CN109187152B - Corrosive agent for displaying heat-resistant steel original austenite grain boundary and display method - Google Patents
Corrosive agent for displaying heat-resistant steel original austenite grain boundary and display method Download PDFInfo
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- CN109187152B CN109187152B CN201811031640.3A CN201811031640A CN109187152B CN 109187152 B CN109187152 B CN 109187152B CN 201811031640 A CN201811031640 A CN 201811031640A CN 109187152 B CN109187152 B CN 109187152B
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- G—PHYSICS
- G01—MEASURING; TESTING
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- 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
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention relates to a corrosive agent for displaying the original austenite grain boundary of heat-resistant steel and a display method, belongs to the technical field of metallographic sample preparation, and solves the problems that the original austenite grain boundary of heat-resistant steel is not clearly displayed and the display method is complicated in the prior art. The corrosive agent in the application consists of potassium permanganate, concentrated sulfuric acid and distilled water; the display method comprises the following steps: s1, preparing, grinding and polishing a sample, S2, preparing a corrosive and chemically corroding, and S3, observing an original austenite crystal boundary. The method can quickly and simply display the original austenite grain boundary of the heat-resistant steel, judge whether the problem of coarse grains exists in the heat-resistant steel through analysis, further deduce the performance of the heat-resistant steel, and provide an important basis for establishing a production process.
Description
Technical Field
The invention relates to the technical field of metallographic sample preparation, in particular to a corrosive agent for displaying the original austenite grain boundary of heat-resistant steel and a display method.
Background
The heat-resistant steel is widely used in ultra-supercritical steam turbines, boilers and cylinder bodies, and has high use temperature and strict performance requirements, and the original austenite grains and the uniformity thereof directly influence various performances of the steel, such as performance indexes of strength, toughness, oxidation resistance, fatigue life and the like of the steel, and the coarse austenite grains often cause the material to obtain a coarse structure after being cooled, so that the material has low toughness and plasticity, and the comprehensive mechanical properties of the material are greatly reduced. Therefore, the grain boundary display technology is indispensable work in the production research process of steel. The heat-resistant steel has strict requirements on grain size, so that the display technology of the prior austenite grain boundary of the ferrite heat-resistant steel is particularly important, and the display technology has important significance for judging the structure evolution, the performance, the heat treatment process and the like of the material.
In view of the great influence of ferrite heat-resistant steel original austenite grains on material performance, the problem of displaying original austenite grain boundaries is always a key point and a difficult point. The method has certain effect on carbon steel and quenched and tempered steel with uniform grain structure and low alloy element content, but the original austenite grain boundary of ferrite heat-resistant steel with high alloy element content and non-uniform grain structure is difficult to clearly and completely show, so that the measurement accuracy of the original austenite grain size is influenced, and the quality control of the material is not facilitated.
In the case of ferritic heat-resistant steel, when grains are corroded by a conventional corrosion method, a martensite structure is easy to appear, corroded grain boundaries are easy to be covered by an intragranular structure, the grain boundaries are difficult to appear, and the original austenite grain boundaries of the ferritic heat-resistant steel are shown to be a problem recognized in the industry. The prior art exists the following methods: (1) the precipitates are aggregated near the grain boundaries by adopting a heat treatment method to display the grain boundaries, but the method needs to carry out heat treatment on the sample, and is troublesome and time-consuming; (2) the corroded sample is lightly polished by an electrolytic corrosion method to display a grain boundary, but the electrolytic corrosion method has high requirements on equipment; (3) the sample is corroded for 2 hours by heating the corrosive under the condition that the corrosive is boiled, but the corrosion condition is harsh and the corrosion time is long. Although these corrosion methods can exhibit prior austenite grain boundaries, they are complicated to operate, have high demands on operators, and are not suitable for large-scale industrial applications.
Disclosure of Invention
In view of the above analysis, the present invention aims to provide a corrosive agent for displaying the prior austenite grain boundary of heat-resistant steel and a display method thereof, so as to solve the problems that the existing display method is complex in operation, unclear in displaying the grain boundary, high in requirement on operators, and not beneficial to large-scale industrial application.
