CN113670684A - Novel aluminum alloy anode film coating liquid and testing method thereof - Google Patents
Novel aluminum alloy anode film coating liquid and testing method thereof Download PDFInfo
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- CN113670684A CN113670684A CN202110889884.0A CN202110889884A CN113670684A CN 113670684 A CN113670684 A CN 113670684A CN 202110889884 A CN202110889884 A CN 202110889884A CN 113670684 A CN113670684 A CN 113670684A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/18—After-treatment, e.g. pore-sealing
- C25D11/20—Electrolytic after-treatment
- C25D11/22—Electrolytic after-treatment for colouring layers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
Abstract
The invention relates to a novel aluminum alloy anode membrane-coating liquid and a test method thereof, wherein the anode membrane-coating liquid comprises 0.5-2% of hydrofluoric acid, 0.5-2% of fluoboric acid, 17-29% of absolute ethyl alcohol and 70-79% of deionized water; the test method comprises the following steps: firstly, sequentially pouring 70-79% of deionized water, 17-29% of absolute ethyl alcohol, 0.5-2% of fluoboric acid and 0.5-2% of hydrofluoric acid into an anode film coating device, fixing a sample in the anode film coating device and connecting the sample with an anode, starting the anode film coating device, selecting anodic oxidation time according to different samples, and finally taking out the sample to observe the color metallographic structure of the sample under a polarization microscope; the anode film-coating liquid only contains a small amount of fluoboric acid and hydrofluoric acid, the main reagent solution is deionized water and absolute ethyl alcohol, the operating personnel is safe, and the testing method has the advantages of easy operation, high success rate, excellent effect, long service life and capability of clearly and completely displaying the crystal boundary.
Description
Technical Field
The invention relates to the technical field of electrolysis, in particular to a novel aluminum alloy anode membrane coating solution and a test method thereof.
Background
The properties of the metal material such as strength, hardness and the like are directly and closely related to the internal structure of the metal material, and metallographic observation is the most direct, effective and common method for researching the internal structure of the metal material. Metallographic phases refer to the chemical and physical state of the chemical constituents of a metal within the metal. Through metallographic analysis, the metal performance can be predicted and judged, and the failure and damage reasons can be analyzed.
The color metallographic technique is one of metallographic analysis techniques, and forms a layer of interference films with different thicknesses on the surface of metal by a chemical or physical method, wherein the interference films with different thicknesses have different reflected wavelengths under the interference effect of light and show complementary colors of respective coherent wavelengths, so that different parts of the metal show different colors.
Firstly, mechanically grinding or manually grinding a metal sample, then preparing a metallographic specimen by matching mechanical polishing with electrolytic polishing on the ground sample, and finally carrying out anode film coating; although there is also an anodic film-coating solution on the market, for example, there is a preparation method of 6061 aluminum alloy metallographic specimen disclosed in prior art 201911308913.9, in which the anodic film-coating solution is prepared from sulfuric acid, phosphoric acid and water according to a volume ratio of 38:43:19, which is not only bad in effect and unable to clearly observe the crystal grain structure, but also is easy to be dangerous because both sulfuric acid and phosphoric acid have strong corrosivity and are careless in operation.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a novel aluminum alloy anode coating solution and a test method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: a novel aluminum alloy anode membrane-coating liquid comprises 0.5-2% of hydrofluoric acid, 0.5-2% of fluoboric acid, 17-29% of absolute ethyl alcohol and 70-79% of deionized water.
Preferably, the hydrofluoric acid has a concentration of 40% by volume.
Preferably, the fluoroboric acid has a volume concentration of 48%.
Preferably, the volume concentration of the absolute ethyl alcohol is 99.5%.
