CN113984473A - Ultra-low carbon steel metallographic corrosive and display method of metallographic structure - Google Patents
Ultra-low carbon steel metallographic corrosive and display method of metallographic structure Download PDFInfo
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- CN113984473A CN113984473A CN202111273673.0A CN202111273673A CN113984473A CN 113984473 A CN113984473 A CN 113984473A CN 202111273673 A CN202111273673 A CN 202111273673A CN 113984473 A CN113984473 A CN 113984473A
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- 229910001209 Low-carbon steel Inorganic materials 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 21
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000003518 caustics Substances 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 13
- 229960000583 acetic acid Drugs 0.000 claims abstract description 12
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910000975 Carbon steel Inorganic materials 0.000 claims abstract description 5
- 239000010962 carbon steel Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000007664 blowing Methods 0.000 claims description 4
- 230000003287 optical effect Effects 0.000 claims description 3
- 230000007797 corrosion Effects 0.000 abstract description 14
- 238000005260 corrosion Methods 0.000 abstract description 14
- 239000013078 crystal Substances 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 6
- 239000002352 surface water Substances 0.000 abstract description 2
- 230000002349 favourable effect Effects 0.000 abstract 1
- 238000005498 polishing Methods 0.000 description 8
- 230000003628 erosive effect Effects 0.000 description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 6
- 238000000227 grinding Methods 0.000 description 6
- 229910000859 α-Fe Inorganic materials 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000010587 phase diagram Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 description 2
- 229940001584 sodium metabisulfite Drugs 0.000 description 2
- 235000010262 sodium metabisulphite Nutrition 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- SNIOPGDIGTZGOP-UHFFFAOYSA-N Nitroglycerin Chemical compound [O-][N+](=O)OCC(O[N+]([O-])=O)CO[N+]([O-])=O SNIOPGDIGTZGOP-UHFFFAOYSA-N 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- KSOKAHYVTMZFBJ-UHFFFAOYSA-N iron;methane Chemical group C.[Fe].[Fe].[Fe] KSOKAHYVTMZFBJ-UHFFFAOYSA-N 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229940073020 nitrol Drugs 0.000 description 1
- MYHXWQZHYLEHIU-UHFFFAOYSA-N oxalic acid;sulfuric acid Chemical compound OS(O)(=O)=O.OC(=O)C(O)=O MYHXWQZHYLEHIU-UHFFFAOYSA-N 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
- 235000019345 sodium thiosulphate Nutrition 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 239000000080 wetting agent Substances 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
- 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
-
- 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
- G01N1/32—Polishing; Etching
-
- 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
- G01N1/34—Purifying; Cleaning
-
- 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
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
Abstract
The invention discloses a preparation method of an ultralow-carbon steel metallographic corrosive agent and a display method of a metallographic structure, and relates to the technical field of metallographic preparation. The corrosive agent consists of absolute ethyl alcohol, nitric acid and glacial acetic acid, wherein the volume content of the absolute ethyl alcohol is 90%, the volume content of the nitric acid is 5%, and the balance is the glacial acetic acid, and the corrosive agent can be obtained by uniformly mixing the absolute ethyl alcohol, the nitric acid and the glacial acetic acid. The display method of the metallographic structure is a one-step corrosion method, firstly, the surface water stain of a precisely polished ultra-low carbon steel sample is dried, then the sample is directly corroded for 50s by a corrosive agent at normal temperature, and then the sample surface is washed by clear water and dried, so that the metallographic structure can be observed. The metallographic corrosive provided by the invention has the advantages of short corrosion time, simple corrosion steps and convenience in operation, can make the crystal boundary of crystal grains in the ultra-low carbon steel clear, and is favorable for measuring the size of the crystal grains.
Description
Technical Field
The invention relates to the technical field of metallographic preparation, in particular to a preparation method of an ultralow-carbon steel metallographic corrosive agent and a display method of a metallographic structure.
Background
The ultra-low carbon steel is interstitial-free steel, has excellent deep drawing performance and is widely applied to the industries of automobiles and household appliances. Because the ultra-low carbon steel is relatively pure, the metallographic structure is a pure ferrite structure, and no residual interstitial atoms exist in the grain boundary, the grain boundary of ferrite obtained by corroding the ultra-low carbon steel by using a low-carbon ferrite steel metallographic corrosive agent nitric acid alcoholic solution is fuzzy, as shown in figure 1, and great difficulty is caused to metallographic analysis.
