CN113533398B - Method for representing multi-phase oxide layer of steel plate section by adopting EBSD technology - Google Patents
Method for representing multi-phase oxide layer of steel plate section by adopting EBSD technology Download PDFInfo
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Abstract
The invention relates to a method for rapidly representing a multiphase oxide layer of a steel plate section by adopting an EBSD (electron back scattering) technology, which comprises the following steps of firstly inlaying a steel plate section sample; secondly, thinning, grinding and polishing the steel plate section sample; thirdly, scanning the EBSD surface of the steel plate section sample to obtain image data; and finally, carrying out data processing on the image data to finish characterization. The method for rapidly representing the multiphase oxide layer of the section of the steel plate by adopting the EBSD technology provided by the embodiment of the invention obviously improves the efficiency and the success rate of representing the oxide layer sample by adopting the EBSD technology. In the subsequent EBSD surface scanning, the existing oxide crystallography parameters are utilized, and a professional EBSD system is used for acquiring the information of the micro-morphology, the phase composition, the grain size, the grain orientation and the like of the steel plate section sample, so as to perform a series of qualitative/quantitative characterization on the steel oxide layer.
Description
Technical Field
The invention belongs to the technical field of physical property inspection of metal materials. In particular to a method for representing a multiphase oxide layer on the section of a steel plate by adopting an Electron Back Scattering Diffraction (EBSD) technology.
Background
A series of black skin steel products developed in recent years can find that oxide layers with special structures have certain oxidation resistance and can protect a substrate from further corrosion. Due to a series of problems of loose oxide layer structure, small adhesive force, brittle texture and the like, the preparation of the steel plate oxide layer sample becomes difficult.
By means of an Electron Back-Scattered Diffraction (EBSD) technique, researchers can obtain a large amount of crystallographic information about a sample in a short time, including phase, grain orientation, texture distribution, stress distribution and the like, but the preparation of an EBSD sample is complex, the quality of the EBSD sample often directly affects the quality of EBSD data, and if the prepared sample has problems, a clear chrysanthemum pool pattern cannot be obtained, or even characterization cannot be performed.
Due to the characteristics of small adhesive force, loose structure, large brittleness, poor conductivity and the like of the metal oxide layer, an EBSD sample with qualified quality cannot be obtained during sample preparation, and the difficulty of representing the metal oxide layer by the EBSD technology is increased. Through data search, the fact that the concrete introduction of the preparation of the metal oxide layer EBSD sample is rarely related at present, most of the concrete introduction is related to the preparation of the hot rolled plate oxide layer with strong binding force, and the problems that the steps are complex, the full-automatic sample preparation equipment is highly depended on, the time is too long and the like exist. Meanwhile, due to the phenomena of incomplete scratch removal, oxide layer breakage and falling and the like of the prepared sample, the obtained sample image and data have the problems of unclear crystal grain structure, noise reduction for multiple times (image distortion possibly caused) by using software, incapability of representing large-area oxide layers and the like.
The sample preparation method used in the prior art cannot guarantee the sample preparation effect of the non-hot-rolled oxide layer with weak binding force, and the oxide layer is easy to damage due to the fact that the sample preparation method relies on a full-automatic polishing machine to polish for a long time, and the sample preparation method only aims at the EBSD characterization of the oxide layer of the large-size-thickness steel plate section sample.
Disclosure of Invention
The invention aims to solve the problems of poor conductivity, easiness in crushing, long sample preparation time consumption, difficulty in manual operation and the like of an oxide layer in the prior art, and aims to provide a method for rapidly representing a multiphase oxide layer of a steel plate section by adopting an EBSD (electron back scattering diffraction) technology, which is used for solving the problems in the prior art.
The above technical object of the present invention will be achieved by the following technical solutions.
A method for rapidly characterizing a multiphase oxide layer of a steel plate section by adopting an EBSD technology comprises the following steps:
s1, inlaying a steel plate section sample;
s2, thinning, grinding and polishing the embedded steel plate section sample;
s3, scanning the EBSD surface of the steel plate section sample after grinding and polishing to obtain image data;
and S4, carrying out data processing on the image data to finish characterization.
The above-mentioned aspects and any possible implementation manner further provide an implementation manner, in step S1, a conductive hot insert or cold insert is used to inlay the steel plate section sample.
