CN116083909A - 9-12Cr series heat-resistant steel precipitated phase corrosive and display method - Google Patents

9-12Cr series heat-resistant steel precipitated phase corrosive and display method Download PDF

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CN116083909A
CN116083909A CN202211686445.0A CN202211686445A CN116083909A CN 116083909 A CN116083909 A CN 116083909A CN 202211686445 A CN202211686445 A CN 202211686445A CN 116083909 A CN116083909 A CN 116083909A
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precipitated phase
resistant steel
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王洪利
杜思敏
吴铖川
王婀娜
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Chengdu Advanced Metal Materials Industry Technology Research Institute Co Ltd
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    • G01MEASURING; TESTING
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract

The invention provides a 9-12Cr series heat-resistant steel precipitated phase corrosive and a display method, wherein the ratio of the dosage of ferric trichloride, hydrochloric acid and water in the corrosive is as follows: (2.0-2.5 g): (10-15 ml): 100ml; therefore, the corrosive agent specially suitable for clearly displaying the precipitated phase of the 9-12Cr series heat-resistant steel is successfully developed, and the 9-12Cr series heat-resistant steel corroded by the corrosive agent has high identification degree of the precipitated phase, and the corrosive agent has low toxicity to human bodies, simple and easily obtained components, low cost and easy preparation, so that the corrosive agent can be suitable for large-scale industrialized application; in addition, the method for displaying the precipitated phase of the 9-12Cr series heat-resistant steel provided by the invention has the advantages that the operation process is simple and convenient, the precipitated phase of the 9-12Cr series heat-resistant steel can be obviously displayed, and the quenched or tempered martensite structure is slightly displayed, so that the precipitated phase is very easy to distinguish from the quenched or tempered martensite structure, and an excellent distinguishing display effect is displayed, and the method is very suitable for industrial batch inspection and analysis of the precipitated phase in the 9-12Cr series heat-resistant steel.

Description

9-12Cr series heat-resistant steel precipitated phase corrosive and display method
Technical Field
The invention relates to the technical field of alloy precipitated phase display, in particular to a 9-12Cr series heat-resistant steel precipitated phase corrosive and a display method.
Background
The 9-12Cr series heat-resistant steel is ferrite heat-resistant steel with the mass percent of chromium element reaching 9-12 percent, and is mainly used for parts such as steam pipelines, blades, rotors and the like of power plants. The heat treatment process of the high Cr ferrite heat-resistant steel is quenching and high-temperature tempering, and the obtained typical structure is a precipitated phase of fine lath martensite plus dispersion distribution. The precipitated phases are mainly of two types, one is M 23 C 6 (M is a metal element such as chromium, iron, molybdenum, etc.); the other is MX (M is a metal element such as niobium, vanadium, thallium and the like, and X is a non-metal element such as carbon, nitrogen and the like). M is M 23 C 6 The size is generally 100-600 nm, and mainly precipitates on lath boundaries and grain boundaries, so that the interfaces are stabilized. The MX size is generally 20-80 nm, and is mainly distributed in the strip, so that the dislocation plays a strong role in pinning, dislocation slip is hindered, and the recovery rate of the matrix is reduced. M is attached with the progress of creep or improper forging process in the preparation process 23 C 6 Formed Laves phase such as Fe 2 (W, mo) and Z phase (mainly containing niobium and vanadium) formed by adhering to MX. These precipitated phases have a certain strengthening effect in the initial stage, but with the progress of creep, they grow up at a higher rate than MX and M 23 C 6 The precipitated phase is much larger, so that the strengthening effect is obviously weakened. At the same time, the precipitation of these phases also depletes MX and M 23 C 6 And thus ultimately affect the overall strengthening effect of the carbide.
The current corrosive for corroding the steel is usually saturated picric acid-alcohol solution, namely 5% -10% hydrochloric acid and saturated picric acid-alcohol mixed solution, and the microstructure display method is that the steel is corroded for 10 seconds to 1 minute. The microstructure displayed by the method has tempered martensite structure and precipitated phase, and the precipitated phase is not easy to distinguish and identify in the fine tempered martensite; and picric acid is an easy-to-explode chemical and is strictly controlled, so that picric acid is difficult to buy in the market at present. In the need of rapid detection of the microstructure of ferritic heat-resistant steels, there is a need to find new corrosive formulations to replace picric acid.
