CN112595571A - Metallographic corrosion method, metallographic testing method and application of alkaline solution - Google Patents
Metallographic corrosion method, metallographic testing method and application of alkaline solution Download PDFInfo
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Abstract
本发明提供了一种金相腐蚀方法、金相测试方法以及碱性溶液的用途。所述金相腐蚀方法包括以下步骤：(1)对金相试样进行切割和打磨抛光，得到处理过的金相试样；(2)对步骤(1)所述处理过的金相试样用碱性腐蚀液进行浸蚀，得到腐蚀后的金相试样；其中，步骤(1)所述金相试样为含铝试样。本发明提供的金相腐蚀方法使用碱性溶液作为金相腐蚀液，危害性相对较低，即使人员误操作，对其人身伤害也可降低到最小，而且金相效果也比较可观，可替代酸溶液作为腐蚀液。
The invention provides a metallographic corrosion method, a metallographic testing method and the use of an alkaline solution. The metallographic corrosion method includes the following steps: (1) cutting and polishing the metallographic sample to obtain a processed metallographic sample; (2) processing the processed metallographic sample in step (1) Etching with an alkaline etching solution to obtain a corroded metallographic sample; wherein, the metallographic sample in step (1) is an aluminum-containing sample. The metallographic corrosion method provided by the present invention uses an alkaline solution as the metallographic corrosion solution, and the hazard is relatively low. Even if personnel misuse, the personal injury to them can be minimized, and the metallographic effect is also considerable, which can replace acid solution as corrosive liquid.
Description
Technical Field
The invention belongs to the field of metallographic phase, and relates to a metallographic corrosion method, a metallographic testing method and application of an alkaline solution.
Background
The lithium battery has the advantages of light weight, high capacity, long service life, low self-discharge rate, no memory effect, no pollution and the like, and particularly, the power battery is widely applied to equipment such as electric bicycles, electric hardware tools and the like, the equipment requires the battery to have the conditions of high capacity, high power and the like, and the power lithium battery has certain advantages in this respect. However, when the battery is used, safety needs to be guaranteed, welding reliability of welding of the battery cover plate assembly and welding reliability of the cover plate and the aluminum shell determine safety performance of the battery, therefore, a welding part of the pole and the terminal and a welding part of the cover plate and the aluminum shell need to be observed, whether welding meets requirements or not is judged, metallographic structures and appearance of a welding joint need to be reflected during observation, welding penetration and welding width are accurately tested, metallographic corrosive liquid is generally an acid solution traditionally used as metallographic corrosive liquid, so that metallographic samples of an aluminum alloy welding layer show clear macroscopic metallographic structures, hydrofluoric acid and nitric acid are contained in a formula of the metallographic structures, the hydrofluoric acid solution is extremely harmful, the hydrofluoric acid solution is commonly called bone water, the nitric acid solution is improper to treat, explosion risks easily occur, and inestimable personal injury can be caused to inspectors.
Because the reliability detection indexes of the inside of the battery cover plate and the welding with the aluminum shell are important parts in the safety performance of the battery, the welding of a post and a terminal in the cover plate directly influences the sealing performance and the mechanical performance of the battery, the welding strength and the welding depth of the cover plate and the aluminum shell determine the sealing performance of the single battery, and the mechanical performance and whether the core cladding is damaged or not have a very close relation, so that the observation of the metallographic structure morphology of an aluminum alloy welding layer and the accurate evaluation of the welding penetration and the fusion width are necessary standards for testing the functions of the cover plate and the excellent state of the electric core in the manufacturing process.
CN110553891A discloses a macroscopic metallographic etchant and a metallographic etching method for a stainless steel aluminum alloy connecting layer, which are applied to preparation of metallographic samples. The metallographic corrosive liquid comprises liquid A and liquid B; the A liquid comprises 2-10 wt% of HF and at least 10 wt% of FeCl3And water; the B liquid is 5 to 15 weight percent of HNO3And (3) solution. The metallographic etching method comprises the following steps: dropwise adding the liquid A to a sample polishing surface formed by polishing and polishing a metallographic sample, carrying out corrosion reaction for 10-50 s, and cleaning; and dropwise adding the liquid B to the polished surface of the sample for several seconds, washing, and blow-drying to obtain the corroded metallographic sample.
