CN114395790A - Corrosive liquid and corrosion method for preparing metallographic structure sample of ferrite and austenite dissimilar steel welded joint - Google Patents

Corrosive liquid and corrosion method for preparing metallographic structure sample of ferrite and austenite dissimilar steel welded joint Download PDF

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Publication number
CN114395790A
CN114395790A CN202111651154.3A CN202111651154A CN114395790A CN 114395790 A CN114395790 A CN 114395790A CN 202111651154 A CN202111651154 A CN 202111651154A CN 114395790 A CN114395790 A CN 114395790A
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sample
ferritic
austenitic
welded joint
metallographic structure
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CN114395790B (en
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李锦华
纪冬梅
金震杰
高巍
张世龙
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Shanghai University of Electric Power
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25FPROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F3/00Electrolytic etching or polishing
    • C25F3/02Etching
    • C25F3/06Etching of iron or steel
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25FPROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F3/00Electrolytic etching or polishing
    • C25F3/16Polishing
    • C25F3/22Polishing of heavy metals
    • C25F3/24Polishing of heavy metals of iron or steel

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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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Abstract

The invention relates to a corrosive liquid and a corrosion method for preparing a metallographic structure sample of a ferrite and austenite dissimilar steel welded joint, wherein the corrosive liquid comprises an electrolytic corrosive liquid and an electrolytic polishing liquid, the electrolytic corrosive liquid comprises picric acid, sodium dodecyl benzene sulfonate and concentrated hydrochloric acid, the proportion of the picric acid, the sodium dodecyl benzene sulfonate and the concentrated hydrochloric acid is 20 g: 8 g: 80-100 ml, the electrolytic polishing liquid comprises alcohol, perchloric acid and glycerol, and the volume ratio of the alcohol, the perchloric acid and the glycerol is 150 ml: 50 ml: 25 ml. The corrosive liquid can be used for preparing samples of metallographic structures of ferrite and austenite dissimilar steel welded joints, and is used for pretreating ferrite and austenite dissimilar steel welded joint samples and then carrying out electrolytic corrosion polishing treatment by using the corrosive liquid to obtain metallographic structure samples. Compared with the prior art, the corrosive liquid is not easy to generate excessive corrosion, and can quickly and clearly display the metallographic structure of the dissimilar steel welded joint; the etching method is simple to operate.

