CN112129686A - Positioning tracking characterization method for corrosion research - Google Patents
Positioning tracking characterization method for corrosion research Download PDFInfo
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- CN112129686A CN112129686A CN201910549262.6A CN201910549262A CN112129686A CN 112129686 A CN112129686 A CN 112129686A CN 201910549262 A CN201910549262 A CN 201910549262A CN 112129686 A CN112129686 A CN 112129686A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/006—Investigating resistance of materials to the weather, to corrosion, or to light of metals
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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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- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/2005—Preparation of powder samples therefor
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- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
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- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
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- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
Abstract
The invention relates to a positioning, tracking and characterizing method for corrosion research, and belongs to the field of research on material corrosion. The method comprises the steps of marking a hardness indentation on the surface of a sample by using a micro Vickers hardness tester as a mark for positioning, tracking and observing, recording the position of the indentation on the surface of the sample, and testing the shape, components and microstructure of the sample which is not corroded in a positioning area; repeating the process of taking out and retesting after the corrosion to obtain the corrosion appearance of the surface of the material and the time sequence data of the product; and positioning, tracking and analyzing the microstructure by using image processing software and taking the indentation as an anchor point. The method can obtain the corrosion characteristics of different stages by observing only one sample, can realize the effect of approximate in-situ test without using a special in-situ test instrument, can continuously observe the evolution process of the microstructure of the material at different corrosion stages in any corrosion environment, and expands the corrosion analysis from the whole material to the microscopic level.
Description
Technical Field
The invention relates to a positioning, tracking and characterizing method for corrosion research, in particular to a high-flux positioning, tracking and characterizing technology and application thereof in corrosion research, belonging to the field of research on material corrosion.
Background
For the research of metal materials in the corrosion field, generally, a plurality of control samples are prepared, corrosion is carried out under different environmental conditions or for different time, the corrosion mechanism of the materials is analyzed by methods of measuring corrosion weight loss, observing corrosion morphology and corrosion products and the like, and finally, a conclusion is drawn. The traditional method uses a plurality of samples and has long experimental time.
The in-situ test can trace and research the transformation rule and mechanism of the material microstructure. However, in-situ testing must be accomplished by special and expensive special equipment, and for in-situ testing of corrosion of materials, observation is required by a special Environmental Scanning Electron Microscope (ESEM). However, the method cannot observe the corrosion morphology of the material matrix under the corrosion product; in addition, the method creates a corrosive environment by circulating a flowing gas corrosive medium in the sample chamber, but cannot circulate a liquid corrosive medium in the equipment, so that certain corrosive environments, such as a marine corrosive environment, cannot be simulated.
In the conventional corrosion research, the material is generally analyzed as a whole, and the microstructure of the material is rarely researched.
Disclosure of Invention
The invention aims to overcome the defects that the traditional method has more samples and long time consumption, the in-situ test is limited by a simulated corrosion environment and the like in the prior art, provides a positioning tracking characterization technology similar to the in-situ test, can continuously observe the evolution rule of a microstructure in the material corrosion process at different corrosion stages, obtains the material surface corrosion morphology and the time sequence data of a product, and analyzes the corrosion mechanism of the material.
The invention relates to a positioning tracking characterization method for corrosion research, which utilizes a micro Vickers hardness indentation as a positioning mark; and positioning, tracking and analyzing the sample microstructure by using image processing software.
A location tracking characterization method for corrosion research is characterized in that a micro Vickers hardness tester is used for punching hardness indentations on the surface of a sample as a mark for location tracking observation, the positions of the indentations on the surface of the sample are recorded, and the shape, components and microstructure of the sample which is not corroded in a location area are tested; repeating the process of taking out and retesting after the corrosion to obtain the corrosion appearance of the surface of the material and the time sequence data of the product; and finally, positioning, tracking and analyzing the microstructure by using image processing software and taking the indentation as an anchor point.
