CN112160018B - Method for preparing super martensitic stainless steel EBSD sample - Google Patents

Method for preparing super martensitic stainless steel EBSD sample Download PDF

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CN112160018B
CN112160018B CN202011034253.2A CN202011034253A CN112160018B CN 112160018 B CN112160018 B CN 112160018B CN 202011034253 A CN202011034253 A CN 202011034253A CN 112160018 B CN112160018 B CN 112160018B
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stainless steel
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CN112160018A (en
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庞阳
邹德宁
李苗苗
佟立波
赵碧芳
闫星宇
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Xian University of Architecture and Technology
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F3/00—Electrolytic etching or polishing
    • C25F3/16—Polishing
    • C25F3/22—Polishing of heavy metals
    • C25F3/24—Polishing of heavy metals of iron or steel
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/32—Polishing; Etching

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Abstract

The invention discloses a method for preparing a super martensitic stainless steel EBSD sample, which comprises the steps of polishing solution preparation, sample grinding, electrolytic polishing and polished surface cleaning; the polishing solution consists of HCLO with the volume ratio of (1 +/-0.1) to (3 +/-0.1) to (6 +/-0.1)4、CH3COOH and C2H5OH is mixed to prepare, a cathode uses a stainless steel sheet, and a super martensitic stainless steel sample is used as an anode; then placing the electrolysis device on a magnetic stirrer, cooling the electrolyte by using liquid nitrogen, and adjusting the power supply voltage; finally, a stainless steel clamp is utilized to immerse the sample into the electrolyte, the grinding surface is parallel to the cathode stainless steel sheet, the power supply current is adjusted, and polishing is started; and taking out the sample after polishing, wiping and drying. The invention has short polishing time and high polishing efficiency, and can lead the EBSD acquisition and calibration rate to reach more than 95 percent.

Description

Method for preparing super martensitic stainless steel EBSD sample
Technical Field
The invention belongs to the technical field of electrolytic polishing methods, and particularly relates to a method for preparing a super martensitic stainless steel EBSD sample.
Background
The super martensitic stainless steel not only has the characteristics of the traditional martensitic stainless steel, but also has good corrosion resistance in a carbon dioxide environment or a carbon dioxide and hydrogen sulfide environment, has excellent welding performance, and is widely applied to key structures and parts, such as turbines, ship propellers, airplane parts and oil and gas field pipelines. The super martensitic stainless steel has lath martensite and retained austenite structures, different heat treatment processes can change the structure state in the steel, and the research on the orientation relationship between martensite and austenite and the content, morphology and size of the retained austenite has important significance. The TEM technology is not only tedious in sample preparation, but also less in data acquisition amount. The EBSD sample is easier to prepare, a large amount of data can be collected with high efficiency, but the requirement on the surface quality of the EBSD sample is higher, the surface of the sample needs to be clean and flat, no continuous corrosion pits exist, and no residual stress exists, so that the high-quality chrysanthemum pool pattern can be ensured.
When the EBSD sample is prepared by the electrolytic polishing method, the method has the characteristics of simple sample preparation, time saving and low cost, but the calibration rate of the super martensitic stainless steel EBSD sample prepared by the electrolytic polishing method at present is not high enough, so that a new method for preparing the super martensitic stainless steel EBSD sample with higher calibration rate is urgently needed. When the super martensitic stainless steel EBSD sample is prepared by utilizing an electrolytic polishing mode, the selection of the electrolyte and the polishing time and voltage in the electrolytic polishing process plays a decisive role, the quality of the EBSD sample is directly determined, and the height of the calibration rate is determined, and for different electrolytes, how to find the electrolytic polishing parameters (current, voltage and time) which are correctly matched with the electrolytes to ensure the calibration rate is a technical difficulty.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a method for preparing a super martensitic stainless steel EBSD sample.
The invention adopts the following technical scheme:
a method for preparing a super martensitic stainless steel EBSD sample, comprising the process of:
pretreating the surface of the sample before electrolytic polishing;
and (3) performing electrolytic polishing on the pretreated sample, wherein during electrolytic polishing: the electrolyte is prepared by mixing perchloric acid, acetic acid and alcohol, the anode is a mechanically polished sample, the mechanically polished sample is clamped by a stainless steel clamp with the corrosion rate similar to that of the sample, the distance between the cathode and the anode is 2-4 cm, the voltage between the cathode and the anode is 25-35V, the current is 1.0-1.5A, the polishing time is 60-80 s, and the temperature of the electrolyte is controlled to be-20-0 ℃; continuously stirring the electrolyte in the electrolytic polishing process;
and taking out the sample after the electrolytic polishing is finished, and cleaning and drying to obtain the super martensitic stainless steel EBSD sample.