Description

Corrosive liquid and corrosion method for preparing metallographic structure sample of ferrite and austenite dissimilar steel welded joint
Technical Field
The invention belongs to the technical field of metallographic corrosion, and relates to a corrosive liquid and a corrosion method for preparing a metallographic structure sample of a ferrite and austenite dissimilar steel welded joint.
Background
Thermal power generation, especially coal-fired power generation, is the best comprehensive economy at present, the highest power generation form of technical maturity, and have high-efficient, energy-conserving, characteristics such as environmental protection supercritical (super) unit, can further reduce the energy consumption, raise the efficiency, improve the environment. In a supercritical (super) critical unit, steam temperatures of regions such as a boiler superheater and a reheater are different, requirements on corrosion resistance, oxidation resistance and high-temperature creep property of used pipes are also different, steam parameters of the regions such as the boiler superheater and the reheater are different, and requirements on corrosion resistance, thermal expansion coefficient, high-temperature creep property and the like of materials required by the parts are also different. Therefore, heterogeneous steel welded joint reheat engine unit species are widely applied, and main pipes widely applied to Super (supercritical) critical unit superheater and reheater heating surface pipe systems in China currently comprise T/P91, T/P92, Super304, T22, TP347H, S30432, TP347HFG, HR3C and the like.
The T91/TP347H dissimilar steel welding joint has good high-temperature strength, excellent high-temperature corrosion resistance and lower price, and is often applied to key parts of different working condition handover. However, the dissimilar steel welded joint has a severe service environment, and the structure is aged and the performance is degraded along with the service time, so how to effectively evaluate the metallographic structure of the welded joint has important significance for ensuring the safe use of the dissimilar steel joint.
However, compared with the same steel, the preparation of the dissimilar steel joint sample is difficult, and the reasons are mainly as follows:
(1) the electromagnetic difference of each area of the dissimilar steel welding joint is large;
(2) the welding seam and two base metal in the dissimilar steel welding joint are difficult to meet the requirement of equal strength;
(3) in the welding process of the dissimilar steel materials, the properties of the welded joint are deteriorated due to the change of the metallographic structure or the newly formed structure of the welded zone.
These factors all cause the electrochemical properties of different steel joints to be greatly different, and the corrosion method is more complicated and difficult compared with the same steel. As the traditional corrosive agents are strong acid etching agents, the traditional corrosive agents have good corrosion effect on typical austenitic steel, and for ferritic steel, the corrosion speed is too high, the corrosion time and the corrosion degree are difficult to control, the over-corrosion phenomenon is easy to occur, and the metallographic structure of a welded joint of ferritic and austenitic dissimilar steel is difficult to clearly display at one time by using the corrosive liquid in the prior art. Therefore, it is necessary to find a corrosion solution with moderate corrosion speed, safety and long-term stable use and a corrosion method with simple operation, which can rapidly and clearly display the metallographic structure of the welded joint of ferritic and austenitic dissimilar steels.
Disclosure of Invention
The invention aims to provide a corrosive liquid and a corrosion method for preparing a sample of a metallographic structure of a welded joint of dissimilar steel of ferrite and austenite, so as to overcome the defects that the corrosion method of the dissimilar steel joint in the prior art is complex, the existing corrosive liquid easily over corrodes the dissimilar steel joint or the metallographic structure of the welded joint of the dissimilar steel of ferrite and austenite is difficult to rapidly and clearly display, and the like.
The purpose of the invention can be realized by the following technical scheme:
one of the technical schemes of the invention provides an etching solution for preparing a metallographic structure sample of a welded joint of dissimilar steel of ferrite and austenite, which comprises an electrolytic etching solution and an electrolytic polishing solution, wherein the electrolytic etching solution comprises picric acid, sodium dodecyl benzene sulfonate and concentrated hydrochloric acid, the ratio of the picric acid to the sodium dodecyl benzene sulfonate to the concentrated hydrochloric acid is 20 g: 8 g: 80-100 ml, the electrolytic polishing solution comprises alcohol, perchloric acid and glycerol, and the volume ratio of the alcohol to the perchloric acid to the glycerol is 150 ml: 50 ml: 25 ml.
Further, the purity of the concentrated hydrochloric acid is 37 wt%, the purity of the alcohol is 95 vol%, the purity of the perchloric acid is 30 wt%, and the purity of the glycerol is 25 wt%.