Patent application No. 202210471807.8 discloses a microscopic structure development observation method suitable for low-carbon medium alloy corrosion resistant steel. The corrosive agent is prepared by the following steps: the mass volume ratio of the ferric trichloride, the concentrated hydrochloric acid and the deionized water is as follows: 10g:60ml:100ml. The microscopic structure developing method comprises the following steps: soaking the prepared low-carbon medium-alloy corrosion-resistant steel in a container containing corrosive for 5s, flushing the surface corrosive with purified water, and drying the sample by adopting a blower. However, the microstructure displayed by the method has a tempered martensite structure and a precipitated phase, and the precipitated phase is not easy to distinguish and identify in the fine tempered martensite. In addition, no relevant papers or patent publications of corrosive agents or methods for developing precipitated phases in medium-low carbon ferrite heat-resistant steel are published at home and abroad.
Disclosure of Invention
The invention aims to provide a corrosive preparation method and a precipitated phase display method which are specially suitable for displaying a 9-12Cr series heat-resistant steel precipitated phase, and aims to solve the defects that the existing corrosive formula is difficult to distinguish and accurately identify tempered martensite structure and the precipitated phase in the developing process, and the corrosive preparation is simple and convenient, so that the corrosive preparation method is suitable for metallographic examination in a large-scale production process.
In order to achieve the aim, the invention provides a 9-12Cr series heat resistant steel precipitated phase corrosive,
the ratio of the dosage of the ferric trichloride, the hydrochloric acid and the water in the corrosive is as follows: (2.0-2.5 g): (10-15 ml): 100ml.
As a further improvement of the invention, the ferric trichloride is FeCl with the concentration of more than or equal to 99 percent 3 ·6H 2 O。
As a further improvement of the invention, the concentration of the hydrochloric acid is 36-38%.
As a further improvement of the present invention, the water is deionized water or tap water.
The invention also provides a 9-12Cr series heat-resistant steel precipitated phase display method, which comprises the following steps:
carrying out surface cleaning treatment on a 9-12Cr series heat-resistant steel metallographic specimen with a bright observation surface;
immersing the metallographic specimen after the cleaning treatment in the 9-12Cr series heat-resistant steel precipitated phase corrosive agent according to any one of claims 1 to 4 for 3 to 5 seconds;
washing the metallographic sample soaked with the corrosive agent by using an organic solvent, and then airing to obtain a sample to be observed;
and observing and photographing the sample to be observed by using a microscope, and completing the display of the precipitated phase.
As a further improvement of the present invention, the magnification of the microscope is 100 times to 500 times.
As a further improvement of the invention, the surface cleaning treatment of the 9-12Cr series heat resistant steel metallographic specimen with bright observation surface comprises the following steps:
and washing the observation surface of the metallographic specimen by water and alcohol in sequence, and then airing.
As a further improvement of the present invention, the organic solvent includes alcohol.
Compared with the prior art, the invention has at least the following beneficial effects:
the 9-12Cr series heat-resistant steel precipitated phase corrosive agent is a mixed solution formed by ferric chloride, hydrochloric acid and water, wherein the dosage ratio of the ferric chloride, the hydrochloric acid and the water is as follows: (2.0-2.5 g): (10-15 ml): 100ml; through the mode, the corrosive agent specially suitable for clearly displaying the precipitated phase of the 9-12Cr series heat-resistant steel is successfully developed, and the 9-12Cr series heat-resistant steel corroded by the corrosive agent has high identification degree of the precipitated phase, and the corrosive agent has low toxicity to human bodies, simple and easily obtained components, low cost and easy preparation, so that the corrosive agent can be suitable for large-scale industrialized application;