Preferably, the pretreatment of the surface of the sample before electropolishing comprises: and sequentially carrying out mechanical grinding and mechanical polishing on the surface of the sample, wherein an aluminum oxide polishing solution is adopted during the mechanical polishing.
Preferably, when the sample surface is mechanically ground, 400#, 600#, 1000#, 1500# and 2000# aqueous sandpaper are used for grinding in sequence, and each grinding is performed with the previous-time sandpaper vertically until the previous-time grinding mark is ground off.
Preferably, the mechanical polishing time is 2-3 min.
Preferably, the electrolyte is a mixture formed by mixing perchloric acid, acetic acid and alcohol according to the volume ratio of (1 +/-0.1) to (3 +/-0.1) to (6 +/-0.1).
Preferably, the electrolyte is magnetically stirred in the electrolytic polishing process, and the rotating speed of a magnetic stirrer is set to be 120-160 r/min.
Preferably, during electrolytic polishing, liquid nitrogen is added into the electrolyte to control the temperature of the electrolyte to be-20-0 ℃.
Preferably, the corrosion rate of the sample does not deviate more than 0.05mm/a from the corrosion rate of the stainless steel jig.
Compared with the prior art, the invention has the following beneficial effects:
compared with the conventional perchloric acid and alcohol electrolyte, the method for preparing the EBSD sample of the super martensitic stainless steel has the advantages that part of acetic acid is added, the acetic acid has an adsorption effect on the electrolyzed metal ions and is adsorbed on the convex part, and the dissolving speed of the concave part is reduced, so that the dissolving speed of the convex part is accelerated. The perchloric acid has the strongest acidity in acetic acid, so that the polishing effect can be greatly improved, the acetic acid can also reduce the decomposition speed of the perchloric acid, and the service life of the polishing solution is prolonged. The anode uses a martensitic stainless steel clamp with the corrosion rate similar to that of the sample to clamp the sample, and the corrosion speed of the stainless steel clamp is similar to that of the super martensitic stainless steel sample, so that a dark area can be eliminated, and the whole surface of the sample is smooth and bright; the electrolyte is continuously stirred in the polishing process, so that the electrolyte flow can be promoted, the ion diffusion of a polishing area and the supplement of new electrolyte are ensured, and spots on the uneven surface during polishing are avoided. The method has the advantages that the set parameters of polishing voltage, current and time directly influence the quality of a sample in the electrolytic polishing process, the voltage between a cathode and an anode is set to be 25-35V, the current is 1.0-1.5A, the polishing time is 60-80 s, if the voltage exceeds the current range or the polishing time is too long, the alloy is easily over-corroded, if the voltage is lower than the current range or the polishing time is too short, the stress layer of the sample cannot be effectively removed, and the two conditions influence the calibration rate, so that the experimental result is influenced. The temperature of the electrolyte can be increased in the electrolytic polishing process, so that the current is easy to increase and is difficult to control, and the temperature of the electrolyte is controlled to be-20-0 ℃. According to the method, a new electrolyte is adopted, and the electropolishing parameters which are correctly matched with the electrolyte are determined, so that the standard rate of the super martensitic stainless steel EBSD sample prepared by the method is higher than that of the prior art, and the standard rate of the super martensitic stainless steel EBSD sample reaches more than 95%.
Further, the pretreatment of the surface of the sample before the electrolytic polishing comprises: the method has the advantages that the surface of the sample is sequentially subjected to mechanical grinding and mechanical polishing, and then electropolishing is performed after the mechanical polishing, so that the adverse effect of scratches on the sample calibration rate can be effectively prevented, and the aluminum oxide polishing solution is adopted during the mechanical polishing to prevent the stress concentration of the sample during the polishing.
Furthermore, the electrolyte is a mixture formed by mixing perchloric acid, acetic acid and alcohol according to the volume ratio of (1 +/-0.1) to (3 +/-0.1) to (6 +/-0.1), wherein the addition of the acetic acid can improve the polishing effect and prolong the service life of the polishing solution.