The above-described aspect and any possible implementation manner further provide an implementation manner, where the step S2 includes:
s21, polishing the back of the steel plate section sample, and reducing the height of the steel plate section sample to 1.0-3.5 mm;
s22, performing rough polishing on the front surface of the thinned steel plate section sample;
and S23, finely polishing the roughly polished steel plate section sample to obtain a section sample without scratches.
The above-described aspect and any possible implementation manner further provide an implementation manner, where the step S3 includes: and fixing the section sample without the scratches on a sample table, placing the section sample into a scanning electron microscope sample chamber, and acquiring image data.
In one implementation manner, the step S3 further includes selecting parameters of the oxide layer, adjusting the scanning step size to 0.1-0.8 μm, and performing EBSD full field scanning at 500-5000 times magnification.
In one implementation manner, the step S4 includes performing noise reduction processing on the image data to obtain a complete scanning result, analyzing the scanning result, and distinguishing the obtained different phases with different colors.
The above aspects and any possible implementation manners further provide an implementation manner, wherein a metallographic polishing machine is used for mechanically polishing the steel plate section sample, the rotational speed of the metallographic polishing machine is less than 200rpm, and the polishing time per mesh is not more than 60 s.
In the above aspect and any possible implementation manner, a further implementation manner is provided, when the steel plate section sample is roughly polished after being thinned at S22, the polishing agent used is diamond paste with a particle size greater than 1 μm, and the polishing cloth is a woolen fabric.
In the above aspect and any possible implementation manner, a further implementation manner is provided, when the step S23 performs fine polishing on the roughly polished steel plate section sample, the polishing agent used includes diamond paste, Al 2 O 3 And/or SiO 2 And the particle sizes of the polishing agents are all smaller than 1 mu m.
The above aspect and any possible implementation manner further provide an implementation manner, wherein the different phases at least include Ferrite, FeO and Fe 2 O 3 And Fe 3 O 4 。
The invention has the beneficial technical effects
The method for rapidly representing the multiphase oxide layer of the section of the steel plate by adopting the EBSD technology provided by the embodiment of the invention obviously improves the efficiency and the success rate of representing the oxide layer sample by adopting the EBSD technology. In the subsequent EBSD surface scanning, the existing oxide crystallography parameters are utilized, and a professional EBSD system is used for collecting the information of the microscopic morphology, the phase composition, the grain size, the grain orientation and the like of the steel plate section sample, so as to carry out a series of qualitative/quantitative characterization on the oxide layer of the steel. The method can rapidly represent the oxide layer with weaker bonding force, does not need a full-automatic polishing machine in the polishing process, and can greatly reduce the time cost and the economic cost spent in the sample preparation process.
Drawings
Embodiments of the invention are described in detail below with reference to the attached drawing figures, wherein:
FIG. 1 is a schematic flow chart of a method in an embodiment of the present invention;
FIG. 2(a) is a schematic cross-sectional view of a steel plate after being inlaid in an embodiment of the present invention;
FIG. 2(b) is a schematic front view of a steel plate cross-sectional sample according to an embodiment of the present invention;
FIG. 3 is a phase distribution diagram of a thermoformed steel oxide layer in an embodiment of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved by the present invention clearer, the following detailed description is made with reference to the accompanying drawings and specific examples, but the embodiments of the present invention are not limited thereto.
As shown in FIG. 1, a method for characterizing a multiphase oxide layer of a steel plate section by adopting an EBSD technology comprises the following specific operation steps:
step 1, inlaying a steel plate section sample;
step 2, thinning, grinding and polishing the section sample of the inlaid steel plate;
step 3, scanning the EBSD surface of the steel plate section sample after grinding and polishing to obtain image data;
and 4, carrying out data processing on the image data to finish characterization.
The EBSD technique is a material analysis method for analyzing a phase, an orientation, a stress state, and the like by irradiating an electron beam to a sample surface and collecting special electrons emitted from the sample surface as an information source, and thus the quality of the sample surface plays an important role in collecting material information, and it is necessary to obtain a highly flat, smooth, clean, and scratch-free sample surface when preparing a sample.
