CN114892172A - Metallographic corrosive liquid and application thereof - Google Patents

Metallographic corrosive liquid and application thereof Download PDF

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Publication number
CN114892172A
CN114892172A CN202210569459.8A CN202210569459A CN114892172A CN 114892172 A CN114892172 A CN 114892172A CN 202210569459 A CN202210569459 A CN 202210569459A CN 114892172 A CN114892172 A CN 114892172A
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metallographic
sample
cofe alloy
nitric acid
hydrochloric acid
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肖惠云
蔡新志
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Vital Thin Film Materials Guangdong Co Ltd
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Vital Thin Film Materials Guangdong Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23FNON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00Etching metallic material by chemical means
    • C23F1/10Etching compositions
    • C23F1/14Aqueous compositions
    • C23F1/16Acidic compositions
    • C23F1/28Acidic compositions for etching iron group metals
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/32Polishing; Etching
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C19/00Alloys based on nickel or cobalt
    • C22C19/07Alloys based on nickel or cobalt based on cobalt
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/10Ferrous alloys, e.g. steel alloys containing cobalt

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  • General Chemical & Material Sciences (AREA)
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Abstract

The invention belongs to the field of metallographic phase display, and discloses a metallographic phase corrosive liquid and application thereof. The metallographic etchant is a mixed solution of concentrated nitric acid, concentrated hydrochloric acid and water, and the volume ratio of the concentrated nitric acid to the concentrated hydrochloric acid to the water in the mixed solution is 2: 1: 1; the mass percentage concentration of the concentrated nitric acid is 60-70%, and the mass percentage concentration of the concentrated hydrochloric acid is 28-35%. The metallographic corrosive liquid can effectively corrode CoFe alloys with different components, enables the metallographic structure of the CoFe alloy to be clearly observed, and can clearly mark the grain size. Obvious defects of the CoFe alloy can be observed under a metallographic microscope, and whether the alloy meets the product requirements or not is convenient to judge, so that the preparation process and related parameters of the alloy can be adjusted in time, the failure rate of related products is reduced, and the economic benefit of the products is improved.