Furthermore, magnetic stirring is carried out on the electrolyte in the electrolytic polishing process, the rotating speed of a magnetic stirrer is set to be 120-160 r/min, and the electrolyte is stirred to ensure the ion diffusion of a polishing area and the supplement of new electrolyte.
Furthermore, during electrolytic polishing, liquid nitrogen is added into the electrolyte to control the temperature of the electrolyte to be-20-0 ℃, and the liquid nitrogen is adopted to cool the electrolyte aiming at the characteristic that the temperature of the electrolyte is increased in the electrolytic polishing process and the current is easy to increase and is not easy to control, so that the temperature of the electrolyte is easy to control, and the electrolytic polishing process is time-saving and convenient.
Drawings
FIG. 1 is an EBSD mass contrast chart for example 1 of the inventive preparation of a super martensitic stainless steel EBSD sample.
FIG. 2 is an EBSD orientation image of example 1 of the invention for preparing a sample of a super martensitic stainless steel EBSD.
FIG. 3 is an EBSD mass contrast chart for example 2 of the inventive preparation of a super martensitic stainless steel EBSD sample.
FIG. 4 is an EBSD orientation image of example 2 of the invention for preparing a super martensitic stainless steel EBSD sample.
FIG. 5 is an EBSD mass contrast plot for example 3 of a super martensitic stainless steel EBSD sample prepared in accordance with the present invention.
FIG. 6 is an EBSD orientation image of example 3 of the invention for preparing a super martensitic stainless steel EBSD sample.
FIG. 7 is an EBSD orientation image of a prior art EBSD sample prepared from the super martensitic stainless steel.
Detailed Description
The invention is explained in detail below with reference to the figures and the specific examples.
The method for preparing the super martensitic stainless steel EBSD sample comprises the following steps:
step 1, carrying out mechanical grinding and mechanical polishing on the surface of a sample;
step 2, preparing polishing solution, and uniformly mixing perchloric acid, acetic acid and alcohol to obtain the polishing solution;
step 3, placing the beaker filled with the electrolyte on a magnetic stirrer, then placing the stainless steel sheet into the beaker, connecting the stainless steel sheet with the negative electrode of a power supply, connecting the martensitic stainless steel clamp with the positive electrode of the power supply, adjusting the voltage of the power supply, and finally pouring liquid nitrogen into the beaker for cooling;
step 4, clamping the sample prepared in the step 1 by using a stainless steel clamp, putting the sample into electrolyte, adjusting the power supply current, and starting polishing, wherein the grinding surface of the sample is parallel to the cathode stainless steel sheet;
and 5, taking out the sample electropolished in the step 4, wiping and cleaning the sample by using alcohol, and finally drying the sample to finish polishing.
The specific process of the step 1 is as follows: and mechanically grinding and polishing the surface of the stainless steel, and grinding by using 400#, 600#, 1000#, 1500#, and 2000# water-based sandpaper in sequence, wherein the sandpaper is vertical to the previous one time during each grinding until the grinding mark of the previous one time is ground off. And polishing by using a polishing machine, wherein an aluminum oxide polishing agent is used as a polishing solution, and the polishing time is 2-3 min.
The electrolyte adopted in the step 2 is HCLO4:CH3COOH:C2H5A mixture of 1:3:6, wherein, when the volumes of the individual components are measured, the volume error does not exceed 10% of the respective volume.
And 3, setting the rotating speed of the magnetic stirrer to be 120-160 r/min.
And 3, the power supply voltage is 25-35V.
And (3) cooling to-20-0 ℃ by adopting liquid nitrogen.
In the step 4, the power supply current is 1.0-1.5A, and the polishing time is 60-80 s.
Example 1
In this example, the surface of a 10 × 10 sample of 0.03c13cr0.23n super martensitic stainless steel was polished.
Step 1, mechanically grinding the surface of a sample, grinding with 400#, 600#, 1000#, 1500#, and 2000# aqueous sandpaper in sequence, wherein each grinding is performed with the previous-time sandpaper vertically until the previous-time grinding mark is ground off. And polishing by using a polishing machine for 2min to obtain a mechanically polished sample, wherein the polishing solution adopts an aluminum oxide polishing agent.
Step 2, pouring 240ml of C into a beaker2H5OH and 120ml CH3COOHThen 40ml HCLO was added4And draining by using a glass rod, and uniformly mixing to obtain the polishing solution.