The invention relates to a positioning, tracking and characterizing method for corrosion research, which comprises the following specific steps:
(1) preparing a metal material experimental sample for corrosion research;
(2) manufacturing a hardness indentation on the surface of a sample by using a micro Vickers hardness tester as a mark for positioning, tracking and observing;
(3) recording the position of the positioning indentation on the surface of the sample, and carrying out Scanning Electron Microscope (SEM) shooting on the surface of the sample to obtain the non-corroded surface appearance of the positioning area of the sample; obtaining microstructure information of crystal orientation and grain boundary type of the positioning area through a grain orientation distribution diagram (Auto IPF diagram) and a grain boundary characteristic distribution diagram (CSL diagram) in an Electron Back Scattering Diffraction (EBSD) test; performing energy spectrum testing (EDS) to obtain element composition information of the area;
(4) simulating a corrosion environment to corrode the sample;
(5) taking out a sample, observing the sample by a Scanning Electron Microscope (SEM), and shooting the corrosion characteristics of the positioning area at the corrosion stage; obtaining the element content of the corrosion product of the localized area by an energy spectrum test (EDS) test;
(6) repeating the steps (4) and (5) to obtain the surface corrosion morphology of the sample and the time sequence data of the product;
(7) and covering an Electron Back Scattering Diffraction (EBSD) test result on Scanning Electron Microscope (SEM) corrosion morphology photographs at different corrosion stages by using image processing software, taking the positioning indentation as an anchor point of overlapping operation, and simultaneously combining the information of morphology and components to realize the joint analysis of SEM + EDS + EBSD.
In the step (1), when preparing the metal material experimental sample for corrosion research, a conventional Electron Back Scattering Diffraction (EBSD) sample preparation technique may be adopted.
For example, a suitably sized sample is obtained by cutting; after inlaying, the surface is polished by five sand papers from coarse to fine (120#, 220#, 500#, 1000#, 2400 #); sequentially spraying diamond spraying polishing paste with the particle sizes of 2.5 mu m and 1.0 mu m for mechanical polishing; electropolishing was performed using an 8V dc power supply in a polishing solution of 70% (vol%) phosphoric acid (analytically pure) + 30% (vol%) absolute ethanol (analytically pure); the residual stains were washed sequentially with distilled water and absolute ethanol (analytical grade) and dried with a blower.
In the step (2), a plurality of micro-vickers hardness instruments are utilized to punch a plurality of indentations on the surface of the sample, for example, 3 hardness indentations are used as marks for positioning, tracking and observing, working pressures with different sizes are selected according to different experimental materials, and the indentations are clear and distinguishable. And selecting the clearest and complete one of the hardness indentations as an observed positioning mark.
In the step (3), an image processing software is utilized to cover a grain orientation distribution diagram (Auto IPF diagram) and a grain boundary characteristic distribution diagram (CSL diagram) obtained by an EBSD test on an SEM topography photograph, and a positioning indentation is taken as an anchor point of an overlapping operation, and simultaneously, the time sequence data of the surface topography and components of the sample are combined to realize the evolution rule of the microstructure of the SEM + EDS + EBSD combined analysis sample at different corrosion stages.
Compared with the prior art, the invention has the beneficial effects that: the positioning tracking characterization of the invention only needs to observe one sample to obtain the corrosion characteristics of different stages; the effect similar to the in-situ test can be realized only by using an SEM equipped with EBSD and EDS accessories without using special ESEM; the corrosion environment is not limited to a gas atmosphere any more, and can be any corrosion environment; the evolution process of the microstructure of the material at different corrosion stages can be continuously observed, and the corrosion analysis is expanded from the whole material to the microscopic level. In addition, the method conforms to the concept of high-throughput experiments in material genome engineering.
Drawings
FIG. 1 is an SEM topography of localized areas of a test sample without erosion.
Fig. 2 is a distribution diagram of the grain orientation near the positioning indentations obtained by the EBSD test.
FIG. 3 is a distribution diagram of grain boundary features near the localized indentation obtained from the EBSD test.