The second technical scheme of the invention provides a corrosion method for preparing a metallographic structure sample of a welded joint of ferritic and austenitic dissimilar steel, which comprises the following steps:
(1) sampling a test sample at a welding joint of ferritic and austenitic dissimilar steels, and then pretreating the test sample to enable a surface to be observed to achieve a mirror surface effect, so as to obtain the test sample to be observed;
(2) taking a sample to be observed as an anode, a stainless steel plate as a cathode, and the electrolytic corrosion solution as electrolyte, carrying out electrolysis, and then washing to obtain a corroded sample to be observed;
(3) and taking the corroded sample to be observed as an anode, a stainless steel plate as a cathode, and the electrolytic polishing solution as electrolyte, electrolyzing, washing and blow-drying to finish sample preparation.
Further, in the step (1), the ferritic steel is T91 steel, and the austenitic steel is TP347H stainless steel.
Further, in the step (1), the pretreatment process is as follows:
and washing, roughly grinding, finely grinding and polishing the sample until the observation surface of the sample achieves a mirror surface effect.
Further, the washing process is as follows:
the sample was ultrasonically cleaned in absolute ethanol and then washed with water.
Further, the test piece was roughly ground using a grinder.
Furthermore, the fine grinding process comprises the following steps:
and (3) carrying out fine grinding treatment on the surface of the roughly ground sample by using 400-mesh, 600-mesh, 800-mesh and 1200-mesh metallographic abrasive paper in sequence.
Further, in the step (2), in the electrolysis process, the voltage is 12V, the temperature is 25 ℃, and the electrolysis time is 30-60 seconds.
Further, in the step (2), during the electrolysis, the voltage is 12V, the temperature is 25 ℃, and the electrolysis time is 45 seconds.
Further, in the step (3), in the electrolysis process, the voltage is 40-50V, the temperature is 25 ℃, and the electrolysis time is 5-15 seconds.
Further, step (2) and step (3) were carried out using an electrolytic polishing etcher of EP-06 type.
Further, in the step (3), after sample preparation is completed, metallographic structure observation is carried out by adopting a 10XB-PC type metallographic microscope.
The electrolytic corrosion liquid is prepared by dispersing picric acid in concentrated hydrochloric acid, and the electrolytic polishing liquid is prepared by uniformly mixing alcohol, perchloric acid and glycerol.
The corrosive liquid is used for the metallographic structure sample preparation process of a ferrite and austenite dissimilar steel welding joint, please refer to fig. 1, firstly, the adopted ferrite and austenite dissimilar steel welding joint sample is pretreated, then the corrosive liquid is prepared, and electrolytic corrosion polishing treatment is carried out, in the electrolytic corrosion, oxidizing ions with high electrode potential are subjected to discharge reduction at a cathode due to an external power supply, and more active metals with low electrode potential in an anode region are oxidized to form cations to be separated from the surface of a material, so that the corrosion of the anode is formed, and finally, the metallographic structure sample of the dissimilar steel welding joint is obtained.
For welding joints of ferritic and austenitic dissimilar steels, the sodium dodecyl benzene sulfonate is added into the picric acid salt solution as a corrosion inhibitor, so that intragranular corrosion can be reduced, the contrast of grain size corrosion can be improved, and the corrosion degree can be better mastered.
Compared with the prior art, the invention has the following advantages:
(1) the corrosive liquid can be used for preparing samples of metallographic structures of welded joints of ferritic and austenitic dissimilar steels, is not easy to excessively corrode, and can quickly and clearly display the metallographic structures of the welded joints of the dissimilar steels;
(2) the corrosion method is simple to operate and easy to operate and control, and has important guiding significance for production.
Drawings
FIG. 1 is a flow chart of the etching method of the present invention;
FIG. 2 is a metallographic structure morphology of a T91 side of a T91/TP347H dissimilar steel welded joint obtained in example 1;
FIG. 3 shows the metallographic structure of the TP347H side of the T91/TP347H dissimilar steel welded joint obtained in example 1;
FIG. 4 shows the metallographic structure of the weld of the T91/TP347H dissimilar steel weld joint obtained in example 1.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
In the following examples, unless otherwise specified, all of the conventional commercial starting materials and conventional processing techniques are used.
Example 1:
the embodiment provides a corrosive liquid for preparing a metallographic structure sample of a welded joint of dissimilar steel of ferrite and austenite, and a preparation method and application thereof, wherein the ferritic steel is T91 steel, the austenitic steel is TP347H stainless steel, and the specific operation steps are as follows:
(1) sampling: samples were taken at the T91/TP347H dissimilar steel weld joint.
