CN114384102B - Evaluation method for ultrasonically cleaning oxide film on aluminum alloy surface - Google Patents
Evaluation method for ultrasonically cleaning oxide film on aluminum alloy surface Download PDFInfo
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- CN114384102B CN114384102B CN202111500417.0A CN202111500417A CN114384102B CN 114384102 B CN114384102 B CN 114384102B CN 202111500417 A CN202111500417 A CN 202111500417A CN 114384102 B CN114384102 B CN 114384102B
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- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 91
- 238000004140 cleaning Methods 0.000 title claims abstract description 9
- 238000011156 evaluation Methods 0.000 title claims abstract description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052802 copper Inorganic materials 0.000 claims abstract description 22
- 239000010949 copper Substances 0.000 claims abstract description 22
- 239000000523 sample Substances 0.000 claims abstract description 17
- 150000001879 copper Chemical class 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000012266 salt solution Substances 0.000 claims abstract description 12
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 11
- 238000005498 polishing Methods 0.000 claims abstract description 8
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 7
- 238000009826 distribution Methods 0.000 claims abstract description 7
- 230000003647 oxidation Effects 0.000 claims abstract description 7
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 7
- 238000006073 displacement reaction Methods 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 6
- 229910003460 diamond Inorganic materials 0.000 claims description 4
- 239000010432 diamond Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 3
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 5
- 239000000463 material Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 229920000426 Microplastic Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000035876 healing Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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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]
-
- 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
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
- Sampling And Sample Adjustment (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
An evaluation method for ultrasonically cleaning an oxide film on the surface of an aluminum alloy belongs to the field of aluminum alloys. The method comprises the following steps: 1) Placing the fixed table in the container; 2) Polishing the lower surface of the aluminum alloy, and then carrying out natural oxidation treatment to form a compact oxide film on the lower surface of the aluminum alloy; 3) Placing the oxidized aluminum alloy on a fixed table; 4) Pouring copper salt solution into the container, wherein the liquid level exceeds the upper surface of the aluminum alloy; 5) Vertically contacting an ultrasonic probe with the upper surface of the aluminum alloy, performing ultrasonic treatment, wherein in the ultrasonic treatment process, a compact oxide film on the lower surface of the aluminum alloy is damaged, the aluminum alloy leaks out, aluminum and copper salt solution undergo a displacement reaction, and copper is attached to the lower surface of the aluminum alloy; 6) Taking a distribution picture of copper element by using a scanning electron microscope or an electronic probe; 7) The area occupied by copper element was analyzed by image processing. The invention evaluates the effect of ultrasonic cleaning of the oxide film on the surface of the aluminum alloy by comparing the occupied areas of copper elements before and after ultrasonic treatment.
Description
Technical Field
The invention belongs to the field of aluminum alloy, and relates to an evaluation method for ultrasonically cleaning an oxide film on the surface of an aluminum alloy.
Background
The small-size homogeneous materials are connected through means of surface processing, clean assembly, high-temperature deformation and the like, so that high-quality and large-size products are prepared, and the metallurgical defects of macrosegregation, shrinkage porosity, shrinkage cavity and the like of large castings are overcome. However, a dense oxide film exists on the surface of the aluminum alloy, which can prevent the interface from healing in the homogeneous hot-pressing diffusion connection process.
When the intensity of ultrasonic waves exceeds a certain critical value, the dislocation structure in the material can be changed, and the dislocation is moved, so that micro plastic deformation, namely the 'sound plastic effect' of the ultrasonic waves, occurs in the material. The periodic vibration of ultrasonic waves can lead the continuous and compact brittle oxide film on the surface of the aluminum alloy not to deform along with the aluminum alloy matrix, thereby breaking the oxide film and achieving the purpose of cleaning the oxide film on the surface of the aluminum alloy.
However, as the growth speed of the aluminum alloy oxide film is extremely high, after the aluminum alloy surface oxide film is broken, the newly leaked aluminum alloy surface can be rapidly oxidized in the air within a few seconds, so that no corresponding method is used for evaluating the effect of ultrasonic cleaning of the aluminum alloy surface oxide film at present.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for evaluating the effect of ultrasonically cleaning an oxide film on the surface of an aluminum alloy.