The invention also discloses a test method of the novel aluminum alloy anode membrane-coating liquid, which is characterized by comprising the following steps: the method comprises the following steps:
s1: pouring 70-79% of deionized water into a container of an anode laminating device;
s2: pouring 17-29% of absolute ethyl alcohol into deionized water;
s3: 0.5 to 2 percent of fluoboric acid is taken and poured into the mixed liquid of S2;
s4: pouring 0.5-2% of hydrofluoric acid into the mixed liquid of S3 to obtain a novel aluminum alloy anode membrane-coating liquid;
s5: fixing the sample in an anode film covering device and connecting the sample with the anode;
s6: starting an anode film covering device, and selecting anodic oxidation time according to different samples;
s7: after the oxidation was complete, the sample was removed, rinsed with deionized water, then rinsed with alcohol, air dried, and finally the color metallographic structure of the sample was observed under a polarizing microscope.
Preferably, the container is made of PP material.
Preferably, the sample is connected to the positive electrode by a conductive clamping device.
Preferably, the negative electrode of the anode coating device is made of 304 stainless steel plate.
Preferably, the voltage of the anode coating device is 45-50V, and before the anode coating device is started, the power supply must be turned off.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
the anode film-coating liquid only contains a small amount of fluoboric acid and hydrofluoric acid, the main reagent solution is deionized water and absolute ethyl alcohol, the operating personnel is safe, the testing method is easy to operate, has extremely high success rate, excellent effect and long service life, can clearly and completely display crystal boundaries, and is almost suitable for aluminum alloy samples of various series and different shapes.
Drawings
The technical scheme of the invention is further explained by combining the accompanying drawings as follows:
FIG. 1 is a photograph showing the grain structure of a 1-series aluminum bar sliced sample according to the present invention;
FIG. 2 is a photograph showing the grain structure of a 3-series aluminum bar sliced sample according to the present invention;
FIG. 3 is a photograph showing the grain structure of a 6-series aluminum bar sliced sample according to the present invention;
FIG. 4 is a photograph of the grain structure of a microchannel flat tube sample in accordance with the present invention;
FIG. 5 is a photograph showing the grain structure of a 3-series alloy light pipe sample according to the present invention;
FIG. 6 is a photograph showing the grain structure of a 3-series alloy high-tooth pipe sample according to the present invention.
Detailed Description
The invention is described in further detail below with reference to the figures and the embodiments.
The first embodiment is as follows:
s1: pouring 720ml to 740ml of deionized water into a PP material container of an anode laminating device;
s2: pouring 240ml of absolute ethyl alcohol into deionized water;
s3: pouring 10-20 ml of fluoboric acid into the mixed liquid of S2;
s4: pouring 10-20 ml of hydrofluoric acid into the mixed liquid of S3 to obtain a novel aluminum alloy anode coating liquid;
s5: fixing a 1-series aluminum bar slice sample in an anode film coating device, and clamping the sample by a conductive clamping device connected with an anode;
s6: starting the anode film coating device, setting the anodic oxidation time to be 2-3 min, wherein the voltage of the anode film coating device is 48V, before the anode film coating device is started, a power supply needs to be turned off, and the cathode is made of 304 stainless steel plates, so that the anode film coating device is cheap and easy to obtain and has a good effect;
s7: after the oxidation is finished, the 1-series aluminum rod slice sample is taken out, washed by deionized water, then washed by alcohol, dried by air, and finally observed under a polarizing microscope to obtain a sample color metallographic structure, and a grain structure picture is taken, wherein the grain boundary structure of the 1-series aluminum rod slice sample is clear as shown in fig. 1.
Example two:
s1: pouring 720ml to 740ml of deionized water into a PP material container of an anode laminating device;
s2: pouring 240ml of absolute ethyl alcohol into deionized water;
s3: pouring 10-20 ml of fluoboric acid into the mixed liquid of S2;
s4: pouring 10-20 ml of hydrofluoric acid into the mixed liquid of S3 to obtain a novel aluminum alloy anode coating liquid;
s5: fixing a 3-series aluminum bar slice sample in an anode film coating device, and clamping the sample by a conductive clamping device connected with the anode;
s6: starting the anode film coating device, setting the anodic oxidation time to be 2-3 min, wherein the voltage of the anode film coating device is 48V, before the anode film coating device is started, a power supply needs to be turned off, and the cathode is made of 304 stainless steel plates, so that the anode film coating device is cheap and easy to obtain and has a good effect;
s7: after the oxidation is finished, the 3-series aluminum rod slice sample is taken out, washed by deionized water, then washed by alcohol, dried by air, and finally observed under a polarizing microscope to obtain a sample color metallographic structure, and a grain structure picture is taken, wherein the grain boundary structure of the 3-series aluminum rod slice sample is clear as shown in fig. 2.