In the prior art, the corrosive agent consisting of potassium permanganate, concentrated sulfuric acid and distilled water is only used for displaying the original austenite crystal boundary of 40Cr15Mo2VN bearing steel and is different from the type of the steel suitable for the invention; the corrosive agent containing the components is not adopted in the field of heat-resistant steel, a picric acid solution is generally selected for corrosion of the heat-resistant steel in the prior art, and the corrosive agent has harsh corrosion conditions and poor corrosion effect when the heat-resistant steel is corroded; the invention creatively discovers that when the corrosive agent consisting of potassium permanganate, concentrated sulfuric acid and distilled water is used for corroding the 13Cr9Mo2Co1NiVNbNB steel in the application, the corrosion process is simple and convenient, the corrosion effect is good, and the original austenite grain boundary can be clearly displayed. In addition, the proportion of the corrosive in the prior art is 2g of potassium permanganate, 4ml of concentrated sulfuric acid with the mass fraction of 98% and 96ml of distilled water, and the original austenite crystal boundary of the heat-resistant steel cannot be clearly displayed by corrosion of the corrosive in the proportion.
The purpose of the invention is mainly realized by the following technical scheme:
an etching agent for displaying the prior austenite grain boundary of heat-resistant steel, wherein each 1L of the etching agent comprises: 8-12 g of potassium permanganate, 100-150 ml of 98% concentrated sulfuric acid and 850-900 ml of distilled water;
the heat-resistant steel is 13Cr9Mo2Co1NiVNbNB steel.
The corrosive agent is prepared by simple proportioning of sulfuric acid, potassium permanganate and distilled water, the preparation process is simple and convenient, compared with other corrosive agents, the corrosive agent has good corrosion effect on 13Cr9Mo2Co1NiVNbNB heat-resistant steel, and simultaneously compared with an electrolytic corrosion method in the prior art, the corrosive agent has low requirement on equipment and can be industrially applied in a large scale.
Further, each 1L of the etchant comprises: 8g of potassium permanganate, 100ml of concentrated sulfuric acid with the mass fraction of 98 percent and 900ml of distilled water.
Further, each 1L of the etchant comprises: 12g of potassium permanganate, 100ml of concentrated sulfuric acid with the mass fraction of 98 percent and 900ml of distilled water.
The invention also provides a method for displaying the original austenite grain boundary of the heat-resistant steel, which comprises the following steps:
s1, preparing, grinding and polishing a sample;
s2, preparing a corrosive agent and chemically corroding the sample;
and S3, observing the original austenite grain boundary of the heat-resistant steel.
Further, the preparation of the sample was: cutting a metallographic specimen by a cutting machine; the grinding of the sample was: grinding a sample by using 180-mesh 1200-mesh silicon carbide waterproof abrasive paper, wherein the rotating speed of a grinding disc is 300-mesh 600rpm, rotating the sample by 90 degrees along the grinding surface when the abrasive paper is replaced each time, and using distilled water as a lubricant in the grinding process; the polishing of the test specimens was: polishing by using a diamond particle suspending agent until the interface is smooth, no scratch and no stain are generated, and then washing the polished surface by using clear water and alcohol and drying.
Further, the particle size of the diamond particle suspending agent includes 2.5 μm and 1.0 μm.
Further, in step S2, the etchant is formulated as: weighing 0.8-1.0 g of potassium permanganate, pouring the potassium permanganate into a beaker filled with 85 ml-90 ml of distilled water, adding 10-15 ml of 98% concentrated sulfuric acid, uniformly stirring, and standing for later use.
Further, in step S2, the chemically etching the sample includes: 1) putting the prepared corrosive into a water bath kettle for heating, and uniformly stirring the solution in the heating process; 2) after the sample is heated to 65-70 ℃ and the temperature is constant, putting the sample into the corrosive agent with the polished surface facing upwards; 3) and taking out the sample after 20-30 minutes, then soaking and washing the sample in an oxalic acid solution for 5-10 seconds, then taking out the sample, slightly wiping the surface of the sample with absorbent cotton under distilled water, washing the surface with alcohol, and then drying the sample by blowing.
The corrosive agent is adopted, the original austenite grain boundary of the 13Cr9Mo2Co1NiVNbNB heat-resistant steel can be completely displayed through water bath heating, the original grain size and the grain size can be conveniently and accurately measured, and powerful support is provided for formulation and optimization of the production process of the material.
Further, in the step S3, the sample is placed on a metallographic microscope for observation, and a metallographic picture of the sample is taken.