The invention adopts the technical scheme that:
an evaluation method for ultrasonically cleaning an oxide film on the surface of an aluminum alloy comprises the following steps:
(1) A fixing table 5 is placed on the inner bottom surface of the container 4 for fixing the aluminum alloy 2 thereon; the fixed table 5 is of a frame strip structure.
(2) The lower surface of the aluminum alloy 2 is subjected to grinding and polishing treatment, then natural oxidation treatment is carried out, and a compact oxide film is formed on the lower surface of the aluminum alloy 2.
(3) The oxidized aluminum alloy 2 is placed on the fixed table 5, and the lower surface thereof is not completely contacted with the fixed table 5.
(4) The container 4 is filled with a saturated copper salt solution 3, and the liquid level exceeds the upper surface of the aluminum alloy 2.
(5) Vertically contacting the ultrasonic probe 1 with the upper surface of the aluminum alloy 2, and performing ultrasonic treatment with ultrasonic power of 30W-150W for 1-3 min; in the ultrasonic treatment process, a compact oxide film at a non-contact part of the lower surface of the aluminum alloy 2 and the fixed table 5 is broken, the aluminum alloy 2 leaks out, and the aluminum and the saturated copper salt solution 3 undergo a displacement reaction, so that copper is attached to the lower surface of the aluminum alloy 2.
(6) Taking out the aluminum alloy 2, and taking a distribution photo of copper elements on the lower surface of the aluminum alloy 2 by using a scanning electron microscope or an electronic probe; the area percentage occupied by the copper element is analyzed through image processing, the area percentage of aluminum on the surface of the aluminum alloy is obtained through conversion of the area percentage of the copper element (the area percentage of the copper element and the aluminum alloy are in equal proportion), and then the judgment result after ultrasonic cleaning is obtained (the oxide film on the surface of the aluminum alloy is evaluated).
Further, in the step (2), the thickness of the aluminum alloy 2 is 5-10 mm.
Further, in the step (2), the grinding and polishing process is to coarsely grind the aluminum alloy 2 by using 240# abrasive paper, then finely grind the aluminum alloy by using 600# abrasive paper, 1000# abrasive paper, 1500# abrasive paper and 2000# abrasive paper in sequence, and change the abrasive paper when the scratch directions are consistent each time, and grind samples along the vertical scratch directions. After fine grinding, polishing was performed with a diamond paste having a particle size of 1.5.
Further, in the step (2), the natural oxidation treatment is to put the polished aluminum alloy 2 into air and oxidize for 10-120 min.
Further, the copper salt solution 3 in the step (4) is one of a copper sulfate solution and a copper chloride solution.
Further, in the step (5), the ultrasonic probe 1 is a stainless steel probe.
Compared with the prior art, the invention has the beneficial effects that: the effect of ultrasonic cleaning of the oxide film on the surface of the aluminum alloy can be evaluated by analyzing the area occupied by the copper element on the surface of the sample after the aluminum alloy is subjected to ultrasonic treatment and substitution reaction with copper salt solution.
Drawings
FIG. 1 is a schematic diagram of an apparatus for ultrasonically cleaning an oxide film on an aluminum alloy surface; in the figure: 1 ultrasonic probe, 2 aluminum alloy, 3 copper salt solution, 4 container and 5 fixing table;
FIG. 2 is a photograph showing the distribution of copper on the lower surface of the aluminum alloy in example 1 of the present invention;
FIG. 3 is a photograph showing the distribution of copper elements on the lower surface of the aluminum alloy after ultrasonic treatment in example 2 of the present invention.
Detailed Description
The invention is further illustrated with reference to specific examples.