according to the 9-12Cr series heat-resistant steel precipitated phase display method provided by the invention, the surface cleaning treatment is carried out on the 9-12Cr series heat-resistant steel metallographic sample with a bright observation surface; then soaking the metallographic sample after the cleaning treatment in the prepared 9-12Cr series heat-resistant steel precipitated phase corrosive for 3-5 s; then washing the metallographic specimen soaked with the corrosive agent by using an organic solvent, and airing to obtain a specimen to be observed; finally, observing and photographing the sample to be observed by utilizing a microscope, thereby completing the display of the precipitated phase; the display method of the 9-12Cr series heat-resistant steel precipitated phase provided by the invention is simple and convenient in operation process, and has good distinguishing display effect on tempered martensite structure and the precipitated phase, so that the method is very suitable for industrial batch inspection and analysis of the precipitated phase in the 9-12Cr series heat-resistant steel.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention may be realized and attained by the method or steps of the invention as particularly pointed out in the written description and drawings.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions of the prior art, the following description will briefly explain the drawings used in the embodiments or the description of the prior art, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a morphology diagram of a tempered 10Cr11Co3W3NiMoVNbNB steel microstructure at 100 Xmagnification under a Zeiss optical microscope after 3s corrosion using the etchant formulation of example 1 of the present invention;
FIG. 2 is a morphology diagram of a tempered 10Cr11Co3W3NiMoVNbNB steel microstructure at 500 Xmagnification under a Zeiss optical microscope after 3s corrosion using the etchant formulation of example 1 of the present invention;
FIG. 3 is a morphology of a tempered 10Cr11Co3W3NiMoVNbNB steel microstructure of comparative example 1 after 8s corrosion using the etchant formulation of the present application, at 100 Xmagnification under a Zeiss optical microscope;
FIG. 4 is a morphology of a tempered 10Cr11Co3W3NiMoVNbNB steel microstructure after 8s corrosion using the etchant formulation of comparative example 1 at 500 Xmagnification under a Zeiss optical microscope;
FIG. 5 is a morphology of a tempered 10Cr11Co3W3NiMoVNbNB steel microstructure after 1s corrosion using the etchant formulation of comparative example 2 at 500 Xmagnification under a Zeiss optical microscope;
FIG. 6 is a morphology of a tempered 10Cr11Co3W3NiMoVNbNB steel microstructure after 5s corrosion using a prior art etchant formulation of comparative example 3 at 100 Xmagnification under a Zeiss optical microscope;
FIG. 7 is a morphology of a tempered 10Cr11Co3W3NiMoVNbNB steel microstructure after 5s corrosion using a prior art etchant formulation of comparative example 3 at 500 Xmagnification under a Zeiss optical microscope;
FIG. 8 is a morphology of a tempered 10Cr11Co3W3NiMoVNbNB steel microstructure after 3s corrosion using the etchant formulation of comparative example 4 at 500 Xmagnification under a Zeiss optical microscope;
FIG. 9 is a morphology of a tempered 10Cr11Co3W3NiMoVNbNB steel microstructure after 3s corrosion using the etchant formulation of comparative example 5 at 500 Xmagnification under a Zeiss optical microscope.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In order to solve the defects that the existing corrosive formulation is difficult to distinguish and accurately identify the tempered martensite structure and the precipitated phase in the developing process, the invention provides a preparation method and a corresponding display method of the corrosive suitable for displaying the 9-12Cr series heat-resistant steel precipitated phase, the 9-12Cr series heat-resistant steel corroded by the corrosive has high identification degree, and the configuration process of the corrosive is simple and convenient, so that the corrosive can be suitable for metallographic examination in the mass production process, and has wide application prospect.
Specifically, in order to achieve the above purpose, the invention provides a method suitable for displaying a 9-12Cr series heat-resistant steel precipitated phase, which comprises the following steps:
step 1: corrosive agent preparation
The precipitated phase corrosive is a mixed solution formed by ferric trichloride, hydrochloric acid and water; the ratio of the dosages of the ferric trichloride, the hydrochloric acid and the water is as follows: 2.0 to 2.5g: 10-15 ml:100ml, after the corrosive agent is prepared, filling into a brown bottle for standby;
step 2: sample preparation
Preparing 9-12Cr series heat-resistant steel which needs metallographic examination into a metallographic specimen with a bright observation surface, sequentially flushing with water and alcohol, and drying with a blower;
step 3: sample corrosion
Placing the prepared corrosive agent into a glass reaction vessel, opening a ventilation device, soaking the prepared 9-12Cr series heat-resistant steel metallographic sample in the vessel containing the corrosive agent for 3-5 s, flushing the surface corrosive agent with alcohol, and drying the sample by adopting a blower;
step 4: observation of
The corroded sample was observed and photographed by a zeiss microscope.
Furthermore, the ferric trichloride is FeCl3.6H2O with the concentration of more than or equal to 99 percent.
Further, the concentration of the hydrochloric acid is 36-38%.
Further, the water may be deionized water or tap water.