CN111778507A discloses a metallographic etchant and a preparation method thereof, wherein the metallographic etchant comprises 8-12% of hydrofluoric acid solution, 40-50% of nitric acid solution, 4-8% of hydrochloric acid solution and the balance of water according to volume percentage.
CN110983339A discloses a formula of a metallographic corrosive liquid for duplex stainless steel and a using method thereof, wherein each corrosive liquid contains 4045ml of phosphoric acid, 5060 ml of sulfuric acid, 155165 ml of glycerol, 4050 ml of water, 1530 g of sodium sulfite and 25 g of thiourea.
However, the metallographic etchant adopted by the scheme is an acidic solution, and even contains hydrofluoric acid and nitric acid, so that the safety problem is easily caused.
Disclosure of Invention
In view of the above problems in the prior art, the present invention is directed to a metallographic etching method, a metallographic testing method, and use of an alkaline solution. The metallographic etching method provided by the invention uses the alkaline solution as the metallographic etchant, has relatively low harmfulness, can reduce the personal injury to the staff to the minimum even if the staff operates by mistake, has considerable metallographic effect, and can replace the acid solution as the etchant.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a metallographic etching method comprising the steps of:
(1) cutting, grinding and polishing the metallographic specimen to obtain a processed metallographic specimen;
(2) etching the metallographic sample treated in the step (1) by using an alkaline corrosive liquid to obtain a corroded metallographic sample;
wherein the metallographic sample in the step (1) is an aluminum-containing sample.
In the metallographic corrosion method provided by the invention, the reason that the alkaline corrosive liquid can corrode the metallographic sample is that the alkaline corrosive liquid and the metallographic sample have ionic reaction and have a chemical formula of 2Al +2H2O+2OH-＝2AlO2 -+3H2↑。
In the metallographic etching method provided by the invention, the alkaline solution is used as the etching solution instead of the acidic solution, so that the harm of the etching solution to personnel is minimized, and meanwhile, the etching effect is very ideal.
The following is a preferred technical solution of the present invention, but not a limitation to the technical solution provided by the present invention, and the technical objects and advantageous effects of the present invention can be better achieved and achieved by the following preferred technical solution.
As a preferable technical scheme of the invention, the metallographic sample in the step (1) is an aluminum alloy sample.
Preferably, the aluminum alloy test sample is an aluminum alloy welding layer.
Preferably, the aluminum alloy welding layer is an aluminum alloy welding layer for a lithium battery.
As a preferable technical scheme of the invention, the cutting in the step (1) is carried out by a metallographic cutting machine.
Preferably, the grinding and polishing in step (1) comprises rough grinding and fine grinding and polishing.
According to the invention, the rough grinding is used for removing residual metal chips on the section and foreign matters such as scratches generated in the cutting process, and the fine grinding and polishing is used for grinding and polishing the section to a smooth and perfect mirror surface, so that the special analysis requirements can be met.
Preferably, the rough grinding comprises grinding with 150-220 mesh sand paper, such as 150 mesh, 180 mesh, 220 mesh, or the like.
Preferably, the fine grinding and polishing comprises grinding with 320-500-mesh sand paper, such as 320 mesh, 400 mesh or 500 mesh.
In a preferred embodiment of the present invention, the alkaline substance of the alkaline corrosion solution in step (2) includes any one or a combination of at least two of sodium hydroxide, calcium hydroxide, and potassium hydroxide.
Preferably, the basic substance is analytically pure.
Preferably, the solvent of the alkaline corrosive liquid is water.