Example 1
The stationary table 5 is placed in the container 4. The 5mm thick aluminum alloy 2 is coarsely ground by 240# abrasive paper, then the aluminum alloy 2 is finely ground by 600# abrasive paper, 1000# abrasive paper, 1500# abrasive paper and 2000# abrasive paper in sequence, and the abrasive paper is replaced when the scratch directions are consistent each time, and samples are ground along the vertical scratch directions. After fine grinding, polishing was performed with a diamond paste having a particle size of 1.5. And then carrying out natural oxidation treatment for 10min to form a compact oxide film on the lower surface of the aluminum alloy 2. The oxidized aluminum alloy 2 is placed on a stationary table 5. The container 4 is filled with a saturated copper sulfate solution, and the liquid level exceeds the upper surface of the aluminum alloy 2. The stainless steel ultrasonic probe 1 is vertically contacted with the upper surface of the aluminum alloy 2, the ultrasonic power is 30W, and the treatment time is 3min. In the treatment process, a compact oxide film on the lower surface of the aluminum alloy 2 is damaged, the aluminum alloy 2 leaks out, the aluminum and the saturated copper salt solution 3 undergo a displacement reaction, and copper is attached to the lower surface of the aluminum alloy 2. A photograph of the distribution of copper element on the lower surface of the aluminum alloy 2 was taken using a scanning electron microscope, as shown in fig. 2. The area percentage occupied by copper elements before and after ultrasonic treatment is respectively 0.47 percent and 13.92 percent through image processing analysis, and the surface oxide film of the aluminum alloy with the area percentage of 13.45 percent is cleaned through ultrasonic treatment through conversion.
Example 2
The stationary table 5 is placed in the container 4. The aluminum alloy 2 with the thickness of 10mm is coarsely ground by adopting 240# abrasive paper, then the aluminum alloy 2 is finely ground by adopting 600# abrasive paper, 1000# abrasive paper, 1500# abrasive paper and 2000# abrasive paper in sequence, and the abrasive paper is replaced when the scratch directions are consistent each time, and the sample is ground along the vertical scratch directions. After fine grinding, polishing was performed with a diamond paste having a particle size of 1.5. And then carrying out natural oxidation treatment for 120min to form a compact oxide film on the lower surface of the aluminum alloy 2. The oxidized aluminum alloy 2 is placed on a stationary table 5. The container 4 is filled with a saturated copper chloride solution, and the liquid level exceeds the upper surface of the aluminum alloy 2. The stainless steel ultrasonic probe 1 is vertically contacted with the upper surface of the aluminum alloy 2, the ultrasonic power is 150W, and the treatment time is 1min. In the treatment process, a compact oxide film on the lower surface of the aluminum alloy 2 is damaged, the aluminum alloy 2 leaks out, the aluminum and the saturated copper salt solution 3 undergo a displacement reaction, and copper is attached to the lower surface of the aluminum alloy 2. A photograph of the distribution of copper element on the lower surface of the aluminum alloy 2 was taken using an electron probe, as shown in fig. 3. The area percentage occupied by copper element is 2.53% by image processing analysis, and the ultrasonic processing is converted to obtain the aluminum alloy surface oxide film with the area percentage of 2.06%.
The examples described above represent only embodiments of the invention and are not to be understood as limiting the scope of the patent of the invention, it being pointed out that several variants and modifications may be made by those skilled in the art without departing from the concept of the invention, which fall within the scope of protection of the invention.
Claims (4)
1. The evaluation method for ultrasonically cleaning the oxide film on the surface of the aluminum alloy is characterized by comprising the following steps of:
(1) Placing a fixing table (5) on the inner bottom surface of the container (4) for fixing the aluminum alloy (2) thereon;
(2) Polishing the lower surface of the aluminum alloy (2), and then carrying out natural oxidation treatment to form a compact oxide film on the lower surface of the aluminum alloy (2);
(3) Placing the oxidized aluminum alloy (2) on a fixed table (5), wherein the lower surface of the oxidized aluminum alloy is not completely contacted with the fixed table (5);
(4) Pouring saturated copper salt solution (3) into the container (4), wherein the liquid level exceeds the upper surface of the aluminum alloy (2);
(5) Vertically contacting the ultrasonic probe (1) with the upper surface of the aluminum alloy (2), and performing ultrasonic treatment with ultrasonic power of 30W-150W for 1-3 min; in the ultrasonic treatment process, a compact oxide film at a non-contact part of the lower surface of the aluminum alloy (2) and the fixed table (5) is damaged, the aluminum alloy (2) leaks, aluminum and saturated copper salt solution (3) undergo a displacement reaction, and copper is attached to the lower surface of the aluminum alloy (2) at the moment;
(6) Taking out the aluminum alloy (2), and taking a distribution photo of copper elements on the lower surface of the aluminum alloy (2) by using a scanning electron microscope or an electronic probe; analyzing the area percentage occupied by the copper element through image processing, and converting the area percentage of the copper element to obtain the area percentage of aluminum on the surface of the aluminum alloy, so as to obtain a judgment result after ultrasonic cleaning;
the copper salt solution (3) in the step (4) is one of a copper sulfate solution and a copper chloride solution;
the ultrasonic probe (1) in the step (5) is a stainless steel probe.