Further, the magnification of the Zeiss microscope is 100-500 times.
The invention successfully develops the corrosive agent specially suitable for clearly displaying the precipitated phase of the 9-12Cr series heat-resistant steel, and the 9-12Cr series heat-resistant steel corroded by the corrosive agent has high identification degree of the precipitated phase, and the corrosive agent has low toxicity to human bodies, simple and easily obtained components, low cost and easy preparation, so that the corrosive agent can be suitable for large-scale industrialized application. In addition, the method for displaying the precipitated phase of the 9-12Cr series heat-resistant steel provided by the invention has the advantages of simple and convenient operation process, good distinguishing and displaying effect on tempered martensite structure and the precipitated phase, and is very suitable for industrial batch inspection and analysis of the precipitated phase in the 9-12Cr series heat-resistant steel.
In order to better facilitate the understanding of the present invention by the skilled person, the technical solutions provided by the present invention will be more clearly and completely described below by taking tempered 10Cr11Co3W3 nimocnbnb steel as an example, in combination with specific examples and comparative examples, and it is obvious that the described examples are only some examples of the present invention, but not all examples. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides a 9-12Cr series heat-resistant steel precipitated phase corrosive and a related display method thereof, which comprises the following specific steps:
step 1: corrosive agent preparation
The precipitated phase corrosive is a mixed solution formed by ferric trichloride, hydrochloric acid and water; the ratio of the dosages of the ferric trichloride, the hydrochloric acid and the water is as follows: 2.5g:10ml:100ml, after the corrosive agent is prepared, filling into a brown bottle for standby; wherein, the liquid crystal display device comprises a liquid crystal display device,
the ferric trichloride is FeCl with the concentration of more than or equal to 99 percent 3 ·6H 2 O。
The concentration of the hydrochloric acid is 37%.
The water is tap water.
Step 2: sample preparation
Preparing 10Cr11Co3W3NiMoVNbNB heat-resistant steel to be subjected to metallographic examination into a metallographic specimen with a bright observation surface, sequentially flushing with water and alcohol, and drying with a blower;
step 3: sample corrosion
Placing the prepared corrosive agent into a glass reaction vessel, opening a ventilation device, soaking the prepared 10Cr11Co3W3NiMoVNbNB heat-resistant steel metallographic sample in the vessel containing the corrosive agent for 3s, flushing the surface corrosive agent with alcohol, and drying the sample by adopting a blower;
step 4: observation of
And (3) observing and photographing the corroded sample by using a Zeiss microscope, wherein the amplification factors of the Zeiss microscope are respectively set to 100 times and 500 times, and the morphology of the precipitated phase is shown in figures 1 and 2.
The difference between tempered martensite structure and the precipitated phase is very clearly seen in fig. 1 and 2, wherein the dark particle strings within the black circles in both figures are the precipitated phase. Therefore, the method provided by the invention has good precipitated phase display effect.
Comparative example 1
The comparative example provides a 9-12Cr series heat resistant steel precipitated phase corrosive and a related display method thereof, and the specific steps are as follows:
step 1: corrosive agent preparation
The precipitated phase corrosive is a mixed solution formed by ferric trichloride, concentrated hydrochloric acid and water; the ratio of the dosages of the ferric trichloride, the hydrochloric acid and the water is as follows: 2.5g:10ml:100ml, after the corrosive agent is prepared, filling into a brown bottle for standby; wherein, the liquid crystal display device comprises a liquid crystal display device,
the ferric trichloride is FeCl with the concentration of more than or equal to 99 percent 3 ·6H 2 O。
The concentration of the hydrochloric acid is 37%.
The water is tap water.
Step 2: sample preparation
Preparing 10Cr11Co3W3NiMoVNbNB heat-resistant steel to be subjected to metallographic examination into a metallographic specimen with a bright observation surface, sequentially flushing with water and alcohol, and drying with a blower;
step 3: sample corrosion
Placing the prepared corrosive agent into a glass reaction vessel, opening a ventilation device, soaking the prepared 10Cr11Co3W3NiMoVNbNB heat-resistant steel metallographic sample in the vessel containing the corrosive agent for 8s, flushing the surface corrosive agent with alcohol, and drying the sample by adopting a blower;
step 4: observation of
And (3) observing and photographing the corroded sample by using a Zeiss microscope, wherein the magnification of the Zeiss microscope is respectively set to 100 times and 500 times, and the microstructure morphology is shown in figures 3 and 4.