Preferably, the mass fraction of the alkaline substance in the alkaline etching solution is 5-15 wt%, such as 5 wt%, 7 wt%, 10 wt%, 12 wt% or 15 wt%, etc., preferably 10-15 wt%. In the invention, if the mass fraction of alkaline substances in the alkaline corrosive liquid is too low, the appearance of a metallographic sample is unclear, and the tested welding penetration and fusion width data have low reliability; if the mass fraction of the alkaline substance in the alkaline etching solution is too high (more than 15 wt%), a large amount of heat may be generated when the alkaline substance (e.g., sodium hydroxide) is dissolved in a solvent (e.g., water), the reaction process is severe, and a large amount of bubbles are formed on the surface of the solution, which causes a safety problem.
Preferably, the preparation method of the alkaline corrosive liquid comprises the following steps: mixing the solid particles of the alkaline substance and the solvent in a container.
As a preferable technical scheme of the invention, the etching time in the step (2) is 2-10min, such as 2min, 3min, 4min, 5min, 6min, 7min, 8min, 9min or 10min, and the like, and is preferably 4-10 min. In the invention, if the etching time is too short, the appearance of the metallographic specimen is unclear, and the tested welding penetration and fusion width data have low reliability; if the etching time is too long, the efficiency of the metallographic experiment is affected.
As a preferable embodiment of the present invention, the etching method further includes: and cleaning and drying the metallographic specimen obtained after etching.
Preferably, the cleaning is water washing.
Preferably, the temperature of the water washing is 30-40 ℃, such as 30 ℃, 32 ℃, 35 ℃, 38 ℃ or 40 ℃ and the like.
Preferably, the drying method is wiping.
As a further preferable technical scheme of the metallographic corrosion method, the method comprises the following steps:
(1) cutting the metallographic specimen into a required shape along the cross section by using a metallographic cutting machine, polishing by using 180-mesh abrasive paper, and polishing by using 400-mesh abrasive paper to obtain a treated metallographic specimen;
(2) etching the metallographic sample treated in the step (1) by using an alkaline corrosive liquid with the alkaline substance mass fraction of 10-15 wt% for 4-10min, and then cleaning and wiping the metallographic sample by using water at the temperature of 30-40 ℃ to obtain an etched metallographic sample;
and (2) the metallographic specimen in the step (1) is an aluminum alloy welding layer.
In a second aspect, the present invention provides a metallographic test method comprising: metallographic etching a metallographic specimen according to the method of any one of claims 1 to 7 to obtain an etched metallographic specimen, and testing said etched metallographic specimen, said metallographic specimen being an aluminium-containing specimen.
As the preferable technical scheme of the invention, the test comprises morphology observation and/or fusion penetration and fusion width measurement;
preferably, the test is performed with a three-dimensional meter.
In a third aspect, the present invention provides the use of an alkaline solution as a metallographic etchant for etching a metallographic specimen containing aluminium.
Preferably, the alkaline substance in the alkaline solution comprises any one of sodium hydroxide, potassium hydroxide or calcium hydroxide or a combination of at least two of the above.
Preferably, the basic substance is analytically pure.
Preferably, the solvent of the alkaline solution is water.
Preferably, the mass fraction of alkaline substance in the alkaline solution is 5-15 wt%, such as 5 wt%, 7 wt%, 10 wt%, 12 wt% or 15 wt%, etc., preferably 10-15 wt%.
Compared with the prior art, the invention has the following beneficial effects:
the metallographic etching method provided by the invention uses the alkaline solution as the metallographic etchant, has relatively low harmfulness, can reduce the personal injury to the staff to the minimum even if the staff operates by mistake, has considerable metallographic effect, and can replace the acid solution as the etchant. When the mass fraction of alkaline substances in the alkaline corrosive liquid is 10-15 wt%, and the etching time is 4-10min, the metallographic corrosion effect which is not lower than that of the acidic corrosive liquid can be obtained.