FIG. 4 is a graph of the corrosion profile of the test samples after cumulative immersion for 0-7 days, wherein (a) day 0, (b) day 1, (c) day 2, (d) day 3, (e) day 4, (f) day 5, (g) day 6, and (h) day 7.
FIG. 5 is a graph of the grain orientation distribution map and grain boundary characteristic distribution map of localized areas of the sample overlaid on the SEM corrosion topography photographs for the effects of localization tracking characterization, wherein (a) is 1 day, (b) is 2 days, (c) is 3 days, (d) is 4 days, (e) is 5 days, (f) is 6 days, and (g) is 7 days.
Detailed Description
Firstly, preparing a metal material experimental sample for corrosion research, and then, utilizing a micro Vickers hardness tester to make a positioning indentation on the surface of the sample as a mark for positioning, tracking and observing; respectively carrying out Scanning Electron Microscope (SEM), Electron Back Scattering Diffraction (EBSD) and energy spectrum analysis (EDS) tests on the surface of the sample to obtain the unetched surface morphology, microstructure information and element component information of a sample positioning area; simulating a corrosion environment to corrode the sample; taking out samples periodically, and carrying out SEM test to obtain the surface corrosion morphology of the samples and the time sequence data of the products; and utilizing image processing software to take the positioning indentation as an anchor point, covering the EBSD test result on the SEM morphology picture, and simultaneously combining the morphology and component information to carry out SEM + EDS + EBSD joint analysis.
The method comprises the following specific steps:
(1) firstly, preparing a metal material experimental sample for corrosion research by a conventional Electron Back Scattering Diffraction (EBSD) sample preparation technology;
(2) using a micro Vickers hardness tester to punch 3 hardness indentations on the surface of a sample, and selecting the clearest and complete indentation as a mark for positioning, tracking and observing;
(3) recording the position of the positioning indentation on the surface of the sample, shooting the non-corroded surface appearance of the positioning area of the sample through a Scanning Electron Microscope (SEM), obtaining the microstructure information of the area through an EBSD test, and obtaining the element composition information of the area through an energy spectrum test (EDS);
(4) creating a corrosive environment, and corroding the sample to be realized;
(5) taking out a sample, placing the sample in an SEM (scanning electron microscope) for observation, shooting the corrosion characteristics of the sample at the corrosion stage, and determining the element content of a corrosion product;
(6) repeating the steps (4) and (5) to obtain the material surface corrosion morphology and the time sequence data of the product;
(7) and covering the EBSD test result on the SEM topography photograph by using image processing software, taking the positioning indentation as an anchor point of the overlapping operation, and simultaneously combining the information of the topography and the components to realize the combined analysis of SEM + EDS + EBSD.
The following takes the corrosion of B10 cupronickel alloy pipe in seawater for a marine condenser as an example, and the method for locating, tracking and characterizing the present invention is explained in detail with reference to the accompanying drawings and the specific implementation mode:
(1) in order to research the corrosion problem of the B10 copper-nickel alloy pipe for the marine condenser soaked in static seawater, firstly preparing a B10 sample for an EBSD test, and specifically, cutting a sample with a proper size on the pipe wall in a linear manner; after inlaying, the surface is polished by five sand papers of 120#, 220#, 500#, 1000#, 2400 #; mechanically polishing with diamond spray polishing paste with particle size of 2.5 μm and 1.0 μm; performing electrolytic polishing in a polishing solution of 70% phosphoric acid and 30% absolute ethyl alcohol by using an 8V direct-current power supply; the residual stains are cleaned by distilled water and alcohol, and dried by a blower.
(2) Selecting a representative part on the surface of the sample, punching three hardness indentations on the surface of the sample by using a micro Vickers hardness tester, and selecting the clearest and complete indentation as a positioning mark.
(3) The surface topography of the area at the initial stage is photographed by using SEM, as shown in FIG. 1; raw ingredients were measured using EDS as shown in table 1; the grain orientation distribution map and the grain boundary characteristic distribution map in the vicinity of the positioning indentation are obtained by the EBSD test, as shown in fig. 2 and 3. The results of the unetched appearance, composition and microstructure of the sample in the positioning area are obtained through the tests.