Description

Metallographic corrosive liquid and application thereof
Technical Field
The invention belongs to the field of metallographic phase display, relates to a metallographic phase corrosive liquid and application thereof, and particularly relates to a CoFe alloy metallographic phase corrosive liquid and application thereof.
Background
The internal structure of the metal material is directly and closely related to the material properties such as hardness, strength, ductility and the like, and metallographic observation is the most direct and effective method for researching the internal structure of the metal material. The metallographic phase refers to chemical components of metal or alloy and physical states and chemical states of various components in the metal or alloy, and the metallographic phase display is a common technology for observing the internal structure of the metal and the alloy thereof.
In the metallographic observation process, the metallographic corrosive liquid is essential, and the corrosion effect of the metallographic specimen is a key factor for metallographic structure analysis and defect analysis. The corrosion effect of the metallographic corrosive liquid on the alloy mainly depends on the acid used for preparing the corrosive liquid and the preparation proportion thereof, and if the type of the acid is not proper, the required corrosion effect cannot be achieved no matter what preparation proportion. If the proper acid type is selected, over corrosion is easily formed if the preparation ratio is too high, and the grain boundary cannot be corroded if the preparation ratio is too low. Therefore, the preparation of the corrosive liquid is extremely critical to observe a clear metallographic structure.
The CoFe alloy is used for producing magnetic alloy and hard alloy with abrasion resistance and high temperature resistance, and has wide application prospect in the fields of magnetic recording, catalysis, wave absorption, biomedicine and the like. The chemical components of the CoFe alloy can be divided into the following classes according to the mass percentage: co70% Fe30%, Co50% Fe50% and Co5% Fe 95%. At present, the metallographic corrosion data of the CoFe alloy is less, and only a document that the metallographic corrosion is carried out on the CoFe alloy containing Co5% and Fe95% by using an ethanol-nitric acid corrosive liquid is found out, but tests prove that the corrosive liquid has a good corrosion effect only on the CoFe alloy containing Co5% and Fe95%, and the corrosion effect on the CoFe alloy containing Co70% Fe30%, Co50% Fe50% or other components is not ideal.
Disclosure of Invention
In view of the problems in the prior art, one of the objectives of the present invention is to provide a metallographic etchant that can effectively corrode CoFe alloys of different compositions.
The second purpose of the invention is to provide the application of the metallographic corrosive liquid in the preparation process of the CoFe alloy metallographic phase.
In order to realize the purpose of the invention, the specific technical scheme is as follows:
the utility model provides a metallographic etchant which is the mixed solution of concentrated nitric acid, concentrated hydrochloric acid and water, and the volume ratio of concentrated nitric acid, concentrated hydrochloric acid and water in the mixed solution is 2: 1: 1; the mass percentage concentration of the concentrated nitric acid is 60-70%, and the mass percentage concentration of the concentrated hydrochloric acid is 28-35%.
Preferably, the mass percentage concentration of the concentrated nitric acid is 68%, and the mass percentage concentration of the concentrated hydrochloric acid is 32%.
The invention also discloses an application of the metallographic corrosive liquid in a CoFe alloy metallographic preparation process.
Preferably, the CoFe alloy metallographic preparation process comprises the following steps:
(1) preparing a metallographic corrosive liquid: adding distilled water into the container, then adding concentrated nitric acid and concentrated hydrochloric acid, and uniformly stirring to obtain a metallographic corrosive liquid;
(2) adding the polished CoFe alloy sample into a container containing the metallographic corrosive liquid obtained in the step (1), and immersing the sample in the corrosive liquid;
(3) after the corrosion is finished, cleaning with pure water and absolute ethyl alcohol;
(4) and (4) carrying out metallographic structure observation on the sample cleaned in the step (3).
Preferably, in the step (2), the etching time is 1.5-3 min.
Preferably, in the step (2), the preparation method of the sanded and polished CoFe alloy sample comprises the following steps:
providing a CoFe alloy metallographic sample, cutting the sample according to a gold phase sample preparation standard to obtain a sample, and then carrying out sample embedding treatment;
and (4) performing rough polishing and fine polishing on the embedded sample in sequence until the surface is bright, and showing an obvious mirror surface without scratches to obtain the polished CoFe alloy sample.
Preferably, the process of the mounting treatment is as follows: placing the sample in a mold, and mixing the epoxy resin and the curing agent according to the mass ratio of the epoxy resin: curing agent = 4: 1 mixing materials, pouring into a mould, and taking out after curing.
Preferably, the rough polishing is performed using P180, P320, P500, P1200, P2500 sandpaper in sequence.
Preferably, the rough polishing step is:
grinding the mixture for 30-60 min by using P180 sand paper, wherein the rotating speed is 200-300 r/min;
and (3) sequentially replacing the P320, P500, P1200 and P2500 sandpaper for grinding, wherein the grinding is carried out for 1-2 min each time at the rotating speed of 200-300 r/min.
Preferably, the finish polishing is performed using a 0.25 μm polishing cloth.
Compared with the prior art, the invention has the beneficial effects that:
(1) the metallographic corrosive liquid can effectively corrode CoFe alloys with different components, but is not effective on the CoFe alloy with one component. The corrosive liquid enables the metallographic structure of the CoFe alloy to be clearly observed, and the grain size can be clearly marked. Defects can be obviously observed under a metallographic microscope after the alloy is corroded, and whether the alloy meets the product requirements or not can be conveniently judged, so that the preparation process and related parameters of the alloy can be timely adjusted, the failure rate of related products is reduced, and the economic benefit of the products is improved.
(2) The method has the advantages of simple operation steps, low cost and short time consumption, and the CoFe alloy sample treated by the method has clear metallographic structure when observed under a metallographic microscope, so that an excellent metallographic observation result is obtained.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a gold phase diagram (5 times) of a CoFe alloy in example 2;
FIG. 2 is a gold phase diagram (10 times) of a CoFe alloy in example 2;
FIG. 3 is a gold phase diagram (10 times) of a CoFe alloy in comparative example 2;
FIG. 4 is a gold phase diagram (5 times) of a CoFe alloy in example 3;