2. The method for evaluating the ultrasonic cleaning of the oxide film on the surface of the aluminum alloy according to claim 1, wherein the thickness of the aluminum alloy (2) in the step (2) is 5-10 mm.
3. The method for evaluating an oxide film on an aluminum alloy surface by ultrasonic cleaning according to claim 1, wherein the grinding and polishing treatment in the step (2) is to perform rough grinding on the aluminum alloy (2) by using 240# abrasive paper, and then sequentially performing fine grinding on 600#, 1000#, 1500# and 2000# abrasive paper, wherein the abrasive paper is replaced when the scratch directions are consistent each time, and the sample is ground along the vertical scratch direction; after fine grinding, polishing was performed with a diamond paste having a particle size of 1.5.
4. The method for evaluating the ultrasonic cleaning of the oxide film on the surface of the aluminum alloy according to claim 1, wherein the natural oxidation treatment in the step (2) is to put the polished aluminum alloy (2) into air and oxidize for 10-120 min.
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| CN202111500417.0A CN114384102B (en) | 2021-12-09 | 2021-12-09 | Evaluation method for ultrasonically cleaning oxide film on aluminum alloy surface |
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| CN202111500417.0A CN114384102B (en) | 2021-12-09 | 2021-12-09 | Evaluation method for ultrasonically cleaning oxide film on aluminum alloy surface |
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| CN114384102B true CN114384102B (en) | 2024-01-26 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004263267A (en) * | 2003-03-04 | 2004-09-24 | C Uyemura & Co Ltd | Removal liquid for aluminum oxide film, and surface treatment method for aluminum or aluminum alloy |
| CN101852772A (en) * | 2009-03-30 | 2010-10-06 | 高海生 | Metal impurity detection device |
| CN102312259A (en) * | 2011-09-22 | 2012-01-11 | 珠海市赛日包装材料有限公司 | Preparation method of aluminium or aluminium alloy anodic oxide film |
| CN112129825A (en) * | 2019-06-25 | 2020-12-25 | 深圳市裕展精密科技有限公司 | Oxide film detection method and oxide film detection device |
-
2021
- 2021-12-09 CN CN202111500417.0A patent/CN114384102B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004263267A (en) * | 2003-03-04 | 2004-09-24 | C Uyemura & Co Ltd | Removal liquid for aluminum oxide film, and surface treatment method for aluminum or aluminum alloy |
| CN101852772A (en) * | 2009-03-30 | 2010-10-06 | 高海生 | Metal impurity detection device |
| CN102312259A (en) * | 2011-09-22 | 2012-01-11 | 珠海市赛日包装材料有限公司 | Preparation method of aluminium or aluminium alloy anodic oxide film |
| CN112129825A (en) * | 2019-06-25 | 2020-12-25 | 深圳市裕展精密科技有限公司 | Oxide film detection method and oxide film detection device |
Non-Patent Citations (2)
| Title |
|---|
| 超声场对连续铸造7A09铝合金微观缺陷的影响;唐靖川 等;特种铸造及有色合金;36(02);第196-199页 * |
| 铝合金表面氧化膜去除方法研究进展;熊金平 等;电镀与精饰;35(11);第15-19页 * |
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