The invention has the following beneficial effects:
(1) the corrosive agent used by the invention has the advantages of easily available raw materials, simple preparation, economy and practicability, and can be industrially applied in a large scale;
(2) the display method disclosed by the invention is simple and convenient to operate, the sample does not need to be repeatedly and lightly polished, soaked or wiped in the corrosion process, and the original austenite grain boundary of the 13Cr9Mo2Co1NiVNbNB heat-resistant cast steel can be clearly displayed;
(3) the display method of the invention quickly and simply displays the grain size of the original austenite of the 13Cr9Mo2Co1NiVNbNB heat-resistant steel in actual production, judges whether the problem of coarse grains exists in the heat-resistant steel through analysis, further infers the performance of the heat-resistant steel, and provides an important basis for establishing a production process.
In the invention, the technical schemes can be combined with each other to realize more preferable combination schemes. 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 will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
Drawings
The drawings are only for purposes of illustrating particular embodiments and are not to be construed as limiting the invention, wherein like reference numerals are used to designate like parts throughout.
FIG. 1 is a graph showing prior austenite grain boundaries of 13Cr9Mo2Co1NiVNbNB heat-resistant steel in example 1;
FIG. 2 is a graph showing prior austenite grain boundaries of 13Cr9Mo2Co1NiVNbNB heat-resistant steel in example 2;
FIG. 3 is a graph showing prior austenite grain boundaries of 13Cr9Mo2Co1NiVNbNB heat-resistant steel in comparative example 1;
FIG. 4 is a graph showing prior austenite grain boundaries of 13Cr9Mo2Co1NiVNbNB heat-resistant steel when a supersaturated picric acid aqueous solution is used as a corrosive agent;
FIG. 5 is a graph showing prior austenite grain boundaries of 13Cr9Mo2Co1NiVNbNB heat-resistant steel when picric acid alcohol hydrochloride solution is used as a corrosive agent.
Detailed Description
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate preferred embodiments of the invention and together with the description, serve to explain the principles of the invention and not to limit the scope of the invention.
All of the starting materials of the present invention, without particular limitation as to their source, may be purchased commercially or prepared according to conventional methods well known to those skilled in the art.
All the raw materials of the present invention are not particularly limited in their purity, and analytical purification is preferably employed in the present invention.
Example 1
The corrosive in the embodiment comprises the following components: 1.2g of potassium permanganate, 10ml of concentrated sulfuric acid with the mass fraction of 98 percent and 90ml of distilled water.
In this embodiment, a method for displaying the prior austenite grain boundary of heat-resistant steel includes the following steps:
s1, preparing, grinding and polishing a sample;
the method comprises the following steps:
a. preparation of a sample: cutting a metallographic specimen with the size of 10 multiplied by 20mm from 13Cr9Mo2Co1NiVNbNB steel by a wire electric discharge machine;
b. grinding of the sample: grinding a sample by using 180-mesh, 400-mesh, 600-mesh, 800-mesh, 1000-mesh and 1200-mesh silicon carbide waterproof abrasive paper in sequence, setting the rotation speed of a grinding disc to be 300-mesh 600rpm, rotating the sample by 90 degrees along the grinding surface when replacing the next-pass abrasive paper each time, enabling the grinding mark of a new pass to be vertical to the grinding mark of a previous pass until the grinding mark is covered, and replacing the abrasive paper in sequence until the silicon carbide waterproof abrasive paper of 1200-mesh is ground, wherein distilled water is used as a lubricating agent in the grinding process;
c. polishing of the sample: and (3) polishing the ground sample on a polishing machine by sequentially using diamond particle suspending agents with the particle size of a polishing agent of 2.5 microns and 1.0 micron until the interface is smooth and has no scratch or stain, washing the polished surface by using clean water and alcohol, and drying by using a blower.