The patent CN102890027A discloses a metallographic structure display method for a gapless atomic steel cold-rolled sheet containing Ti, the method comprises the steps of preparing a polished sample by using an ethanol aqueous solution prepared by mixing absolute ethanol and water according to a volume ratio of 2: 3-7: 3 as a lubricant in the polishing process of the polished sample, then corroding by using a two-step method, wherein in the first step of corroding, a first corrosive agent prepared by adding an oxalic acid sulfate aqueous solution, hydrogen peroxide and hydrofluoric acid is used for corroding; and the second step of erosion adopts the nital solution to continue the erosion. Although clear metallographic specimen ferrite grain boundaries can be obtained through the operation of the patent, cementite structures in the ferrite grain boundaries and on the grain boundaries and fiber structures in an incompletely recrystallized state can also be clearly displayed, the whole operation process is long in time and complicated in steps, a polishing agent is required to be prepared by using absolute ethyl alcohol and water, and the erosion operation is also carried out through two steps. In addition, the hydrofluoric acid in the corrosive agent needs special care during the use process, because once the hydrofluoric acid is stained on the skin, the harm to human bodies is large.
Patent CN1167257A discloses a method for displaying metallographic structure of cold-rolled annealed interstitial-free steel, which comprises the steps of firstly eroding by nital, then carrying out secondary erosion by a corrosive agent containing sodium metabisulfite and sodium thiosulfate, then washing, and wiping off a light blue surface layer to obtain a clear metallographic structure. This patent also adopts the two-step method to carry out the erosion operation, needs to dispose two kinds of corrosive agents, and the erosion step is loaded down with trivial details, and in the actual operation, the failure of any process can all produce unclear metallographic structure, brings great work load for the metallographic system appearance, and in addition, sodium metabisulfite is extremely easy to oxidize in the air, and it is all difficult to deposit and transport.
Disclosure of Invention
The invention aims to solve the problems of difficult corrosion, poor operation controllability, long test time consumption, high manufacturing cost and difficult medicament storage in the prior art in the process of metallographic detection of ultra-low carbon steel, and provides a display method for an ultra-low carbon steel metallographic corrosive agent and a metallographic structure. The metallographic corrosive agent has short corrosion time, simple corrosion steps and easy control, can make the crystal boundary of crystal grains in the ultra-low carbon steel clear after being corroded by the corrosive agent, and is beneficial to the measurement of the size of the crystal grains.
In order to realize the technical purpose, the invention adopts the following scheme:
the ultra-low carbon steel metallographic corrosive agent consists of absolute ethyl alcohol, nitric acid and glacial acetic acid, and the mixing volume ratio of the absolute ethyl alcohol, the nitric acid and the glacial acetic acid is 18:1: 1.
The mass percentage concentration of the absolute ethyl alcohol is 99.5%, the mass percentage concentration of the nitric acid is 65-68%, and the mass percentage concentration of the glacial acetic acid is 99.5%.
The method for displaying the metallographic structure of the ultra-low carbon steel is characterized in that the surface water stain of the ultra-low carbon steel sample after being polished is dried by blowing, then the corrosive agent is directly used for corroding the ultra-low carbon steel sample for 50s at normal temperature, then the surface of the sample is washed by clear water, and the metallographic structure is observed by adopting an optical microscope after being dried by blowing.
Compared with the prior art, the invention has the beneficial effects that: the metallographic corrosive provided by the invention has the advantages of short corrosion time, simple corrosion steps and convenience in operation, and clear metallographic structures can be obtained after corrosion.
Drawings
FIG. 1 is a ferritic gold phase diagram of ultra low carbon steel nitrol corrosion;
FIG. 2 is a ferritic gold phase diagram of ultra-low carbon steel according to an embodiment of the present invention.
Detailed Description
The present invention will be described in detail with reference to the following embodiments in order to fully understand the objects, features and effects of the invention, but the present invention is not limited thereto.
The invention provides an ultralow-carbon steel metallographic corrosive agent which is formed by mixing absolute ethyl alcohol, nitric acid and glacial acetic acid, wherein the volume content of the absolute ethyl alcohol is 90%, the volume content of the nitric acid is 5%, and the balance is the glacial acetic acid, wherein the mass percentage concentration of the absolute ethyl alcohol is 99.5%, the mass percentage concentration of the nitric acid is 65-68%, and the mass percentage concentration of the glacial acetic acid is 99.5%. The three substances are mixed uniformly to obtain the corrosive provided by the invention.
The method for displaying the metallurgical structure of the ultra-low carbon steel is a one-step corrosion method and comprises the following steps of:
step one, sample preparation: preparing an ultra-low carbon steel sample according to a metallographic sample preparation standard, and sequentially grinding until scratches of the previous pass completely disappear by adopting a mechanical grinding mode and using coarse-to-fine water-based abrasive paper (600 meshes, 1200 meshes and 2000 meshes) and water as a grinding medium. The ground sample is roughly polished by using water as a wetting agent and using a high-efficiency polishing agent (components: diamond micro powder and grinding medium) with the granularity of 2.5 mu m on the damping cloth polishing cloth; then fine polishing is carried out on the velvet polishing cloth by using a high-efficiency polishing agent (the components are diamond micro powder and a grinding medium) with the granularity of 1 mu m; the rotating speed of the grinding wheel for mechanical polishing is 600 r/min-750 r/min, and the time for mechanical polishing is 1 min-2 min.