It can be seen from fig. 3 and 4 that once the etching time is prolonged, even if it is only 8 seconds, it is difficult to clearly distinguish tempered martensite structure from precipitated phases under a microscope, so that it is important to control the etching time suitable for the etchant in order to achieve a good precipitated phase display effect by the display method provided by the present invention.
Comparative example 2
The comparative example provides a 9-12Cr series heat resistant steel precipitated phase corrosive and a related display method thereof, and the specific steps are as follows:
step 1: corrosive agent preparation
The precipitated phase corrosive is a mixed solution formed by ferric trichloride, concentrated hydrochloric acid and water; the ratio of the dosages of the ferric trichloride, the hydrochloric acid and the water is as follows: 2.5g:10ml:100ml, after the corrosive agent is prepared, filling into a brown bottle for standby; wherein, the liquid crystal display device comprises a liquid crystal display device,
the ferric trichloride is FeCl with the concentration of more than or equal to 99 percent 3 ·6H 2 O。
The concentration of the hydrochloric acid is 37%.
The water is tap water.
Step 2: sample preparation
Preparing 10Cr11Co3W3NiMoVNbNB heat-resistant steel to be subjected to metallographic examination into a metallographic specimen with a bright observation surface, sequentially flushing with water and alcohol, and drying with a blower;
step 3: sample corrosion
Placing the prepared corrosive agent into a glass reaction vessel, opening a ventilation device, soaking the prepared 10Cr11Co3W3NiMoVNbNB heat-resistant steel metallographic sample in the vessel containing the corrosive agent for 1s, flushing the surface corrosive agent with alcohol, and drying the sample by adopting a blower;
step 4: observation of
The corroded sample was observed and photographed by a zeiss microscope, the magnification of which was set to 500 times, and the microstructure morphology is shown in fig. 5.
As can be seen from FIG. 5, the etching time is shortened to 1s, and it is also difficult to clearly distinguish the tempered martensite structure from the precipitated phase under a microscope, so that it is necessary to control the etching time of the etchant to 3-5 s, which proves that the display method provided by the invention is intended to achieve a good display effect of the precipitated phase.
Comparative example 3
The microstructure of the 9-12Cr series tempered 10Cr11Co3W3NiMoVNbNB heat resistant steel was also observed for the precipitated phase by the closest prior art method (patent application No. 202210471807.8), and the specific steps are as follows:
step 1: corrosive agent preparation
The precipitated phase corrosive is ferric trichloride, concentrated hydrochloric acid and deionized water, and the mass volume ratio is as follows: 10g:60ml:100ml. After the corrosive agent is prepared, filling the mixture into a brown bottle for standby;
wherein the concentration of the hydrochloric acid is 37%.
Step 2: sample preparation
The 10Cr11Co3W3NiMoVNbNB heat-resistant steel used in example 1 was prepared again into a metallographic specimen with a bright observation surface, and was rinsed with water and alcohol in sequence and dried with a blower;
step 3: sample corrosion
Placing the prepared corrosive agent into a glass reaction vessel, opening a ventilation device, soaking the prepared 10Cr11Co3W3NiMoVNbNB heat-resistant steel metallographic sample in the vessel containing the corrosive agent for 5s, washing the surface corrosive agent with purified water, and drying the sample by adopting a blower;
step 4: observation of
The corroded sample is observed and photographed by a Zeiss microscope, the magnification of the Zeiss microscope is respectively set to be 100 times and 500 times, and the microstructure morphology is shown in fig. 6 and 7.
It can be seen from fig. 6, 7 that the use of the formulation provided in the closest prior art does not allow a clear differentiation of tempered martensitic structure and precipitated phases under a microscope.
Comparative example 4
The comparative example provides a 9-12Cr series heat resistant steel precipitated phase corrosive and a related display method thereof, and the specific steps are as follows:
step 1: corrosive agent preparation
The precipitated phase corrosive is a mixed solution formed by ferric trichloride, hydrochloric acid and water; the ratio of the dosages of the ferric trichloride, the hydrochloric acid and the water is as follows: 2.5g:20ml:100ml, after the corrosive agent is prepared, filling into a brown bottle for standby; wherein, the liquid crystal display device comprises a liquid crystal display device,
the ferric trichloride is FeCl with the concentration of more than or equal to 99 percent 3 ·6H 2 O。
The concentration of the hydrochloric acid is 37%.