The specific process steps of the invention are as follows:
(1) preparation of the samples
The method comprises the following steps of inlaying a steel plate section sample by adopting a conductive hot inlaying material or a conductive cold inlaying material, polishing the back surface of the steel plate section sample by using sand paper, and grinding the steel plate section sample to be 1.0-3.5 mm in height to expose a matrix, wherein the size range can enhance the conductivity of the steel plate section sample to improve the scanning quality on one hand, and can prevent the steel plate section sample from mistakenly colliding with an EBSD probe due to overlarge height on the other hand, and an oxide layer is completely stored as far as possible; using abrasive paper which is from coarse to fine and is not more than 2000# finally, sequentially grinding the back surface of the steel plate section sample along the direction parallel to the oxide layer and the matrix, as shown in the interface of fig. 2(b), and if a metallographic polishing machine is used, grinding for 5-60 s for each mesh number; polishing the section sample of the steel plate on a metallographic polishing machine at the rotating speed of not more than 200rpm, roughly polishing by using diamond grinding paste with the granularity of more than 1 mu m and wool fabric polishing cloth to remove rough scratches on a substrate and an oxide skin, and using diamond with the granularity of less than 1 mu m and Al 2 O 3 And/or SiO 2 Polishing agent is used for fine polishing to remove unremoved fine scratches on the substrate and the oxide layer, and the used polishing cloth comprises wool fabric, panne fabric and/or silkPolishing time of each polishing agent of the silk fabric is about 5-15 min, and total polishing time is 15-40 min;
(2) EBSD surface scanning
Fixing a polished steel plate section sample on a sample table inclined at 70 degrees by using a conductive adhesive, placing the sample table into a scanning electron microscope sample chamber, collecting an image, selecting the image to a region to be scanned, and removing the back bottom after adjusting parameters to obtain a clear chrysanthemum pool pattern; selecting parameters of the oxide layer at least comprising Ferrite, FeO and Fe 2 O 3 And Fe 3 O 4 Adjusting the scanning step length to be 0.1-0.8 mu m, performing EBSD full-view scanning under the magnification of 500-5000 times, and collecting data;
(3) EBSD surface scan data analysis
Firstly, noise reduction processing is carried out on acquired data, noise points in scanning results are removed, complete scanning results are obtained, then different colors or gray levels are set, and different phases are calibrated and distinguished.
Examples
The steel plate section sample is obtained by heating hot forming steel to 900 ℃, preserving heat in air for 20min, then cooling in air, scanning an oxide layer of the steel plate section sample to obtain scanning data of an EBSD surface, and analyzing a microstructure of a scanning area on the basis of phase composition analysis and texture analysis.
The specific technical steps are as follows:
the steel plate section sample is embedded by using a conductive thermal embedding material so as to protect an oxide layer and facilitate subsequent grinding and polishing.
Selecting 200# abrasive paper, and grinding the back of the inlaid steel plate section sample at a low speed, wherein as shown in fig. 2(a) -2 (b), the inlay material has a certain fixing effect, so that the integrity of the front of the steel plate section sample can be ensured when the back of the steel plate section sample is ground at the low speed, when the sample is ground to a substrate, the sample is ground at the low speed by 400# abrasive paper, and the grinding thickness is 2.0mm, so that a weaker oxide layer on the steel plate section is ensured and is completely preserved as far as possible.
And sequentially adopting 1000#, 1200#, 1500# and 2000# sandpaper to polish the front surface of the steel plate section sample on a metallographic polishing machine, using water as lubrication and removing pollutants, and always polishing along the direction parallel to the interface of an oxide layer and a matrix, as shown in fig. 2 (b). The rotating speed of the metallographic polishing machine does not exceed 200rpm, and the polishing time of the sample on each piece of sand paper is less than 1 min.
Polishing the front surface of the steel plate section sample on a metallographic polishing machine by using fine polishing cloth, wherein the rotation speed of the polishing machine is 150rpm, rough polishing is carried out by using diamond grinding paste with the granularity of 2.5 mu m, and the diamond grinding paste with the granularity of 0.5 mu m and Al with the granularity of 0.05 mu m are used 2 O 3 Polishing with 0.05 μm SiO 2 And final polishing is carried out on the polishing agents, the polishing time of each polishing agent is about 7min, the total polishing time is about 30min, and fine polishing is completed after scratches on the front surface of the steel plate section sample are completely removed.
Fixing the polished steel plate section sample on a sample table by using conductive adhesive, then placing the sample table into a sample chamber of a scanning electron microscope, and vacuumizing.