FIG. 5 is a first (5-fold) phase diagram of the CoFe alloy of comparative example 3;
FIG. 6 is a second (5-fold) phase diagram of the CoFe alloy in comparative example 3;
FIG. 7 is a gold phase diagram (5 times) of a CoFe alloy in example 4;
FIG. 8 is a gold phase diagram (5 times) of the CoFe alloy in comparative example 4.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1
This embodiment provides a metallographic etchant, and metallographic etchant is the mixed solution of concentrated nitric acid, concentrated hydrochloric acid and water, and the volume ratio of concentrated nitric acid, concentrated hydrochloric acid and water is 2 in the mixed solution: 1: 1.
in this example, the mass percentage concentration of the concentrated nitric acid is 68%, and the mass percentage concentration of the concentrated hydrochloric acid is 32%.
The preparation method of the metallographic etchant of the embodiment is as follows:
firstly, measuring 20ml of pure water by using a measuring cup, pouring the pure water into a beaker with the capacity of 150ml, then measuring 40ml of concentrated hydrochloric acid and 20ml of concentrated nitric acid respectively, slowly pouring the concentrated nitric acid into the beaker, and stirring the concentrated hydrochloric acid and the concentrated nitric acid by using a glass rod to uniformly mix the concentrated hydrochloric acid and the concentrated nitric acid.
Comparative example 1
The comparative example provides a metallographic etchant, which is an ethanol-nitric acid etchant, and the etchant is prepared from ethanol (96%): nitric acid (68%) was added at volume ratio = 49: 1, preparing the mixture.
The preparation method comprises the following steps:
98ml of ethanol (96%) was measured in a measuring cup, and poured into a beaker with a capacity of 150ml, and 2ml of nitric acid (68%) was measured, slowly poured into the beaker, and stirred with a glass rod to mix them uniformly.
Example 2
The embodiment discloses a metallographic preparation method of a CoFe alloy, the CoFe alloy comprises the following components of Co70% and Fe30%, and the CoFe alloy metallographic corrosive liquid in the embodiment 1 is used, and the method specifically comprises the following steps:
(1) sampling the CoFe target by using water cutting equipment to obtain a sample with the thickness of 15 multiplied by 7 mm;
(2) the sample was placed in a mold, with the epoxy resin: curing agent = 4: 1, pouring the prepared sample into a mold, and taking out the sample from the mold after the sample is solidified;
(3) roughly polishing the sample on a metallographic automatic polishing machine, grinding the sample by using new P180 sand paper for 30min at a rotating speed of 250 r/min, and removing obvious cutting marks on the surface; then sequentially replacing P320, P500, P1200 and P2500 sandpaper for rough polishing, and grinding for 1min each time at the rotating speed of 300 r/min;
(4) replacing polishing cloth with a diameter of 0.25 μm, finely polishing the sample by matching with polishing solution with a diameter of 0.25 μm, and after 2min, the sample surface is bright, presents an obvious mirror surface and has no scratch, can be washed by clean water and then scrubbed by alcohol;
(5) pouring CoFe alloy metallographic corrosive liquid into a small beaker with the capacity of 50ml, putting a polished sample into the corrosive liquid to ensure that the sample is immersed in the corrosive liquid, so that the surface of the sample to be corroded is fully contacted with the corrosive liquid, corroding for 2.5min, taking out the sample after corrosion is finished, washing the sample with a large amount of pure water, and scrubbing the surface of the sample by using dust-free paper and alcohol to ensure that no corrosive liquid remains on the surface of the sample;
(6) and after the corrosion is finished, the surface of the sample is placed under a microscope for observation.
Referring to the attached drawings 1-2, the metallographic pictures of the CoFe alloy in the present embodiment are shown in different multiples. After the alloy is treated by the method of the embodiment 2, the metallographic structure of the alloy is clear and obvious, the grain boundary is clear, and the grains are fine.
Comparative example 2
Comparative example 2 is substantially the same as example 2 except that the etching solution in step (5) is different, and comparative example 2 employs the ethanol-nitric acid etching solution in comparative example 1.
And (3) placing the metallographic sample obtained in the comparative example 2 in a metallographic microscope for observation, wherein the attached figure 3 is a metallographic picture of the CoFe alloy in the comparative example 2, and comparing the metallographic picture with the pictures 1 and 2 in the example 2, so that the corrosive liquid used in the comparative example 2 has no corrosive effect on the CoFe alloy.
Example 3
This embodiment is basically the same as embodiment 2, except that:
the CoFe alloy comprises the components of Co50% and Fe 50%.
Referring to fig. 4, a metallographic picture of the CoFe alloy in the present example is shown. After the alloy is treated by the method of the embodiment 3, the metallographic structure of the alloy is clear and obvious, the grain boundary is clear, and the grains are fine.
Comparative example 3
Comparative example 3 is substantially the same as example 3 except that the etching solution in step (5) is different, and comparative example 3 employs the ethanol-nitric acid etching solution in comparative example 1.
And (3) placing the metallographic sample obtained in the comparative example 3 in a metallographic microscope for observation, wherein the attached drawings 5 and 6 are metallographic pictures of the CoFe alloy in the comparative example 3 under different multiples respectively, and comparing with the figure 4 in the example 3, it can be seen that the corrosive liquid used in the comparative example 3 has no corrosive effect on the CoFe alloy.
Example 4
This embodiment is basically the same as embodiment 2, except that:
the CoFe alloy comprises the components of Co5% and Fe 95%.
Referring to fig. 7, the metallographic images of the CoFe alloy in this example are shown. After the alloy is treated by the method of the embodiment 4, the metallographic structure of the alloy is clear and obvious, the grain boundary is clear, and the grains are fine.
Comparative example 4
Comparative example 4 is substantially the same as example 4 except that the etching solution in step (5) is different, and comparative example 4 employs the ethanol-nitric acid etching solution in comparative example 1.
The metallographic sample obtained in the comparative example 4 is placed in a metallographic microscope for observation, and the attached figure 8 is a metallographic picture of the CoFe alloy in the comparative example 4 and can be seen by comparing with the picture 7 in the example 4: the alloy has clear and obvious metallographic structure, clear grain boundary and fine grains, and shows that the corrosive liquids used in the example 4 and the comparative example 4 have better corrosive effects on CoFe alloys containing Co5% and Fe 95%.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (10)