The water is tap water.
Step 2: sample preparation
Preparing 10Cr11Co3W3NiMoVNbNB heat-resistant steel to be subjected to metallographic examination into a metallographic specimen with a bright observation surface, sequentially flushing with water and alcohol, and drying with a blower;
step 3: sample corrosion
Placing the prepared corrosive agent into a glass reaction vessel, opening a ventilation device, soaking the prepared 10Cr11Co3W3NiMoVNbNB heat-resistant steel metallographic sample in the vessel containing the corrosive agent for 3s, flushing the surface corrosive agent with alcohol, and drying the sample by adopting a blower;
step 4: observation of
The corroded sample is observed and photographed by a Zeiss microscope, the amplification factor of the Zeiss microscope is set to be 500 times, and the morphology of the precipitated phase is shown in figure 8.
It can be seen from fig. 8 that once the amount of hydrochloric acid in the formulation is increased, the difference between tempered martensite structure and precipitated phase in the micrograph becomes no longer apparent, and thus it is necessary to control the amount of hydrochloric acid in the etchant formulation in order to achieve good indication of the precipitated phase.
Comparative example 5
The comparative example provides a 9-12Cr series heat resistant steel precipitated phase corrosive and a related display method thereof, and the specific steps are as follows:
step 1: corrosive agent preparation
The precipitated phase corrosive is a mixed solution formed by ferric trichloride, hydrochloric acid and water; the ratio of the dosages of the ferric trichloride, the hydrochloric acid and the water is as follows: 3g:10ml:100ml, after the corrosive agent is prepared, filling into a brown bottle for standby; wherein, the liquid crystal display device comprises a liquid crystal display device,
the ferric trichloride is FeCl with the concentration of more than or equal to 99 percent 3 ·6H 2 O。
The concentration of the hydrochloric acid is 37%.
The water is tap water.
Step 2: sample preparation
Preparing 10Cr11Co3W3NiMoVNbNB heat-resistant steel to be subjected to metallographic examination into a metallographic specimen with a bright observation surface, sequentially flushing with water and alcohol, and drying with a blower;
step 3: sample corrosion
Placing the prepared corrosive agent into a glass reaction vessel, opening a ventilation device, soaking the prepared 10Cr11Co3W3NiMoVNbNB heat-resistant steel metallographic sample in the vessel containing the corrosive agent for 3s, flushing the surface corrosive agent with alcohol, and drying the sample by adopting a blower;
step 4: observation of
The corroded sample was observed and photographed by a zeiss microscope, the magnification of which was set to 500 times, and the morphology of the precipitated phase was shown in fig. 9.
It can be seen from fig. 9 that once the usage ratio of ferric trichloride in the formulation is increased, the difference between tempered martensitic structure and precipitated phase in the micrograph becomes no longer obvious, thereby further explaining that to achieve the technical effect of clearly showing the precipitated phase, it is important to control the relative usage concentration of ferric trichloride and hydrochloric acid in the etchant formulation.
In summary, the 9-12Cr series heat resistant steel precipitated phase corrosive provided by the invention is a mixed solution formed by ferric trichloride, hydrochloric acid and water, wherein the dosage ratio of the ferric trichloride, the hydrochloric acid and the water is as follows: (2.0-2.5 g): (10-15 ml): 100ml; through the mode, the corrosive agent specially suitable for clearly displaying the precipitated phase of the 9-12Cr series heat-resistant steel is successfully developed, and the 9-12Cr series heat-resistant steel corroded by the corrosive agent has high identification degree of the precipitated phase, and the corrosive agent has low toxicity to human bodies, simple and easily obtained components, low cost and easy preparation, so that the corrosive agent can be suitable for large-scale industrialized application; in addition, the 9-12Cr series heat-resistant steel precipitated phase display method provided by the invention carries out surface cleaning treatment on the 9-12Cr series heat-resistant steel metallographic sample with a bright observation surface; then soaking the metallographic sample after the cleaning treatment in the prepared 9-12Cr series heat-resistant steel precipitated phase corrosive for 3-5 s; then washing the metallographic specimen soaked with the corrosive agent by using an organic solvent, and airing to obtain a specimen to be observed; finally, observing and photographing the sample to be observed by utilizing a microscope, thereby completing the display of the precipitated phase; the display method of the 9-12Cr series heat-resistant steel precipitated phase provided by the invention has the advantages that the operation process is simple and convenient, the distinguishing display effect on the tempered martensite structure and the precipitated phase is good, the precipitated phase of the 9-12Cr series heat-resistant steel can be obviously displayed, and the quenched or tempered martensite structure is slightly displayed, so that the precipitated phase is very easy to distinguish from the quenched or tempered martensite structure, and the method is very suitable for industrial batch inspection and analysis of the precipitated phase in the 9-12Cr series heat-resistant steel.