Step 3, adding polishing solution into the beaker, placing the beaker on a magnetic stirrer, setting the rotating speed of the stirrer to be 120r/min, then placing a stainless steel plate into the beaker and connecting the stainless steel plate with the negative pole of a power supply, taking the stainless steel plate as the cathode, connecting a martensitic stainless steel clamp with the positive pole of the power supply, adjusting the voltage of the power supply to 25V, finally pouring liquid nitrogen into the beaker for cooling, and preparing for polishing when the temperature is reduced to-20 ℃;
step 4, clamping the mechanically polished sample prepared in the step 1 by using a stainless steel clamp, putting the sample into electrolyte, taking the sample as an anode, and adjusting the distance between the anode and a cathode steel plate to be 4cm, so that the power supply current is 1.0A, and the polishing time is 80 s;
and 5, taking out the sample electropolished in the step 4, wiping and cleaning the sample by using alcohol, and finally drying the sample to finish polishing.
The experimental results are as follows: EBSD samples were observed using a JSM-6390 field emission scanning electron microscope equipped with Oxford Aztec system, with an operating voltage set at 20kV, an inclination angle of 70.0 DEG, and a scanning step of 0.14 μm/s. The mass contrast of the microstructure EBSD of the polished sample is shown in fig. 1, with a calibration rate of 95.3%, and the black regions indicated by arrows in fig. 1 are unresolved regions. FIG. 2 is an EBSD orientation imaging diagram of the sample, the color contrast of martensite in different orientations is obvious, and the characterization effect is good.
Example 2
In this example, the surface of a 10 × 10 sample of 0.03c13cr0.3n super martensitic stainless steel was polished.
Step 1, mechanically grinding the surface of a sample, grinding with 400#, 600#, 1000#, 1500#, and 2000# aqueous sandpaper in sequence, wherein each grinding is performed with the previous-time sandpaper vertically until the previous-time grinding mark is ground off. And polishing by using a polishing machine for 2.5min to obtain a mechanically polished sample, wherein the polishing solution adopts an aluminum oxide polishing agent.
Step 2, pouring 240mlC into the beaker2H5OH and 120mlCH3COOH, then 40ml HCLO4And draining by using a glass rod, and uniformly mixing to obtain the polishing solution.
Step 3, adding polishing solution into the beaker, placing the beaker on a magnetic stirrer, setting the rotating speed of the stirrer to be 140r/min, then placing a stainless steel plate into the beaker, connecting the stainless steel plate with the negative pole of a power supply, taking the stainless steel plate as the cathode, connecting a martensitic stainless steel clamp with the positive pole of the power supply, adjusting the voltage of the power supply to 30V, finally pouring liquid nitrogen into the beaker for cooling, and preparing for polishing when the temperature is reduced to-10 ℃;
step 4, clamping the mechanically polished sample prepared in the step 1 by using a stainless steel clamp, putting the sample into electrolyte, taking the sample as an anode, and adjusting the distance between the anode and a cathode steel plate to be 3cm, so that the power supply current is 1.3A, and the polishing time is 70 s;
and 5, taking out the sample electropolished in the step 4, wiping and cleaning the sample by using alcohol, and finally drying the sample to finish polishing.
The experimental results are as follows: EBSD samples were observed using a JSM-6390 field emission scanning electron microscope equipped with Oxford Aztec system, with an operating voltage set at 20kV, an inclination angle of 70.0 DEG, and a scanning step of 0.17 μm/s. The mass contrast of the microstructure EBSD of the polished sample is shown in fig. 3, where the calibration rate is 96.9%, and the black part indicated by the arrow in fig. 3 is an unresolved region. FIG. 4 is an EBSD orientation imaging diagram of the sample, the color contrast of martensite in different orientations is obvious, and the characterization effect is good.
Example 3
In this example, the surface of a 10 × 10 sample of 0.03c13cr0.35n super martensitic stainless steel was polished.
Step 1, mechanically grinding the surface of a sample, grinding with 400#, 600#, 1000#, 1500#, and 2000# aqueous sandpaper in sequence, wherein each grinding is performed with the previous-time sandpaper vertically until the previous-time grinding mark is ground off. And polishing by using a polishing machine for 3min to obtain a mechanically polished sample, wherein the polishing solution adopts an aluminum oxide polishing agent.
Step 2, pouring 240mlC into the beaker2H5OH and 120mlCH3COOH, then 40ml HCLO4And the glass rod is used for drainage, the mixture is uniform,and obtaining the polishing solution.