Step two, corrosion: and uniformly spreading a metallographic corrosive agent on the surface of the finely polished ultra-low carbon steel sample in a wetting mode for metallographic corrosion, wherein the corrosion time is 30-50 s, finally washing with clear water, drying the surface of the sample, and observing under an optical microscope, wherein the result is shown in fig. 2.
Comparing fig. 1 and fig. 2, it can be known that the grain boundary of the ultra-low carbon steel ferrite obtained by the ultra-low carbon steel metallographic corrosive and the display method of the metallographic structure provided by the invention is clear, which is beneficial to the measurement of the grain size.
Finally, it is noted that: the above-mentioned list is only the preferred embodiment of the present invention, and naturally those skilled in the art can make modifications and variations to the present invention, which should be considered as the protection scope of the present invention provided they are within the scope of the claims of the present invention and their equivalents.
Claims (3)
1. The ultralow-carbon steel metallographic corrosive agent is characterized by comprising absolute ethyl alcohol, nitric acid and glacial acetic acid, wherein the mixing volume ratio of the absolute ethyl alcohol to the nitric acid to the glacial acetic acid is 18:1: 1.
2. The ultralow-carbon steel metallographic etchant according to claim 1, wherein the absolute ethyl alcohol is 99.5% by mass, the nitric acid is 65-68% by mass, and the glacial acetic acid is 99.5% by mass.
3. A display method of a metallographic structure of ultra-low carbon steel is characterized in that the surface of a polished ultra-low carbon steel sample is dried by blowing, then the corrosive agent in claim 1 or 2 is directly used for corroding the surface of the ultra-low carbon steel sample for 50s at normal temperature, then the surface of the sample is washed by clear water, and the metallographic structure is observed by an optical microscope after the sample is dried by blowing.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111273673.0A CN113984473A (en) | 2021-10-29 | 2021-10-29 | Ultra-low carbon steel metallographic corrosive and display method of metallographic structure |
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| CN202111273673.0A CN113984473A (en) | 2021-10-29 | 2021-10-29 | Ultra-low carbon steel metallographic corrosive and display method of metallographic structure |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114457335A (en) * | 2022-02-15 | 2022-05-10 | 江西省科学院应用物理研究所 | Copper-iron-carbon alloy metallographic etchant and application method thereof |
| CN114774921A (en) * | 2022-04-19 | 2022-07-22 | 东南大学 | Metallographic corrosive agent for deformed tin bronze and grain display method thereof |
| CN115386879A (en) * | 2022-08-15 | 2022-11-25 | 武汉钢铁有限公司 | Corrosive agent and corrosion method for ultra-low carbon silicon steel |
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| CN104532242A (en) * | 2014-11-28 | 2015-04-22 | 振石集团东方特钢股份有限公司 | Austenitic stainless steel metallography corrosion agent and austenitic stainless steel metallography display method |
| CN110118778A (en) * | 2019-05-13 | 2019-08-13 | 中天钢铁集团有限公司 | A kind of medium carbon steel ferrite metallographic etching agent and ferritic structure metallographic phase display method |
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- 2021-10-29 CN CN202111273673.0A patent/CN113984473A/en active Pending
Patent Citations (2)
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| CN104532242A (en) * | 2014-11-28 | 2015-04-22 | 振石集团东方特钢股份有限公司 | Austenitic stainless steel metallography corrosion agent and austenitic stainless steel metallography display method |
| CN110118778A (en) * | 2019-05-13 | 2019-08-13 | 中天钢铁集团有限公司 | A kind of medium carbon steel ferrite metallographic etching agent and ferritic structure metallographic phase display method |
Non-Patent Citations (1)
| Title |
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| 王振等: "La、 Ti 处理对 FeCrAl 不锈钢凝固组织的影响", 钢铁钒钛, vol. 34, no. 3, pages 101 - 105 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114457335A (en) * | 2022-02-15 | 2022-05-10 | 江西省科学院应用物理研究所 | Copper-iron-carbon alloy metallographic etchant and application method thereof |
| CN114457335B (en) * | 2022-02-15 | 2023-10-27 | 江西省科学院应用物理研究所 | Metallographic etchant for copper-iron-carbon alloy and use method thereof |
| CN114774921A (en) * | 2022-04-19 | 2022-07-22 | 东南大学 | Metallographic corrosive agent for deformed tin bronze and grain display method thereof |
| CN114774921B (en) * | 2022-04-19 | 2024-04-09 | 东南大学 | Metallographic corrosive for deformed tin bronze and crystal grain display method thereof |
| CN115386879A (en) * | 2022-08-15 | 2022-11-25 | 武汉钢铁有限公司 | Corrosive agent and corrosion method for ultra-low carbon silicon steel |
| CN115386879B (en) * | 2022-08-15 | 2023-11-28 | 武汉钢铁有限公司 | Corrosive agent for ultra-low carbon silicon steel and corrosion method |
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