Example three:
s1: pouring 720ml to 740ml of deionized water into a PP material container of an anode laminating device;
s2: pouring 240ml of absolute ethyl alcohol into deionized water;
s3: pouring 10-20 ml of fluoboric acid into the mixed liquid of S2;
s4: pouring 10-20 ml of hydrofluoric acid into the mixed liquid of S3 to obtain a novel aluminum alloy anode coating liquid;
s5: fixing a 6-series aluminum bar slice sample in an anode film coating device, and clamping the sample by a conductive clamping device connected with the anode;
s6: starting the anode film coating device, setting the anodic oxidation time to be 2-3 min, wherein the voltage of the anode film coating device is 48V, before the anode film coating device is started, a power supply needs to be turned off, and the cathode is made of 304 stainless steel plates, so that the anode film coating device is cheap and easy to obtain and has a good effect;
s7: after the oxidation is completed, the 6-series aluminum rod slice sample is taken out, washed by deionized water, then washed by alcohol, dried by air, and finally observed under a polarizing microscope to obtain a sample color metallographic structure, and a grain structure picture is taken, so that the 6-series aluminum rod slice sample has a clear grain boundary structure as shown in fig. 3.
Example four:
s1: pouring 720ml to 740ml of deionized water into a PP material container of an anode laminating device;
s2: pouring 240ml of absolute ethyl alcohol into deionized water;
s3: pouring 10-20 ml of fluoboric acid into the mixed liquid of S2;
s4: pouring 10-20 ml of hydrofluoric acid into the mixed liquid of S3 to obtain a novel aluminum alloy anode coating liquid;
s5: fixedly placing a microchannel flat tube sample in an anode film coating device, and clamping the sample by a conductive clamping device connected with the anode;
s6: starting the anode film coating device, setting the anodic oxidation time to be 2-3 min, wherein the voltage of the anode film coating device is 48V, before the anode film coating device is started, a power supply needs to be turned off, and the cathode is made of 304 stainless steel plates, so that the anode film coating device is cheap and easy to obtain and has a good effect;
s7: after the oxidation is finished, taking out the microchannel flat tube sample, washing with deionized water, then washing with alcohol, drying with air, finally observing the color metallographic structure of the sample under a polarizing microscope, and taking a crystal grain structure picture, wherein the crystal grain boundary structure of the microchannel flat tube sample is clear as shown in fig. 4.
Example five:
s1: pouring 720ml to 740ml of deionized water into a PP material container of an anode laminating device;
s2: pouring 240ml of absolute ethyl alcohol into deionized water;
s3: pouring 10-20 ml of fluoboric acid into the mixed liquid of S2;
s4: pouring 10-20 ml of hydrofluoric acid into the mixed liquid of S3 to obtain a novel aluminum alloy anode coating liquid;
s5: fixing a 3-series alloy light tube sample in an anode film coating device, and clamping the sample by a conductive clamping device connected with the anode;
s6: starting the anode film coating device, setting the anodic oxidation time to be 2-3 min, wherein the voltage of the anode film coating device is 48V, before the anode film coating device is started, a power supply needs to be turned off, and the cathode is made of 304 stainless steel plates, so that the anode film coating device is cheap and easy to obtain and has a good effect;
s7: after the oxidation is completed, the 3-series alloy light tube sample is taken out, washed by deionized water, then washed by alcohol, dried by air, and finally observed under a polarizing microscope to obtain a sample color metallographic structure, and a grain structure picture is taken, wherein the grain boundary structure of the 3-series alloy light tube sample is clear as shown in fig. 5.
