acid anodizing is taken to handle aluminium foil raw material, surface layer porous aluminas micropore size is 70-80nm, and thickness is about
1500-2000nm。
(1) aluminium foil is cut into width 1.0cm, length 4.0cm print.
(2) print is fixed print with two panels potsherd, print is kept vertically to stand in crucible as in clean crucible,
The long side for being wherein melted into pre-treatment aluminium foil print is vertical with heating container bottom.
(3) it will be placed in Muffle furnace equipped with print crucible and handle 10min at 1000 DEG C.
(4) oxidation film is taken out after cooling, it is spare.
(5) isolated porous oxide film is placed in scanning electron microscope to analyze, microscopic appearance is good, and accuracy is high.
A kind of analysis method of aluminium foil surface layer porous oxide film microscopic appearance of the present invention, is melted into using high-temperature digestion
Aluminium in pre-treatment aluminium foil, under the effect of gravity, molten aluminum flows to the lower part, and after cooling, aluminium is separated with aluminium oxide, separates porous oxygen
Change film.By passing through high-temperature digestion with not acid and alkali-resistance type aluminum oxide film aluminium foil to surface, pellumina is removed, further
Analysis obtains microscopic appearance parameter, solve the problems, such as porous aluminas not acid and alkali-resistance, be not easily stripped, it is quasi- to improve Morphology analysis
True property.
The above is only the preferred embodiment of the embodiment of the present invention, not makees any shape to the embodiment of the present invention
Limitation in formula, any simple modification to the above embodiments of technical spirit according to an embodiment of the present invention, equivalent variations
With modification, in the range of still falling within technical solution of the embodiment of the present invention.
Claims (6)
1. a kind of analysis method of aluminium foil surface layer porous oxide film microscopic appearance, which comprises the following steps:
Will chemical conversion pre-treatment aluminium foil print carry out high-temperature digestion processing, chemical conversion pre-treatment aluminium foil print described in treatment process with
Heating container bottom shape forms an angle, and under the effect of gravity, molten aluminum flows to the lower part, and after cooling, aluminium is separated with aluminium oxide, is obtained
To porous oxide film；
The porous oxide film is analyzed using scanning electron microscope or electron lens, obtains microscopic appearance.
2. analysis method according to claim 1, which is characterized in that
The wide 0.5-1.5cm of chemical conversion pre-treatment aluminium foil print, the long 2.5-5.0cm.
3. analysis method according to claim 1, which is characterized in that
The long side of the chemical conversion pre-treatment aluminium foil print is vertical with heating container bottom.
4. analysis method according to claim 3, which is characterized in that
In the high-temperature digestion treatment process: using the fixed chemical conversion pre-treatment aluminium foil sample of potsherd, before keeping chemical conversion
It is vertical with heating container bottom to handle aluminium foil print.
5. analysis method according to claim 1, which is characterized in that
The temperature of the high-temperature digestion processing is 700-1000 DEG C, time 10-60min.
6. analysis method according to claim 1, which is characterized in that
In the analytic process, porous oxide film micropore size is greater than 50nm and uses scanning electron microscope analysis；Porous oxide film is micro-
Hole aperture is less than 50nm and is analyzed using electron lens.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110877916A (en) * | 2019-11-27 | 2020-03-13 | 新疆众和股份有限公司 | Method for producing tubular titanium dioxide |
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| CN110877916A (en) * | 2019-11-27 | 2020-03-13 | 新疆众和股份有限公司 | Method for producing tubular titanium dioxide |
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