S2, preparing a corrosive agent and chemically corroding the sample;
the method comprises the following steps:
a. preparation of a corrosive agent: weighing 1.2g of potassium permanganate by using a balance, pouring the potassium permanganate into a beaker filled with 90ml of distilled water, adding 10ml of concentrated sulfuric acid with the mass fraction of 98 percent measured by using a measuring cylinder, uniformly stirring, and standing for later use;
b. chemical corrosion: the prepared corrosive agent is put into a water bath pot for heating, a glass rod is used for uniformly stirring the solution in the heating process, after the temperature is heated to 70 ℃ and is constant, the polished surface of the sample is upward and is clamped by a pair of tweezers to be put into the corrosive agent, the sample is taken out after being corroded in the constant-temperature solution for 20 minutes, then the sample is put into an oxalic acid solution for immersion cleaning for 5 seconds, impurities on the corroded surface are removed, then the sample is taken out, absorbent cotton is used for slightly wiping the surface of the sample under distilled water, the surface is washed by alcohol, and then a blower is used for drying and drying the sample to be observed.
S3, observing the prior austenite grain boundary of the heat-resistant steel;
the method comprises the following steps: the sample is placed on a metallographic microscope for observation, and a metallographic picture of the sample is taken by 50 times, so that the original austenite grain boundary of the 13Cr9Mo2Co1NiVNbNB heat-resistant steel is shown in figure 1.
In the original austenite grain boundary diagram of the 13Cr9Mo2Co1NiVNbNB heat-resistant steel shown in the example 1, the grain boundaries are clear and complete and are in an approximate grid shape.
Example 2
The difference between the embodiment and the embodiment 1 is that the etchant has different components, specifically: 0.8g of potassium permanganate, 10ml of concentrated sulfuric acid with the mass fraction of 98 percent and 90ml of distilled water.
The other display method steps in example 2 are the same as in example 1.
The prior austenite grain boundaries of the 13Cr9Mo2Co1NiVNbNB heat-resistant steel shown in example 2 are shown in FIG. 2, wherein the grain boundaries are clear and complete and are approximately in a grid shape.
Comparative example 1
The difference between the comparative example and the example 1 is that the corrosive agent has different components, specifically: 2g of potassium permanganate, 4ml of concentrated sulfuric acid with the mass fraction of 98 percent and 96ml of distilled water.
The other display process steps in comparative example 1 are the same as in example 1.
The prior austenite grain boundaries of the 13Cr9Mo2Co1NiVNbNB heat-resistant steel shown in comparative example 1 are shown in fig. 3, and the grain boundaries are not clearly shown in the figure.
Comparative examples 2 and 3, which are prior austenite grain boundary maps of 13Cr9Mo2Co1NiVNbNB heat-resistant steel shown in the case of using different corrodent, were also prepared according to the present invention with respect to example 1.
Comparative example 2
The corrosive agent in comparative example 2 was: supersaturated picric acid aqueous solution.
Comparative example 2 shows the procedure of the process specifically:
s1, the step is the same as the step S1 in the embodiment 1;
s2, placing the polished sample in a supersaturated picric acid aqueous solution, heating the sample in a water bath, uniformly stirring the sample in the heating process, placing the polished surface of the sample upwards into corrosive liquid after the temperature reaches 70 ℃ and the constant temperature, corroding the sample in the constant temperature solution for 20 minutes, taking out the sample by using tweezers, washing the surface by using alcohol, and drying the surface by using a blower.
S3, placing the sample on a metallographic microscope for observation, and shooting a metallographic picture of the sample by 50 times to show that the original austenite grain boundary of the 13Cr9Mo2Co1NiVNbNB heat-resistant steel is shown in a figure 4.
Comparative example 3
The corrosive agent in the comparative example 3 is picric acid hydrochloric acid alcohol solution; the method specifically comprises the following steps: 1g picric acid, 5ml hydrochloric acid with mass fraction of 38% and 60ml alcohol with mass fraction of 75%.
Comparative example 3 shows the procedure of the process specifically:
s1, the step is the same as the step S1 in the embodiment 1;
s2, placing the polished sample into a corrosive agent of picric acid hydrochloric acid alcohol solution, placing the prepared corrosive agent into a water bath pot for heating, uniformly stirring the solution in the heating process, clamping the polished surface of the sample upwards by using tweezers and placing the sample into corrosive liquid after the temperature is heated to 70 ℃ and is constant, corroding in a constant-temperature solution for 20 minutes, taking out the sample, washing the surface by using alcohol, and drying the surface by using a blower.
S3, placing the sample on a metallographic microscope for observation, and shooting a metallographic picture of the sample by 50 times to show that the original austenite grain boundary of the 13Cr9Mo2Co1NiVNbNB steel is shown in a figure 5.