Drawings
FIG. 1 is a photograph of a three-dimensional measuring instrument of a metallographic sample after corrosion obtained in example 1;
FIG. 2 is a photograph of a three-dimensional measuring instrument of a metallographic sample after corrosion obtained in example 2;
FIG. 3 is a photograph of a three-dimensional measuring instrument of a metallographic sample after corrosion obtained in example 3;
FIG. 4 is a photograph of a three-dimensional measuring instrument of a metallographic sample after corrosion obtained in example 4;
FIG. 5 is a photograph of a three-dimensional measuring instrument of a metallographic sample after corrosion obtained in example 5;
FIG. 6 is a photograph of a three-dimensional measuring instrument of a metallographic sample after corrosion obtained in example 6;
FIG. 7 is a photograph of a three-dimensional measuring instrument of a metallographic sample after corrosion obtained in example 7;
FIG. 8 is a photograph of a three-dimensional measuring instrument of a metallographic sample after corrosion obtained in example 8;
FIG. 9 is a photograph of a three-dimensional measuring instrument of a metallographic sample after corrosion obtained in example 9;
FIG. 10 is a photograph of a three-dimensional measuring instrument of a metallographic sample after corrosion obtained in example 10;
FIG. 11 is a photograph of a three-dimensional measuring instrument of a metallographic sample after corrosion obtained in example 11;
FIG. 12 is a photograph of a three-dimensional measuring instrument of a metallographic sample after corrosion obtained in example 12;
fig. 13 is a photograph of a corroded metallographic sample obtained in comparative example 1 as a three-dimensional measurement instrument.
Detailed Description
In order to better illustrate the present invention and facilitate the understanding of the technical solutions of the present invention, the present invention is further described in detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
The following are typical but non-limiting examples of the invention:
in the following examples, the alkaline substances used were all of analytical grade, and the water in the alkaline etching solution used was distilled water.
Example 1
This example was metallographically etched as follows:
(1) cutting the metallographic specimen into a required shape along the cross section by using a metallographic cutting machine, polishing by using 180-mesh abrasive paper, and polishing by using 400-mesh abrasive paper to obtain a treated metallographic specimen;
(2) etching the metallographic sample treated in the step (1) by using an alkaline corrosive liquid (a solution consisting of sodium hydroxide and water) with the alkaline substance mass fraction of 5 wt% for 2min, and then cleaning and wiping the metallographic sample by using water with the temperature of 35 ℃ to obtain an etched metallographic sample;
wherein the metallographic specimen in the step (1) is an aluminum alloy welding layer (the mark is Al 3003H14, and the main impurities comprise 0.47 percent of Fe and 1.02 percent of Mn).
The metallographic morphology state of the corroded metallographic specimen obtained in the embodiment was observed under a three-dimensional measurement instrument.
Fig. 1 is a photograph of a three-dimensional measuring instrument of the metallographic sample after etching obtained in this example, and it can be seen from the photograph that the metallographic structure morphology is not revealed.
In each of the following examples, the obtained corroded metallographic sample was observed by using a three-dimensional measuring instrument.
Example 2
This embodiment differs from example 1 only in that: the etching time was 4 min.
Fig. 2 is a photograph of a three-dimensional measuring instrument of the metallographic sample after etching obtained in this example, and it can be seen from this figure that the metallographic structure morphology is microscopic.
Example 3
This embodiment differs from example 1 only in that: the etching time was 10 min.
Fig. 3 is a photograph of a three-dimensional measuring instrument of the metallographic sample after etching obtained in this example, and it can be seen from this figure that the metallographic structure morphology is microscopic.
Example 4
This example differs from example 1 only in that: the mass fraction of alkaline substances in the alkaline corrosive liquid (solution consisting of sodium hydroxide and water) is 8 wt%.
Fig. 4 is a photograph of a three-dimensional measuring instrument of the metallographic sample after etching obtained in this example, and it can be seen from this figure that the metallographic structure morphology is microscopic.
Example 5
This implementation differs from example 4 only in that: the etching time was 4 min.
Fig. 5 is a photograph of a three-dimensional measuring instrument of the metallographic sample after etching obtained in this example, and it can be seen from this figure that the metallographic structure is microscopic in morphology.
Example 6
This implementation differs from example 4 only in that: the etching time was 10 min.
