1J22 magnetically soft alloy welding metallographic etching solution and use method thereof

Abstract

The invention provides a 1J22 magnetically soft alloy welding metallographic etching solution and a use method thereof. The 1J22 magnetically soft alloy welding metallographic etching solution comprises the following components in parts by weight: 1-3 parts of copper chloride, 7-13 parts of absolute ethyl alcohol, 12-20 parts of hydrochloric acid and 42-62 parts of water. The using method comprises the steps that a 1J22 magnetically soft alloy welding pool sample is soaked in the etching solution according to any one of claims 1-3, and after cleaning treatment and drying treatment are conducted in sequence, metallographic structure observation is conducted through a metallographic microscope. The etching liquid provided by the invention is excellent in etching effect, the structure of a 1J22 magnetically soft alloy welding pool after etching is clear and visible, the metallographic phase is clear, and the observation and analysis of geometrical morphology information such as the grain size, the form, the distribution position and the angle between grains of the alloy are completely met.

Description

Technical Field

[0001] The invention belongs to the technical field of metallographic analysis of metal materials, and relates to an etching liquid for metallographic structure morphology of a 1J22 soft magnetic alloy, and in particular to a 1J22 soft magnetic alloy welding metallographic etching liquid and a use method thereof. Background Art

[0002] 1J22 is an iron-cobalt-vanadium soft magnetic alloy with high saturation magnetic induction intensity, magnetostriction coefficient and Curie point, low resistivity, magnetic isotropy, good magnetic stability, and can be used to make parts that work at higher temperatures, but it is not suitable for use at high frequencies. The alloy is expensive, easy to oxidize, and has poor processing performance. It can be used to make electromagnets and can generate large suction forces; it can be used to make magnetostrictive transducers with high output energy, and can also be used to make iron cores and other magnets for micromotors and pulse transformers.

[0003] In products such as servos, sensors, and valves, many magnetic functional components require welding soft magnetic alloys and stainless steel parts together while ensuring the magnetic properties of the product.

[0004] Metallographic testing is an indispensable testing method in the process of deep processing and material research of metal materials. Through metallographic organization observation, the organizational structure and grain size of the product can be timely grasped. Through metallographic analysis, some product defects in the product can be observed, whether the welding process is reasonable, and the product quality can be improved by analyzing and changing the production process and optimizing the production process parameters. Metallographic corrosion is the primary task of metallographic testing. Only by using suitable corrosive agents to etch out the clear metallographic structure and grain boundaries of the product, can the grain size, metallographic structure and the content of each phase be analyzed, and whether the heat treatment process is appropriate can be judged. The rationality of the adjusted heat treatment process can be analyzed and judged. However, the existing 1J22 alloy metallographic etching solution does not clearly observe the organizational structure of the alloy product, the grain size measurement is inaccurate, and it is not easy to judge the defects in the product.

[0005] In order to overcome the above problems, it is necessary to provide an etching solution that can more completely, clearly and accurately display the metallographic structure morphology of the 1J22 soft magnetic alloy sample. Summary of the invention

[0006] The object of the present invention is to provide a 1J22 soft magnetic alloy welding metallographic etching liquid and a method for using the same. The etching liquid solves the problem of difficulty in displaying the metallographic structure morphology during the welding process of the 1J22 soft magnetic alloy; the etching liquid can display the metallographic structure morphology of the 1J22 soft magnetic alloy sample more completely, clearly and accurately. It fully meets the observation and analysis of geometric morphological information such as the grain size, morphology, distribution position and angle between grains of the alloy. The present invention is simple, practical and reliable, and greatly improves the metallographic inspection efficiency and quality of such alloys.

[0007] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0008] In a first aspect, the present invention provides a 1J22 soft magnetic alloy welding metallographic etching solution, wherein the 1J22 soft magnetic alloy welding metallographic etching solution comprises: cupric chloride, anhydrous ethanol, hydrochloric acid and water.

[0009] In the present invention, the raw materials in the etching solution are simple and easy to obtain; the copper chloride is used to outline the gold grid, the anhydrous ethanol is used to remove the etching mixture, and the hydrochloric acid is used to etch the gold grid outline; the three complement each other to achieve clear, complete and accurate display of the metallographic structure morphology during the welding process of 1J22 soft magnetic alloy.