(2) Pretreatment: completely soaking the sample in an absolute ethyl alcohol solution, placing the sample in an ultrasonic cleaning machine for ultrasonic cleaning, and washing the surface with clear water after the ultrasonic cleaning is finished; the method comprises the following steps of firstly, roughly grinding a test sample on a grinding machine, washing the roughly ground test sample by deionized water, and then, finely grinding the ground and polished surface on 400-mesh, 600-mesh, 800-mesh and 1200-mesh metallographic abrasive paper in sequence; and finally, cleaning the ground test sample, and polishing the test sample on a polishing machine until the observation surface of the test sample achieves the mirror surface effect.
(3) Preparing a corrosive liquid: the corrosion solution comprises electrolytic corrosion solution and electrolytic polishing solution, wherein the proportion of the electrolytic corrosion solution is 20g of picric acid, 8g of sodium dodecyl benzene sulfonate and 100ml of concentrated hydrochloric acid (37 wt%); the electrolytic polishing solution comprises 150ml of alcohol (95 vol%), 50ml of perchloric acid (30 wt%) and 25ml of glycerol (25 wt%).
(4) Electrolytic corrosion treatment: the electrolytic corrosion voltage is 12V, the temperature is 25 ℃, the anode is connected to a binding post of the sample, the binding post is connected with a stainless steel insulating clamp, the clamp clamps the test sample, the cathode is connected with the binding post of the stainless steel plate, the bottom end of the stainless steel plate is immersed in the electrolytic corrosion liquid, the liquid level of the electrolytic corrosion liquid submerges the corrosion surface of the test sample to be tested, and the electrolysis is carried out for 45 seconds.
(5) After the sample to be tested is corroded, the sample to be tested is cleaned and then is subjected to electrolytic polishing treatment:
the voltage of electrolytic polishing is 40V, the temperature is 25 ℃, the positive electrode is connected to a binding post of a sample, the binding post is connected with a stainless steel insulating clamp, the clamp clamps a test sample, the negative electrode is connected with the binding post of a stainless steel plate, the bottom end of the stainless steel plate is immersed in electrolytic corrosion liquid, electrolytic polishing is carried out for 10 seconds, and the surface of the test sample is silvery gray.
(6) And after electrolytic corrosion and electrolytic polishing are carried out on the sample to be tested, washing with deionized water, dripping absolute ethyl alcohol, and drying by using a blower to finish sample preparation.
(7) And (3) metallographic observation: and observing the corroded ferrite and austenite dissimilar steel welding joint sample interface by using a 10XB-PC type metallographic microscope to obtain a clear metallographic structure appearance.
As can be seen from FIG. 1, the parent material structures of T91 are both lath-shaped tempered martensite structures, and the sizes of crystal grains are relatively uniform; as can be seen from FIG. 2, the parent material structures of TP347H are all austenite structures, and are composed of polygonal crystal grains, and twin crystals are in the crystal grains; as can be seen from FIG. 3, the weld seams are both austenite and ferrite dual-phase structures, the austenite is in a dendritic form, and the ferrite is distributed along the dendrites. The corrosive liquid is used for preparing samples of the metallographic structures of the welded joints of the ferritic and austenitic dissimilar steels, can quickly and clearly display the metallographic structures of the welded joints of the dissimilar steels, and does not generate an excessive corrosion phenomenon.
Example 2:
most of them were the same as in example 1, except that in this example, the electrolysis in step (4) was changed to 45 seconds to 30 seconds.
Example 3:
most of them were the same as in example 1, except that in this example, the electrolysis in step (4) was changed to 45 seconds to 60 seconds.
Example 4:
compared with example 1, most of them are the same except that in this example, the electropolishing in step (5) for 10 seconds is changed to electropolishing for 5 seconds.
Example 5:
compared with example 1, most of them are the same except that in this example, the electropolishing in step (5) for 10 seconds is changed to electropolishing for 15 seconds.
Example 6:
most of them were the same as in example 1 except that in this example, the voltage for electropolishing in step (5) was changed to 40V to 50V.
Example 7:
most of them were the same as in example 1 except that in this example, the voltage for electropolishing in step (5) was changed to 40V to 45V.
Example 8:
compared with example 1, most of the results were the same except that in this example, 100ml of concentrated hydrochloric acid (37 wt%) in step (3) was changed to 80ml of concentrated hydrochloric acid (37 wt%).
Example 9:
compared with example 1, most of the results were the same except that in this example, 100ml of concentrated hydrochloric acid (37 wt%) in step (3) was changed to 90ml of concentrated hydrochloric acid (37 wt%).
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.