Fig. 6 is a photograph of a three-dimensional measuring instrument of the metallographic sample after corrosion obtained in the present embodiment, and it can be seen from the photograph that the metallographic structure has a clear morphology and a clear profile.
Example 7
This example differs from example 1 only in that: the mass fraction of alkaline substances in the alkaline corrosive liquid (solution consisting of sodium hydroxide and water) is 10 wt%.
Fig. 7 is a photograph of a three-dimensional measuring instrument of the metallographic sample after etching obtained in this example, and it can be seen from this figure that the metallographic structure is microscopic in morphology.
Example 8
This embodiment differs from example 7 only in that: the etching time was 4 min.
Fig. 8 is a photograph of a three-dimensional measuring instrument of the metallographic sample after corrosion obtained in the present embodiment, and it can be seen from the photograph that the metallographic structure has a clear morphology and a clear profile.
Example 9
This embodiment differs from example 7 only in that: the etching time was 10 min.
Fig. 9 is a photograph of a three-dimensional measuring instrument of the metallographic sample after corrosion obtained in the present embodiment, and it can be seen from the photograph that the metallographic structure has a clear morphology and a clear profile.
Example 10
This example differs from example 1 only in that: the mass fraction of alkaline substances in the alkaline corrosive liquid (solution consisting of sodium hydroxide and water) is 15 wt%.
Fig. 10 is a photograph of a three-dimensional measuring instrument of the metallographic sample after etching obtained in the present example, and it can be seen from the photograph that the metallographic structure morphology is gradually clear.
Example 11
This embodiment differs from example 10 only in that: the etching time was 4 min.
Fig. 11 is a photograph of a three-dimensional measuring instrument of the metallographic sample after etching obtained in the present example, and it can be seen from the photograph that the metallographic morphology is clearly shown.
Example 12
This embodiment differs from example 10 only in that: the etching time was 10 min.
Fig. 12 is a photograph of a three-dimensional measuring instrument of the metallographic sample after corrosion obtained in this example, and it can be seen from the photograph that the metallographic structure morphology is completely and clearly presented.
Comparative example 1
This comparative example differs from example 1 in that instead of using an alkaline etching solution, the etching solution was used in a ratio of hydrofluoric acid: hydrochloric acid: nitric acid: the volume ratio of water to water is 2:3:5: 95.
Fig. 13 is a photograph of a three-dimensional measurement instrument of a metallographic sample after corrosion obtained in the present comparative example, and it can be seen from the photograph that the metallographic structure appearance profile is clear.
The clarity of the metallographic morphology observed by the ternary measuring instrument for the examples and comparative examples was graded in the order from low (unclear, completely non-corroding) to high (very clear) on five scales, 0, 1, 2, 3, 4, as listed below:
TABLE 1
| Numbering | Clear degree of metallographic morphology |
| Example 1 | 0 |
| Example 2 | 1 |
| Example 3 | 1 |
| Example 4 | 1 |
| Example 5 | 1 |
| Example 6 | 2 |
| Example 7 | 1 |
| Example 8 | 2 |
| Example 9 | 2 |
| Example 10 | 3 |
| Example 11 | 4 |
| Example 12 | 4 |
| Comparative example 1 | 2 |
It can be known from the above examples and comparative examples that the metallographic etching method provided by the examples uses an alkaline solution as the metallographic etching solution, has relatively low harmfulness, can reduce the personal injury to the staff to the minimum even if the staff operates by mistake, has considerable metallographic effect, and can replace an acid solution as the etching solution. When the mass fraction of alkaline substances in the alkaline corrosive liquid (the solution consisting of sodium hydroxide and water) reaches 10 wt%, the metallographic structure clarity degree identical to that of the acidic corrosive liquid in the comparative example 1 can be achieved after 4min of soaking.