[0010] As a preferred technical solution of the present invention, the 1J22 soft magnetic alloy welding metallographic etching solution includes, by weight: 1 to 3 parts of cupric chloride, 7 to 13 parts of anhydrous ethanol, 12 to 20 parts of hydrochloric acid and 42 to 62 parts of water.

[0011] Exemplarily, the weight proportion of cupric chloride in the 1J22 soft magnetic alloy welding metallographic etching solution is 1 to 3 parts, for example, 1 part, 1.4 parts, 1.8 parts, 2.2 parts, 2.6 parts or 3 parts, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0012] The weight proportion of the anhydrous ethanol is 7 to 13 parts, for example, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts or 13 parts, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0013] The weight proportion of the hydrochloric acid is 12 to 20 parts, for example, 12 parts, 14 parts, 16 parts, 18 parts or 20 parts, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0014] The weight proportion of the water is 42 to 62 parts, for example, 42 parts, 46 parts, 50 parts, 54 parts, 58 parts or 62 parts, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0015] In the present invention, the weight proportion of the copper chloride is 1 to 3 parts. If the content of the copper chloride is too high, the gap between the gold grids will be too wide and the shape and size of the gold grids will be distorted. If the content is too low, the gold grid outline cannot be clearly displayed or even cannot be displayed.

[0016] The weight proportion of the hydrochloric acid is 12 to 20 parts. If the content of the hydrochloric acid is too high, it will cause excessive corrosion of the 1J22 material and the entire surface will turn black. If the content is too low, it will result in the inability to etch the gold grid gap.

[0017] As a preferred technical solution of the present invention, the 1J22 soft magnetic alloy welding metallographic etching solution comprises, by weight: 2 parts of cupric chloride, 10 parts of anhydrous ethanol, 16 parts of hydrochloric acid and 52 parts of water.

[0018] As a preferred technical solution of the present invention, the concentration of the cupric chloride is 38-42wt%, for example, 38wt%, 38.5wt%, 39wt%, 39.5wt%, 40wt%, 40.5wt%, 41wt%, 41.5wt% or 42wt%, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0019] Preferably, the concentration of the hydrochloric acid is 35-37wt%, for example, it can be 35wt%, 35.2wt%, 35.4wt%, 35.6wt%, 35.8wt%, 36wt%, 36.2wt%, 36.4wt%, 36.6wt%, 36.8wt% or 37wt%, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0020] In a second aspect, the present invention provides a method for using the 1J22 soft magnetic alloy welding metallographic etching solution described in the first aspect, the method comprising the following steps:

[0021] The 1J22 soft magnetic alloy welding molten pool sample is immersed in the etching solution according to any one of claims 1 to 3, and is cleaned and dried in sequence, and then the metallographic structure is observed using a metallographic microscope.

[0022] The present invention can achieve etching of the 1J22 soft magnetic alloy welding molten pool sample through a simple immersion process, and further observe to obtain a complete, clear and accurate metallographic structure image.

[0023] As a preferred technical solution of the present invention, the melting depth of the 1J22 soft magnetic alloy welding pool is 0.15-0.3 mm, for example, it can be 0.15 mm, 0.18 mm, 0.21 mm, 0.24 mm, 0.27 mm or 0.3 mm, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0024] As a preferred technical solution of the present invention, the soaking time is 160 to 200 seconds, for example, it can be 160 seconds, 165 seconds, 170 seconds, 175 seconds, 180 seconds, 185 seconds, 190 seconds, 195 seconds or 200 seconds, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable; preferably 180 seconds.

[0025] As a preferred technical solution of the present invention, the immersion temperature is 20-30°C, for example, it can be 20°C, 21°C, 22°C, 23°C, 24°C, 25°C, 26°C, 27°C, 28°C, 29°C or 30°C, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0026] As a preferred technical solution of the present invention, the welding method of the 1J22 soft magnetic alloy includes laser welding.