Example six:
s1: pouring 720ml to 740ml of deionized water into a PP material container of an anode laminating device;
s2: pouring 240ml of absolute ethyl alcohol into deionized water;
s3: pouring 10-20 ml of fluoboric acid into the mixed liquid of S2;
s4: pouring 10-20 ml of hydrofluoric acid into the mixed liquid of S3 to obtain a novel aluminum alloy anode coating liquid;
s5: fixing a 3-series alloy high-tooth pipe sample in an anode film coating device, and clamping the sample by a conductive clamping device connected with the anode;
s6: starting the anode film coating device, setting the anodic oxidation time to be 2-3 min, wherein the voltage of the anode film coating device is 48V, before the anode film coating device is started, a power supply needs to be turned off, and the cathode is made of 304 stainless steel plates, so that the anode film coating device is cheap and easy to obtain and has a good effect;
s7: after the oxidation is completed, the 3-series alloy high-tooth pipe sample is taken out, washed by deionized water, then washed by alcohol, dried by air, and finally observed under a polarizing microscope for the color metallographic structure of the sample, and a picture of the grain structure is taken, wherein the grain boundary structure of the 3-series alloy high-tooth pipe sample is clear as shown in fig. 6.
The above is only a specific application example of the present invention, and the protection scope of the present invention is not limited in any way. All the technical solutions formed by equivalent transformation or equivalent replacement fall within the protection scope of the present invention.
Claims (9)
1. The novel aluminum alloy anode membrane-coating solution is characterized in that: comprises 0.5 to 2 percent of hydrofluoric acid, 0.5 to 2 percent of fluoboric acid, 17 to 29 percent of absolute ethyl alcohol and 70 to 79 percent of deionized water.
2. The novel aluminum alloy anode membrane-coating solution of claim 1, which is characterized in that: the volume concentration of the hydrofluoric acid is 40%.
3. The novel aluminum alloy anode membrane-coating solution of claim 1, which is characterized in that: the volume concentration of the fluoboric acid is 48 percent.
4. The novel aluminum alloy anode membrane-coating solution of claim 1, which is characterized in that: the volume concentration of the absolute ethyl alcohol is 99.5%.
5. The method for testing the novel aluminum alloy anode coating solution according to any one of claims 1 to 4, wherein the method comprises the following steps: the method comprises the following steps:
s1: pouring 70-79% of deionized water into a container of an anode laminating device;
s2: pouring 17-29% of absolute ethyl alcohol into deionized water;
s3: 0.5 to 2 percent of fluoboric acid is taken and poured into the mixed liquid of S2;
s4: pouring 0.5-2% of hydrofluoric acid into the mixed liquid of S3 to obtain a novel aluminum alloy anode membrane-coating liquid;
s5: fixing the sample in an anode film covering device and connecting the sample with the anode;
s6: starting an anode film covering device, and selecting anodic oxidation time according to different samples;
s7: after the oxidation was complete, the sample was removed, rinsed with deionized water, then rinsed with alcohol, air dried, and finally the color metallographic structure of the sample was observed under a polarizing microscope.
6. The testing method of the novel aluminum alloy anode membrane-coating solution according to claim 5, characterized in that: the container is made of PP materials.
7. The testing method of the novel aluminum alloy anode membrane-coating solution according to claim 5, characterized in that: the sample is connected with the anode through a conductive clamping device.
8. The testing method of the novel aluminum alloy anode membrane-coating solution according to claim 5, characterized in that: the cathode of the anode film covering device is made of a 304 stainless steel plate.
9. The testing method of the novel aluminum alloy anode membrane-coating solution according to claim 5, characterized in that: the voltage of the anode film coating device is 45-50V, and before the anode film coating device is started, the power supply must be turned off.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110073272A1 (en) * | 2009-09-28 | 2011-03-31 | Fujifilm Corporation | Method of producing aluminum substrate for planographic printing plate and method of recycling planographic printing plate |
| 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 |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110073272A1 (en) * | 2009-09-28 | 2011-03-31 | Fujifilm Corporation | Method of producing aluminum substrate for planographic printing plate and method of recycling planographic printing plate |
| 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 |
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