Finally, it should be noted that: the foregoing description is only illustrative of the preferred embodiments of the present invention, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described, or equivalents may be substituted for elements thereof, and any modifications, equivalents, improvements or changes may be made without departing from the spirit and principles of the present invention.

Claims (8)

1. A9-12 Cr series heat-resistant steel precipitated phase corrosive agent is characterized in that,
the ratio of the dosage of the ferric trichloride, the hydrochloric acid and the water in the corrosive is as follows: (2.0-2.5 g): (10-15 ml): 100ml.
2. The 9-12Cr series heat resistant steel precipitated phase etchant according to claim 1, wherein,
the ferric trichloride is FeCl with the concentration of more than or equal to 99 percent 3 ·6H 2 O。
3. The 9-12Cr series heat resistant steel precipitated phase etchant according to claim 1, wherein,
the concentration of the hydrochloric acid is 36-38%.
4. The 9-12Cr series heat resistant steel precipitated phase etchant according to claim 1, wherein,
the water is deionized water or tap water.
5. A method for displaying a 9-12Cr series heat-resistant steel precipitated phase, the method comprising:
carrying out surface cleaning treatment on a 9-12Cr series heat-resistant steel metallographic specimen with a bright observation surface;
immersing the metallographic specimen after the cleaning treatment in the 9-12Cr series heat-resistant steel precipitated phase corrosive agent according to any one of claims 1 to 4 for 3 to 5 seconds;
washing the metallographic sample soaked with the corrosive agent by using an organic solvent, and then airing to obtain a sample to be observed;
and observing and photographing the sample to be observed by using a microscope, and completing the display of the precipitated phase.
6. The method for displaying a precipitated phase of a 9-12Cr series heat resistant steel according to claim 5, wherein,
the magnification of the microscope is 100-500 times.
7. The method for displaying a precipitated phase of 9-12 Cr-series heat-resistant steel according to claim 5 or 6, wherein the surface cleaning treatment of the 9-12 Cr-series heat-resistant steel metallographic specimen with a bright observation surface comprises:
and washing the observation surface of the metallographic specimen by water and alcohol in sequence, and then airing.
8. The method for displaying a precipitated phase of a 9-12Cr series heat resistant steel according to claim 5, wherein,
the organic solvent comprises alcohol.
CN202211686445.0A 2022-12-27 2022-12-27 9-12Cr series heat-resistant steel precipitated phase corrosive and display method Pending CN116083909A (en)

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Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU1425252A1 (en) * 1985-09-30 1988-09-23 Предприятие П/Я Г-4517 Agent for detecting macroflaws
SU1691719A1 (en) * 1989-08-28 1991-11-15 Камское объединение по производству большегрузных автомобилей "КамАЗ" Method of revealing austenite grain
JPH0943230A (en) * 1995-07-31 1997-02-14 Kawasaki Steel Corp Corrosion liquid for old austenite grain boundary appearance of steel and exhibition method with the use of it
CN102517586A (en) * 2011-12-26 2012-06-27 上海锅炉厂有限公司 Corrosive agent for displaying 9% Cr steel original austenite grain boundary and application thereof
CN104359743A (en) * 2014-11-18 2015-02-18 天津理工大学 Special solution for corrosion of metallographic phase of high-Cr ferritic heat-resistant steel, as well as preparation method of solution
CN107574439A (en) * 2017-08-23 2018-01-12 华能国际电力股份有限公司 Etching agent for displaying original austenite grain boundary of FB2 steel, preparation method and application
CN108004548A (en) * 2017-12-06 2018-05-08 国网山东省电力公司电力科学研究院 HR3C steel microscopic structures corrosion liquid making method and application after being on active service 50,000 hours