Claims (10)

1. The corrosive liquid for preparing the metallographic structure sample of the welded joint of the ferritic and austenitic dissimilar steel is characterized by comprising an electrolytic corrosive liquid and an electrolytic polishing liquid, wherein the electrolytic corrosive liquid comprises picric acid, sodium dodecyl benzene sulfonate and concentrated hydrochloric acid, the ratio of the picric acid to the sodium dodecyl benzene sulfonate to the concentrated hydrochloric acid is 20 g: 8 g: 80-100 ml, the electrolytic polishing liquid comprises alcohol, perchloric acid and glycerol, and the volume ratio of the alcohol to the perchloric acid to the glycerol is 150 ml: 50 ml: 25 ml.
2. The corrosive liquid for metallographic structure sample preparation of a welded joint of ferritic and austenitic steels according to claim 1, wherein said concentrated hydrochloric acid has a purity of 37 wt%, said alcohol has a purity of 95 vol%, said perchloric acid has a purity of 30 wt%, and said glycerol has a purity of 25 wt%.
3. An etching method for preparing samples of metallographic structures of welded joints of ferritic and austenitic dissimilar steels, characterized in that the method comprises the following steps:
(1) sampling a test sample at a welding joint of ferritic and austenitic dissimilar steels, and then pretreating the test sample to enable a surface to be observed to achieve a mirror surface effect, so as to obtain the test sample to be observed;
(2) taking a sample to be observed as an anode, a stainless steel plate as a cathode, and the electrolytic corrosion solution of claim 1 or 2 as an electrolyte, carrying out electrolysis, and then washing to obtain a corroded sample to be observed;
(3) taking the corroded sample to be observed as an anode, a stainless steel plate as a cathode, and the electrolytic polishing solution as defined in claim 1 or 2 as electrolyte, electrolyzing, washing, and blow-drying to obtain the finished sample.
4. The corrosion method for preparing a metallographic structure sample of a welded joint made of ferritic and austenitic steels according to claim 3, wherein in the step (1), the ferritic steel is T91 steel, and the austenitic steel is TP347H stainless steel.
5. The corrosion method for preparing the metallographic structure sample of the welded joint of ferritic and austenitic dissimilar steels according to claim 3, wherein in the step (1), the pretreatment process is as follows:
and washing, roughly grinding, finely grinding and polishing the sample until the observation surface of the sample achieves a mirror surface effect.
6. The corrosion method for preparing samples of metallographic structures of welded joints of ferritic and austenitic dissimilar steels according to claim 5, characterized in that the samples are coarsely ground using a grinder.
7. The corrosion method for preparing the metallographic structure sample of the welded joint of the ferritic and austenitic dissimilar steels according to claim 5, characterized in that the fine grinding process comprises:
and (3) carrying out fine grinding treatment on the surface of the roughly ground sample by using 400-mesh, 600-mesh, 800-mesh and 1200-mesh metallographic abrasive paper in sequence.
8. The corrosion method for preparing the metallographic structure sample of the welded joint of the ferritic and austenitic dissimilar steels according to claim 3, wherein in the step (2), the voltage is 12V, the temperature is 25 ℃, and the electrolysis time is 30-60 seconds.
9. The corrosion method for preparing the metallographic structure sample of the welded joint of the ferritic and austenitic dissimilar steels according to claim 3, wherein in the step (2), the voltage is 12V, the temperature is 25 ℃, and the electrolysis time is 45 seconds during the electrolysis.
10. The corrosion method for preparing the metallographic structure sample of the welded joint of the ferritic and austenitic dissimilar steels according to claim 3, wherein in the step (3), the voltage is 40-50V, the temperature is 25 ℃, and the electrolysis time is 5-15 seconds in the electrolysis process.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3287237A (en) * 1962-03-28 1966-11-22 Allegheny Ludlum Steel Surface treatment of bright annealed strip
JP2005241635A (en) * 2004-01-30 2005-09-08 Jfe Steel Kk Corrosive liquid for emergence of primary austenite grain boundary of steel material and method for making primary austenite grain boundary of steel material emerge
CN101025391A (en) * 2007-03-13 2007-08-29 北京科技大学 Method for making super-low carbon steel gold-phase sample and displaying its tissue
CN104729963A (en) * 2015-03-31 2015-06-24 常州天山重工机械有限公司 Detection and display method of austenite grains of quenched and tempered steel for gears at room temperature
CN106868578A (en) * 2017-01-25 2017-06-20 西北稀有金属材料研究院 A kind of beryllium material electrobrightening and the integral method of corrosion for EBSD tests
CN108004549A (en) * 2018-01-05 2018-05-08 华北电力科学研究院有限责任公司 The metallographic etchant and caustic solution of ferrite/austenite Dissimilar Steel Welded Joint

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3287237A (en) * 1962-03-28 1966-11-22 Allegheny Ludlum Steel Surface treatment of bright annealed strip
JP2005241635A (en) * 2004-01-30 2005-09-08 Jfe Steel Kk Corrosive liquid for emergence of primary austenite grain boundary of steel material and method for making primary austenite grain boundary of steel material emerge
CN101025391A (en) * 2007-03-13 2007-08-29 北京科技大学 Method for making super-low carbon steel gold-phase sample and displaying its tissue
CN104729963A (en) * 2015-03-31 2015-06-24 常州天山重工机械有限公司 Detection and display method of austenite grains of quenched and tempered steel for gears at room temperature
CN106868578A (en) * 2017-01-25 2017-06-20 西北稀有金属材料研究院 A kind of beryllium material electrobrightening and the integral method of corrosion for EBSD tests
CN108004549A (en) * 2018-01-05 2018-05-08 华北电力科学研究院有限责任公司 The metallographic etchant and caustic solution of ferrite/austenite Dissimilar Steel Welded Joint

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