Comparative example 1 has a good metallographic corrosion effect, but it uses hazardous chemicals such as hydrofluoric acid and nitric acid, which easily causes a safety problem.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. A metallographic etching method, characterized in that it comprises the following steps:
(1) cutting, grinding and polishing the metallographic specimen to obtain a processed metallographic specimen;
(2) etching the metallographic sample treated in the step (1) by using an alkaline corrosive liquid to obtain a corroded metallographic sample;
wherein the metallographic sample in the step (1) is an aluminum-containing sample.
2. The metallographic etching method according to claim 1, wherein said metallographic specimen of step (1) is an aluminum alloy specimen;
preferably, the aluminum alloy sample is an aluminum alloy welding layer;
preferably, the aluminum alloy welding layer is an aluminum alloy welding layer for a lithium battery.
3. The method of claim 1 or 2, wherein said cutting of step (1) is performed with a metallographic cutter;
preferably, the grinding and polishing of step (1) comprises coarse grinding and fine grinding and polishing;
preferably, the rough grinding comprises grinding with 150-220-mesh sand paper;
preferably, the fine grinding and polishing comprises grinding with 320-500-mesh sand paper.
4. The method according to any one of claims 1 to 3, wherein the alkaline substance of the alkaline corrosive solution of the step (2) comprises any one or a combination of at least two of sodium hydroxide, calcium hydroxide or potassium hydroxide;
preferably, the purity of the basic substance is analytical grade;
preferably, the solvent of the alkaline corrosive liquid is water;
preferably, the mass fraction of the alkaline substance in the alkaline corrosive liquid is 5-15 wt%, preferably 10-15 wt%;
preferably, the preparation method of the alkaline corrosive liquid comprises the following steps: mixing the solid particles of the alkaline substance and the solvent in a container.
5. A method according to any one of claims 1 to 4, wherein the etching in step (2) is carried out for a period of 2 to 10min, preferably 4 to 10 min.
6. The method of any one of claims 1-5, wherein the etching method further comprises: cleaning and drying the etched metallographic specimen;
preferably, the washing is water washing;
preferably, the temperature of the water washing is 30-40 ℃;
preferably, the drying method is wiping.
7. The method according to any one of claims 1-7, characterized in that the method comprises the steps of:
(1) cutting the metallographic specimen into a required shape along the cross section by using a metallographic cutting machine, polishing by using 180-mesh abrasive paper, and polishing by using 400-mesh abrasive paper to obtain a treated metallographic specimen;
(2) etching the metallographic sample treated in the step (1) by using an alkaline corrosive liquid with the alkaline substance mass fraction of 10-15 wt% for 4-10min, and then cleaning and wiping the metallographic sample by using water at the temperature of 30-40 ℃ to obtain an etched metallographic sample;
and (2) the metallographic specimen in the step (1) is an aluminum alloy welding layer.
8. A metallographic test method, characterized in that the method comprises: metallographic etching a metallographic specimen according to the method of any one of claims 1 to 7 to obtain an etched metallographic specimen, and testing said etched metallographic specimen, said metallographic specimen being an aluminium-containing specimen.
9. A metallographic test method according to claim 8, characterised in that said test comprises topography observation and/or penetration melt width measurement;
preferably, the test is performed with a three-dimensional meter.
10. The use of an alkaline solution, characterized in that the alkaline solution is used as a metallographic etching solution for etching metallographic specimens containing aluminium;
preferably, the alkaline substance in the alkaline solution comprises any one or a combination of at least two of sodium hydroxide, potassium hydroxide or calcium hydroxide;
preferably, the purity of the basic substance is analytical grade;
preferably, the solvent of the alkaline solution is water;
preferably, the mass fraction of the alkaline substance in the alkaline solution is 5-15 wt%, preferably 10-15 wt%.
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| CN114486459A (en) * | 2022-01-24 | 2022-05-13 | 宁波江丰电子材料股份有限公司 | Method for judging interlayer of aluminum and aluminum alloy bar |
| WO2024193107A1 (en) * | 2023-03-22 | 2024-09-26 | 湖北亿纬动力有限公司 | Color-developing corrosive liquid, and preparation method therefor and use thereof |
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