1. The metallographic etchant is a mixed solution of concentrated nitric acid, concentrated hydrochloric acid and water, wherein the volume ratio of the concentrated nitric acid to the concentrated hydrochloric acid to the water in the mixed solution is 2: 1: 1; the mass percentage concentration of the concentrated nitric acid is 60-70%, and the mass percentage concentration of the concentrated hydrochloric acid is 28-35%.
2. The metallographic etchant according to claim 1, wherein the concentrated nitric acid has a concentration of 68% by mass and the concentrated hydrochloric acid has a concentration of 32% by mass.
3. Use of a metallographic etching solution according to claim 1 or 2 in the preparation of a CoFe alloy metallographic phase.
4. The use of claim 3, wherein said CoFe alloy metallographic phase preparation comprises the steps of:
(1) preparing a metallographic corrosive liquid: adding distilled water into the container, then adding concentrated nitric acid and concentrated hydrochloric acid, and uniformly stirring to obtain a metallographic corrosive liquid;
(2) adding the polished CoFe alloy sample into a container containing the metallographic etchant in the step (1), and immersing the sample in the metallographic etchant;
(3) after the corrosion is finished, cleaning a CoFe alloy sample by using pure water and absolute ethyl alcohol;
(4) and (4) carrying out metallographic structure observation on the CoFe alloy sample cleaned in the step (3).
5. The use according to claim 4, wherein in step (2), the etching time is 1.5-3 min.
6. The use of claim 4, wherein in the step (2), the grinding and polishing step is:
providing a CoFe alloy metallographic sample, cutting the sample according to a gold phase sample preparation standard to obtain a sample, and then carrying out sample embedding treatment;
and (4) performing rough polishing and fine polishing on the embedded sample in sequence until the surface is bright and has no scratch.
7. The use of claim 6, wherein the imbedding process is carried out by: placing the sample in a mold, and mixing the epoxy resin and the curing agent according to the mass ratio of the epoxy resin: curing agent = 4: 1 mixing materials, pouring into a mould, and taking out after curing.
8. The use of claim 6, wherein the rough polishing is performed using P180, P320, P500, P1200, P2500 sandpaper in that order.
9. The use of claim 8, wherein the rough polishing step is:
grinding the mixture for 30-60 min by using P180 sand paper, wherein the rotating speed is set to be 200-300 r/min;
and (3) sequentially replacing the P320, P500, P1200 and P2500 sandpaper for grinding, wherein the grinding time is 1-2 min each time, and the rotating speed is set to be 200-300 r/min.
10. Use according to claim 6, characterized in that the finish polishing is carried out using a 0.25 μm polishing cloth.
CN202210569459.8A 2022-05-24 2022-05-24 Metallographic corrosive liquid and application thereof Pending CN114892172A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102980794A (en) * 2012-11-08 2013-03-20 中国船舶重工集团公司第七二五研究所 Metallographic erosion method for displaying cobalt-chromium alloy structure
CN104562012A (en) * 2014-12-07 2015-04-29 金川集团股份有限公司 Iron-base high-temperature alloy sample metallographic etching solution and etching method
CN105241885A (en) * 2015-09-30 2016-01-13 金川集团股份有限公司 Forged magnetically soft alloy 1J50 alloy metallographic corrosive liquid and applications thereof
CN107727476A (en) * 2017-11-30 2018-02-23 西安诺博尔稀贵金属材料有限公司 A kind of observation procedure of the PtCo alloy microstructures of the atomic ratio such as

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102980794A (en) * 2012-11-08 2013-03-20 中国船舶重工集团公司第七二五研究所 Metallographic erosion method for displaying cobalt-chromium alloy structure
CN104562012A (en) * 2014-12-07 2015-04-29 金川集团股份有限公司 Iron-base high-temperature alloy sample metallographic etching solution and etching method
CN105241885A (en) * 2015-09-30 2016-01-13 金川集团股份有限公司 Forged magnetically soft alloy 1J50 alloy metallographic corrosive liquid and applications thereof
CN107727476A (en) * 2017-11-30 2018-02-23 西安诺博尔稀贵金属材料有限公司 A kind of observation procedure of the PtCo alloy microstructures of the atomic ratio such as

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Application publication date: 20220812