[0027] Preferably, the diameter of the weld in the laser welding is 0.3-0.4 mm, for example, 0.3 mm, 0.32 mm, 0.34 mm, 0.36 mm, 0.38 mm or 0.4 mm, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0028] More specifically, the 1J22 soft magnetic alloy welding metallographic phase of the present invention is: the alloy structure metallographic phase of the 1J22 soft magnetic alloy welding pool during the welding process of the 1J22 soft magnetic alloy and the dissimilar alloy;

[0029] In the present invention, 1J22 soft magnetic alloy is welded with tungsten material, the welding condition is butt welding, and the diameter of the welding spot is 0.35 mm.

[0030] Preferably, the width of the 1J22 soft magnetic alloy welding pool sample is 0.2 to 0.26 mm, for example, it can be 0.2 mm, 0.21 mm, 0.22 mm, 0.23 mm, 0.24 mm, 0.25 mm or 0.26 mm, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0031] More specifically, the 1J22 soft magnetic alloy welding pool sample contains at least one weld spot.

[0032] As a preferred technical solution of the present invention, the method of use comprises:

[0033] Under the temperature condition of 20-30° C., immerse the 1J22 soft magnetic alloy welding pool sample in the etching solution according to any one of claims 1 to 3 for 160-200 seconds, perform cleaning treatment and drying treatment in sequence, and then observe the metallographic structure using a metallographic microscope;

[0034] Wherein, the melting depth of the 1J22 soft magnetic alloy welding pool is 0.15-0.3 mm.

[0035] The numerical range described in the present invention not only includes the point values ​​listed above, but also includes any point values ​​between the above numerical ranges that are not listed. Due to space limitations and for the sake of simplicity, the present invention no longer exhaustively lists the specific point values ​​included in the range.

[0036] Compared with the prior art, the present invention has the following beneficial effects:

[0037] (1) The etching solution provided by the present invention has simple components, is easy to obtain, has low cost, and is suitable for industrial mass production;

[0038] (2) The etching solution provided by the present invention has excellent etching effect. After etching, the structure of the molten pool of the 1J22 soft magnetic alloy welding is clearly visible and the metallographic structure is clear, which fully meets the observation and analysis of geometric morphology information such as the grain size, morphology, distribution position and angle between grains of the alloy;

[0039] (3) The etching solution and the method of use provided by the present invention are simple, practical and reliable, and greatly improve the efficiency and quality of metallographic inspection during the welding process of 1J22 soft magnetic alloy. BRIEF DESCRIPTION OF THE DRAWINGS

[0040] Figure 1 This is a metallographic structure morphology diagram provided for Application Example 1 of the present invention. DETAILED DESCRIPTION

[0041] The technical solution of the present invention is further described below by specific implementation methods. It should be understood by those skilled in the art that the embodiments are only to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0042] Examples 1-5

[0043] A 1J22 soft magnetic alloy welding metallographic etching liquid, the components of the 1J22 soft magnetic alloy welding metallographic etching liquid are shown in Table 1.

[0044] Table 1

[0045] Copper chloride / g Anhydrous ethanol / g Hydrochloric acid / g Water / g Example 1 2 10 16 52 Example 2 1 7 12 42 Example 3 3 13 20 62 Example 4 1.5 11 15 50 Example 5 2.5 9 18 60

[0046] In the above embodiment, the concentration of the cupric chloride is 40 wt %, and the concentration of the hydrochloric acid is 36 wt %.

[0047] Comparative Examples 1-12

[0048] A 1J22 soft magnetic alloy welding metallographic etching solution, the components of the 1J22 soft magnetic alloy welding metallographic etching solution are shown in Table 2.

[0049] Table 2

[0050]

[0051]

[0052] In the above comparative example, the concentration of the cupric chloride is 40wt%, and the concentration of the hydrochloric acid is 36wt%.

[0053] Comparative Example 13

[0054] This comparative example provides a 1J22 soft magnetic alloy welding metallographic etching solution, which includes: 150g of water and 12g of oxalic acid.

[0055] Comparative Example 14

[0056] This comparative example provides a 1J22 soft magnetic alloy welding metallographic etching solution, which differs from Example 1 only in that:

[0057] In this comparative example, cupric chloride is adjusted to copper sulfate of equal mass and concentration.