Comparing the prior austenite grain boundary maps of 13Cr9Mo2Co1NiVNbNB heat-resistant steels shown in examples 1 and 2 and comparative examples 2 and 3, the maps in examples 1 and 2 clearly and completely show the grain boundaries, which are approximately in a grid shape, while the maps in comparative examples 2 and 3 do not clearly show the grain boundaries; the corrosive agent disclosed by the invention has a better corrosion effect on 13Cr9Mo2Co1NiVNbNB heat-resistant steel.
In conclusion, the invention provides the corrosive agent for displaying the original austenite grain boundary of the heat-resistant steel and the display method, the 13Cr9Mo2Co1NiVNbNB heat-resistant steel is subjected to chemical corrosion to display the grain boundary, wherein the corrosive agent has the advantages of easily obtained raw materials, simple preparation and low equipment requirement compared with an electrochemical corrosion method; meanwhile, the display method adopting the corrosive is simple and convenient to operate, and can clearly display the original austenite grain boundary of the 13Cr9Mo2Co1NiVNbNB heat-resistant cast steel, so that the grain size of the original austenite is analyzed, whether the problem of coarse grains exists or not is judged, the performance of the cast steel is deduced, and an important basis is provided for establishing a production process.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (8)
1. A method of indicating prior austenite grain boundaries of a heat resistant steel, the method comprising the steps of:
s1, preparing, grinding and polishing a sample;
s2, preparing a corrosive agent and chemically corroding the sample;
s3, observing the original austenite grain boundary of the heat-resistant steel;
in S2, the chemically etching the sample includes: 1) putting the prepared corrosive into a water bath kettle for heating, and uniformly stirring the solution in the heating process; 2) after the sample is heated to 65-70 ℃ and the temperature is constant, putting the sample into the corrosive agent with the polished surface facing upwards; 3) taking out the sample after 20-30 minutes, then soaking and washing the sample in an oxalic acid solution for 5-10 seconds, then taking out the sample, slightly wiping the surface of the sample with absorbent cotton under distilled water, washing the surface with alcohol, and then drying the sample;
every 1L of the corrosive agent comprises: 8-12 g of potassium permanganate, 100-150 ml of 98% concentrated sulfuric acid and 850-900 ml of distilled water;
the heat-resistant steel is 13Cr9Mo2Co1NiVNbNB heat-resistant cast steel.
2. The method of claim 1, wherein the etching agent comprises, per 1L: 8g of potassium permanganate, 100ml of concentrated sulfuric acid with the mass fraction of 98 percent and 900ml of distilled water.
3. The method of claim 1, wherein the etching agent comprises, per 1L: 12g of potassium permanganate, 100ml of concentrated sulfuric acid with the mass fraction of 98 percent and 900ml of distilled water.
4. The method for indicating the prior austenite grain boundary of the heat-resistant steel as claimed in claim 1, wherein in the step S1, the sample is prepared by: a metallographic specimen was cut out with a cutter.
5. The method for indicating the prior austenite grain boundary of the heat-resistant steel as claimed in claim 1, wherein in the step S1, the grinding of the sample is as follows: the sample is ground by using 180-1200-mesh silicon carbide waterproof abrasive paper, the rotating speed of a grinding disc is 300-600rpm, the sample is rotated by 90 degrees along the grinding surface when the abrasive paper is replaced each time, and distilled water is used as a lubricant in the grinding process.
6. The method for indicating the prior austenite grain boundary of the heat-resistant steel as claimed in claim 1, wherein in the step S1, the polishing of the sample is as follows: polishing by using a diamond particle suspending agent until the interface is smooth, no scratch and no stain are generated, and then washing the polished surface by using clear water and alcohol and drying.
7. The method of claim 6, wherein the diamond particle suspension has a particle size comprising 2.5 μm and 1.0 μm.
8. The method for indicating the prior austenite grain boundary of the heat-resistant steel as claimed in any one of claims 1 to 7, wherein in S3, the specimen is observed on a metallographic microscope and a metallographic picture of the specimen is taken.
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| CN116735310B (en) * | 2023-06-07 | 2023-12-19 | 国标（北京）检验认证有限公司 | Metallographic phase sample preparation method of zinc selenide polycrystalline ceramic material |
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