Selecting a proper observation position by using a scanning electron microscope, extending an EBSD probe into a sample chamber, acquiring data by using an EBSD module of TEAM software after a clear surface image is obtained by using the scanning electron microscope SEM, removing the background after parameters are adjusted to obtain a clear chrysanthemum pool pattern, selecting Fe and O elements in a component database, and then selecting Ferrite, FeO and Fe 2 O 3 、Fe 3 O 4 Amplifying the image to 700 times with four crystallographic parameters, selecting step length of 0.4 μm, starting surface scanning, the oxide layer containing FeO and Fe 2 O 3 、Fe 3 O 4 The three phases have different crystal structures, FeO is a face-centered cubic crystal, Fe 3 O 4 Being cubic crystals, Fe 2 O 3 The Ferrite is a close-packed hexagonal crystal, and the composition and the structure of the Ferrite are relatively fixed. Therefore, Ferrite, FeO and Fe are selected according to the invention 2 O 3 、Fe 3 O 4 The four phases are obtained by collecting the crystallographic parameters, and the properties of the oxide layer are known through the parameters, so that the microstructure of the oxide layer on the surface of the steel plate is changed, and the oxidation resistance of the surface of the steel plate is effectively improved. Providing accurate information of the above phases, storing the collected Julian style in databaseComparing the stored Juchi patterns, and calibrating and determining the phase if the two patterns are consistent.
The EBSD data is processed by using OIM Analysis software of EDAX company, and an image with noise points and error mark points removed is obtained after the EBSD data is processed by a Cleanup dataset module.
Performing qualitative and quantitative analysis on the scanning result of the EBSD surface by using an orientation imaging technology to obtain Ferrite, FeO and Fe 2 O 3 、Fe 3 O 4 The four phases with different crystal structures are distinguished by different shades of gray or color. Because different phases have different crystal structures, the phases can be determined according to the collected Juliangchua patterns and the calibration result, phase imaging can be realized by adopting an orientation imaging technology, the distribution of each phase can be clearly displayed in an image, and the relative content of each phase can be calculated, thereby realizing qualitative and quantitative analysis.
The colors of the different phases are set for each phase, White for Ferrite, Grey-40 for FeO, and Grey-50 for Fe 2 O 3 And Dark grey (Dark grey) represents Fe 3 O 4 . The resulting EBSD data image in this example is shown in figure 3.
While the foregoing description shows and describes several preferred embodiments of the invention, it is to be understood, as noted above, that the invention is not limited to the forms disclosed herein, but is not intended to be exhaustive or to exclude other embodiments and may be used in various other combinations, modifications, and environments and is capable of changes within the scope of the invention as expressed herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. A method for representing a multi-phase oxide layer on a section of a steel plate by adopting an EBSD technology is characterized by comprising the following steps:
(1) preparation of the samples
Inlaying the steel plate section sample, polishing the back of the steel plate section sample by using sand paper, and cutting the steel plateGrinding the surface sample to 1.0-3.5 mm in height to expose the substrate; grinding the back of the section sample of the steel plate by using sand paper from coarse to fine and not exceeding 2000# finally, and if a metallographic polishing machine is used, grinding for 5-60 s is required for each mesh; polishing a steel plate section sample on a metallographic polishing machine, wherein the rotating speed is not more than 200rpm, and roughly polishing by using diamond grinding paste with the granularity of more than 1 mu m and wool fabric polishing cloth to remove rough scratches on a matrix and an oxide skin; using diamond with a particle size of less than 1 μm, Al 2 O 3 And/or SiO 2 The polishing agent is subjected to fine polishing to remove unremoved fine scratches on the substrate and the oxide layer;
(2) EBSD surface scanning
Scanning the EBSD surface of the steel plate section sample after grinding and polishing to obtain image data;
(3) EBSD surface scan data analysis
And carrying out data processing on the image data to finish the characterization.
2. The method according to claim 1, wherein the steel plate section sample is inlaid with a conductive hot or cold inlay in the step (1).
3. The method of claim 1, wherein step (2) comprises: and fixing the steel plate section sample without scratches on a sample table, putting the sample into a scanning electron microscope sample chamber, and collecting image data.
4. The method of claim 3, wherein step (2) further comprises selecting oxide layer parameters, adjusting the scanning step size to 0.1-0.8 μm, and performing EBSD full field scan at 500-5000 times magnification.
5. The method of claim 1, wherein step (3) comprises subjecting the image data to noise reduction to obtain a complete scan result, analyzing the scan result, and distinguishing the obtained different phases with different colors.
6. The method of claim 5, wherein the different phases comprise at least Ferrite, FeO, Fe 2 O 3 And Fe 3 O 4 。
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