[0058] Comparative Example 15

[0059] This comparative example provides a 1J22 soft magnetic alloy welding metallographic etching solution, which differs from Example 1 only in that:

[0060] In this comparative example, hydrochloric acid was adjusted to sulfuric acid of equal mass and concentration.

[0061] Application Examples 1-5

[0062] A method for using the 1J22 soft magnetic alloy welding metallographic etching solution provided in Example 1-5, the method comprising the following steps:

[0063] At 25° C., the 1J22 soft magnetic alloy welding pool samples were immersed in the etching solution provided in Examples 1-5 for 180 seconds, and then cleaned and dried in turn, and then the metallographic structure was observed using a metallographic microscope;

[0064] Wherein, the melting depth of the 1J22 soft magnetic alloy welding pool is 0.2 mm.

[0065] The metallographic structure morphology provided in Application Example 1 is as follows: Figure 1 shown.

[0066] Application Example 6

[0067] This application example provides a method for using the 1J22 soft magnetic alloy welding metallographic etching solution provided in Example 1. The difference between the method and Application Example 1 is that:

[0068] In this application example, the soaking time is adjusted to 120s.

[0069] Application Example 7

[0070] This application example provides a method for using the 1J22 soft magnetic alloy welding metallographic etching solution provided in Example 1. The difference between the method and Application Example 1 is that:

[0071] In this application example, the soaking time is adjusted to 160s.

[0072] Application Example 8

[0073] This application example provides a method for using the 1J22 soft magnetic alloy welding metallographic etching solution provided in Example 1. The difference between the method and Application Example 1 is that:

[0074] In this application example, the soaking time is adjusted to 200s.

[0075] Application Example 9

[0076] This application example provides a method for using the 1J22 soft magnetic alloy welding metallographic etching solution provided in Example 1. The difference between the method and Application Example 1 is that:

[0077] In this application example, the soaking time is adjusted to 240s.

[0078] Comparative Application Examples 1-15

[0079] A method for using the 1J22 soft magnetic alloy welding metallographic etching solution provided in Comparative Example 1-15, the method comprising the following steps:

[0080] At 25° C., the 1J22 soft magnetic alloy welding pool samples were immersed in the etching solution provided in Comparative Examples 1-15 for 180 seconds, and then cleaned and dried in turn, and then the metallographic structure was observed using a metallographic microscope;

[0081] Wherein, the melting depth of the 1J22 soft magnetic alloy welding pool is 0.2 mm.

[0082] Metallographic structure observation results:

[0083] The metallographic structure results provided by the above application examples and comparative application examples are shown in Table 3.

[0084] Table 3

[0085]

[0086]

[0087] According to Table 3, we can know the following points:

[0088] (1) Comprehensive analysis of application examples 1-5 shows that the etching solution provided by the present invention has excellent etching effect. After etching, the structure of the molten pool of the 1J22 soft magnetic alloy welding is clearly visible and the metallographic structure is clear, which fully meets the observation and analysis of geometric morphology information such as the grain size, morphology, distribution position and angle between grains of the alloy;

[0089] (2) Comprehensive analysis of Application Example 1 and Application Examples 6-9 shows that the immersion time of the etching solution provided by the present invention during use will affect the etching effect. If the immersion time is too short, the outline of the solder joint and the gold grid pattern will be blurred. If the immersion time is too long, the entire surface of the black solder joint will be covered with gold grids, and the metallographic structure morphology cannot be clearly displayed.

[0090] (3) Comprehensive analysis of Application Example 1 and Comparative Application Examples 1-12 shows that the content of each component in the etching solution provided by the present invention affects the etching effect of the etching solution;

[0091] For example, when the content of copper chloride is too low, it will result in a completely black surface without gold grid patterns; when the content is too high, it will result in distortion of the shape and size of the gold grid.

[0092] For example, in comparative application examples 4-6, when the content of anhydrous ethanol is too low, the gold grid lines will be blurred; when the content is too high, there will be no gold grid lines;

[0093] For example, when the content of hydrochloric acid is too low, the gold grid gaps cannot be etched, and the gold grid lines are blurred; when the content is too high, the entire surface will turn black without gold grid lines.