Step 3, adding polishing solution into the beaker, placing the beaker on a magnetic stirrer, setting the rotating speed of the stirrer to be 120r/min, then placing a stainless steel plate into the beaker, connecting the stainless steel plate with the negative pole of a power supply, taking the stainless steel plate as the cathode, connecting a martensitic stainless steel clamp with the positive pole of the power supply, adjusting the voltage of the power supply to 30V, finally pouring liquid nitrogen into the beaker for cooling, and preparing for polishing when the temperature is reduced to 0 ℃;
step 4, clamping the mechanically polished sample prepared in the step 1 by using a stainless steel clamp, putting the sample into electrolyte, taking the sample as an anode, and adjusting the distance between the anode and a cathode steel plate to be kept at 2cm, so that the power supply current is 1.5A, and the polishing time is 60 s;
and 5, taking out the sample electropolished in the step 4, wiping and cleaning the sample by using alcohol, and finally drying the sample to finish polishing.
The experimental results are as follows: EBSD samples were observed using a JSM-6390 field emission scanning electron microscope equipped with Oxford Aztec system, with an operating voltage set at 20kV, an inclination angle of 70.0 DEG, and a scanning step of 0.15 μm/s. The mass contrast of the microstructure EBSD of the polished sample is shown in fig. 5, with a calibration ratio of 95.1%, and the black portions indicated by arrows in fig. 5 are unresolved regions. FIG. 6 is an EBSD orientation imaging diagram of the sample, the color contrast of martensite in different orientations is obvious, and the characterization effect is good.
FIG. 7 is a diagram of a prior art EBSD sample for preparing super martensitic stainless steel, which is derived from the document "Effect of carbon partition in the reversed austenite of supermarkentistic stainless steel", and compared with the embodiment of the present invention, it can be seen that the calibration rate is significantly lower than that of the present application, the resolution of the diagram is lower than that of the embodiment of the present invention, and the analysis of EBSD structure is also affected to a certain extent.

Claims (7)

1. A method for preparing a super martensitic stainless steel EBSD sample is characterized by comprising the following steps:
pretreating the surface of the sample before electrolytic polishing;
and (3) performing electrolytic polishing on the pretreated sample, wherein during electrolytic polishing: the electrolyte is prepared by mixing perchloric acid, acetic acid and alcohol, the anode is a mechanically polished sample, the mechanically polished sample is clamped by a stainless steel clamp with the corrosion rate similar to that of the sample, the distance between the cathode and the anode is 2-4 cm, the voltage between the cathode and the anode is 25-35V, the current is 1.0-1.5A, the polishing time is 60-80 s, and the temperature of the electrolyte is controlled to be-20-0 ℃; continuously stirring the electrolyte in the electrolytic polishing process;
taking out the sample after the electrolytic polishing is finished, and cleaning and drying the sample to obtain the super martensitic stainless steel EBSD sample;
the electrolyte is a mixture formed by mixing perchloric acid, acetic acid and alcohol according to the volume ratio of (1 +/-0.1) to (3 +/-0.1) to (6 +/-0.1).
2. The method of preparing the super martensitic stainless steel EBSD sample according to claim 1, wherein the pretreatment of the sample surface before electropolishing comprises: and sequentially carrying out mechanical grinding and mechanical polishing on the surface of the sample, wherein an aluminum oxide polishing solution is adopted during the mechanical polishing.
3. The method for preparing the EBSD sample of the super martensitic stainless steel as claimed in claim 2, wherein the mechanical grinding is performed on the surface of the sample by using 400#, 600#, 1000#, 1500# and 2000# aqueous sandpaper in sequence, and each grinding is performed by using the previous sandpaper vertically until the previous grinding scar is removed.
4. The method of preparing the EBSD sample of the super martensitic stainless steel as claimed in claim 2, wherein the mechanical polishing time is 2min to 3 min.
5. The method for preparing the EBSD sample of the super martensitic stainless steel as claimed in claim 1, wherein the electrolyte is magnetically stirred during the electropolishing process, and the rotating speed of the magnetic stirrer is set to 120-160 r/min.
6. The method for preparing the EBSD sample of the super martensitic stainless steel as claimed in claim 1, wherein during electrolytic polishing, liquid nitrogen is added into the electrolyte to control the temperature of the electrolyte to be-20-0 ℃.
7. The method of preparing a super martensitic stainless steel EBSD sample of claim 1 wherein the sample has a corrosion rate that does not deviate more than 0.05mm/a from the corrosion rate of the stainless steel fixture.
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