CN109468640A (en) * 2018-11-26 2019-03-15 抚顺特殊钢股份有限公司 A kind of SNCrW stainless steel metallographic etchant and its preparation method and application method
CN110068492A (en) * 2018-01-24 2019-07-30 宝山钢铁股份有限公司 A kind of metallographic etching agent and its application method for the dyeing of advanced high-strength steel retained austenite
CN111504753A (en) * 2020-06-11 2020-08-07 中国航发成都发动机有限公司 General corrosive agent and corrosion method for gamma' phase and depletion layer metallographic structure of corrosion-resistant high-temperature alloy
CN112284860A (en) * 2020-09-11 2021-01-29 河钢股份有限公司 Etching agent for displaying austenitic structure of heat-resistant steel for air valve and using method
CN113008639A (en) * 2021-04-22 2021-06-22 浙江泰富无缝钢管有限公司 Display method of P91 and P92 steel original austenite grain boundary
CN114295456A (en) * 2021-12-03 2022-04-08 四川工程职业技术学院 GH4169 high-temperature alloy grain corrosive agent and application thereof
CN114858565A (en) * 2022-04-29 2022-08-05 包头钢铁(集团)有限责任公司 Microscopic structure development observation method suitable for low-carbon medium-alloy corrosion-resistant steel

Patent Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU1425252A1 (en) * 1985-09-30 1988-09-23 Предприятие П/Я Г-4517 Agent for detecting macroflaws
SU1691719A1 (en) * 1989-08-28 1991-11-15 Камское объединение по производству большегрузных автомобилей "КамАЗ" Method of revealing austenite grain
JPH0943230A (en) * 1995-07-31 1997-02-14 Kawasaki Steel Corp Corrosion liquid for old austenite grain boundary appearance of steel and exhibition method with the use of it
CN102517586A (en) * 2011-12-26 2012-06-27 上海锅炉厂有限公司 Corrosive agent for displaying 9% Cr steel original austenite grain boundary and application thereof
CN104359743A (en) * 2014-11-18 2015-02-18 天津理工大学 Special solution for corrosion of metallographic phase of high-Cr ferritic heat-resistant steel, as well as preparation method of solution
CN107574439A (en) * 2017-08-23 2018-01-12 华能国际电力股份有限公司 Etching agent for displaying original austenite grain boundary of FB2 steel, preparation method and application
CN108004548A (en) * 2017-12-06 2018-05-08 国网山东省电力公司电力科学研究院 HR3C steel microscopic structures corrosion liquid making method and application after being on active service 50,000 hours
CN110068492A (en) * 2018-01-24 2019-07-30 宝山钢铁股份有限公司 A kind of metallographic etching agent and its application method for the dyeing of advanced high-strength steel retained austenite
CN109468640A (en) * 2018-11-26 2019-03-15 抚顺特殊钢股份有限公司 A kind of SNCrW stainless steel metallographic etchant and its preparation method and application method
CN111504753A (en) * 2020-06-11 2020-08-07 中国航发成都发动机有限公司 General corrosive agent and corrosion method for gamma' phase and depletion layer metallographic structure of corrosion-resistant high-temperature alloy
CN112284860A (en) * 2020-09-11 2021-01-29 河钢股份有限公司 Etching agent for displaying austenitic structure of heat-resistant steel for air valve and using method
CN113008639A (en) * 2021-04-22 2021-06-22 浙江泰富无缝钢管有限公司 Display method of P91 and P92 steel original austenite grain boundary
CN114295456A (en) * 2021-12-03 2022-04-08 四川工程职业技术学院 GH4169 high-temperature alloy grain corrosive agent and application thereof
CN114858565A (en) * 2022-04-29 2022-08-05 包头钢铁(集团)有限责任公司 Microscopic structure development observation method suitable for low-carbon medium-alloy corrosion-resistant steel

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
尹衍成;王涛;李珊珊;李桂英: "亚共析钢C72D2奥氏体晶粒度腐蚀剂的选用", 物理测试, no. 005, 31 December 2019 (2019-12-31) *
朱剑: "FeCl3-HCl-H2O体系浸出低冰镍界面氧化反应和第一性原理计算", 中国有色金属学报, vol. 30, no. 11, 28 November 2020 (2020-11-28) *
魏建忠;马捷;宗斌;: "Cr35Ni45型失效裂解炉管金相试样的制备与显示方法", 理化检验(物理分册), no. 03, 8 March 2013 (2013-03-08) *

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