[0094] For example, in comparative application examples 10-12, when the water content is low, a completely black fuzzy grid with fuzzy boundaries will be formed; when the water content is high, the outline / boundary of the grid will be fuzzy.

[0095] (4) Comprehensive analysis of Application Example 1 and Comparative Application Examples 13-14 shows that the composition of the etching solution provided by the present invention affects the etching effect of the etching solution;

[0096] For example, in comparative application example 13, when the components of the etching solution include water and oxalic acid, the entire surface will turn black without gold grid patterns; for example, in comparative application example 14, when the components of the etching solution are adjusted from copper chloride to copper sulfate, the gold grid will turn black and the boundary with the surrounding area will be blurred; for example, in comparative application example 15, when the components of the etching solution are adjusted from hydrochloric acid to sulfuric acid, the entire surface will turn black without gold grid patterns.

[0097] In summary, the etching solution provided by the present invention has excellent etching effect. After etching, the structure of the 1J22 soft magnetic alloy welding pool is clearly visible and the metallographic structure is clear, which fully meets the observation and analysis of geometric morphological information such as grain size, shape, distribution position and angle between grains of the alloy.

[0098] The applicant declares that the above is only a specific implementation mode of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily thought of by those skilled in the art within the technical scope disclosed by the present invention shall fall within the protection scope and disclosure scope of the present invention.

Claims

1. A 1J22 soft magnetic alloy welding metallographic etching solution, characterized in that: The 1J22 soft magnetic alloy welding metallographic etching solution comprises: cupric chloride, anhydrous ethanol, hydrochloric acid and water.

2. The 1J22 soft magnetic alloy welding metallographic etching liquid according to claim 1, characterized in that: Calculated by weight, the 1J22 soft magnetic alloy welding metallographic etching solution comprises: 1-3 parts of cupric chloride, 7-13 parts of anhydrous ethanol, 12-20 parts of hydrochloric acid and 42-62 parts of water.

3. The 1J22 soft magnetic alloy welding metallographic etching liquid according to claim 2, characterized in that: Calculated by weight, the 1J22 soft magnetic alloy welding metallographic etching solution includes: 2 parts of cupric chloride, 10 parts of anhydrous ethanol, 16 parts of hydrochloric acid and 52 parts of water.

4. The 1J22 soft magnetic alloy welding metallographic etching solution according to any one of claims 1 to 3, characterized in that: The concentration of the copper chloride is 38-42wt%; Preferably, the concentration of the hydrochloric acid is 35-37 wt %.

5. A method for using the 1J22 soft magnetic alloy welding metallographic etching solution as described in any one of claims 1 to 4, characterized in that: The method of use comprises the following steps: The 1J22 soft magnetic alloy welding pool sample is immersed in the etching solution according to any one of claims 1 to 3, and is cleaned and dried in sequence, and then the metallographic structure is observed using a metallographic microscope.

6. The method of use according to claim 5, characterized in that: The melting depth of the 1J22 soft magnetic alloy welding molten pool is 0.15-0.3 mm.

7. The method of use according to claim 5 or 6, characterized in that: The soaking time is 160 to 200 seconds, preferably 180 seconds.

8. The method of use according to any one of claims 5 to 7, characterized in that: The soaking temperature is 20-30°C.

9. The method of use according to any one of claims 5 to 7, characterized in that: The welding method of the 1J22 soft magnetic alloy includes laser welding; The diameter of the welding spot in the laser welding is 0.3-0.4 mm.

10. The method of use according to any one of claims 5 to 9, characterized in that: The method of use includes: Under the temperature condition of 20-30° C., immerse the 1J22 soft magnetic alloy welding pool sample in the etching solution according to any one of claims 1 to 3 for 160-200 seconds, perform cleaning treatment and drying treatment in sequence, and then observe the metallographic structure using a metallographic microscope; Wherein, the melting depth of the 1J22 soft magnetic alloy welding pool is 0.15-0.3 mm.

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