TABLE 1 EDS measurement of original composition of test sample location area (weight percent/wt%)
| Element(s) | Ni | Fe | |
| Test results | |||
| 1 | 11.31 | 1.99 | 1.06 |
| Test results 2 | 11.16 | 1.98 | 1.07 |
| Test results 3 | 11.25 | 1.89 | 1.09 |
| Mean value of | 11.24 | 1.95 | 1.07 |
| Standard deviation of | 0.062 | 0.045 | 0.012 |
(4) The samples were left to soak in 3.5 wt.% NaCl solution for a period of time to simulate the static corrosion of the cupronickel tubes in real seawater, with the experimental solution being changed every 2 days in order to maintain the oxygen content of the corrosive medium.
(5) The sample after 1 day of soaking was taken out of the NaCl solution, washed with distilled water and alcohol to remove residual corrosive medium, dried and placed in the SEM. And (4) searching indentation marks of the sample through a sample stage system carried by the SEM, and performing identical appearance observation and composition test on the observed area according to the experimental conditions and the method in the step (3).
(6) The steps of soaking, positioning, tracking and observing are repeated to obtain a group of time sequence data of the surface corrosion morphology of the material sample, as shown in fig. 4, a corrosion morphology graph of the test sample after accumulated soaking for 7 days is obtained, and time sequence data of corrosion products are obtained, as shown in table 2.
TABLE 2 EDS measurements (weight percent/wt%) of different corrosion stages at test sample location areas
(7) And covering the grain orientation distribution map and the grain boundary characteristic distribution map obtained by the EBSD test on the SEM topography photograph by using Photoshop software, and taking the positioning indentation as an anchor point of the overlapping operation to obtain a positioning tracking characterization effect map of the test sample which is shown in figure 5 and is soaked for 7 days in an accumulated mode.
And comparing and analyzing the experimental results prolonged along with time, and simultaneously combining the time sequence data of morphology and components to realize the evolution rule of the microstructure of the B10 copper-nickel alloy pipe material in different corrosion stages by SEM + EDS + EBSD combined analysis. The following conclusions were made:
obvious corrosion of the sample occurs in 7 days of accumulated soaking, and relatively corrosion-resistant crystal grains exist, and the crystal orientation of the corrosion-resistant crystal grains is relatively concentrated near the <001> and <101> directions; no regular association of corrosion resistance with grain boundary type was found. The reason for this is probably that the crystal orientation is closely related to the corrosion potential, resulting in better corrosion resistance of the grains with higher corrosion potential.
After the sample is statically soaked, the corrosion product on the surface is particularly high in Fe-rich degree, high in Ni-rich degree and general in Mn-rich degree, and more O and Cl exist in the product; under the corrosion product film is the alloy matrix, with element content close to that of the original sample, the composition being primarily slightly Fe-rich and secondarily slightly Mn-rich. Filling Ni atoms into Cu during etching2O corrosion product film defects make the corrosion product film denser.
The method can obtain the corrosion characteristics of different stages by observing only one sample, can realize the effect of approximate in-situ test without using a special in-situ test instrument, can continuously observe the evolution process of the microstructure of the material at different corrosion stages in any corrosion environment, and expands the corrosion analysis from the whole material to the microscopic level.
The above embodiments are only used for illustrating but not limiting the technical solutions of the present invention, and although the above embodiments describe the present invention in detail, those skilled in the art should understand that: modifications and equivalents may be made thereto without departing from the spirit and scope of the invention and any modifications and equivalents may fall within the scope of the claims.
Claims (6)
1. A location tracking characterization method for corrosion research is characterized in that a micro Vickers hardness tester is used for punching hardness indentations on the surface of a sample as a mark for location tracking observation, the positions of the indentations on the surface of the sample are recorded, and the shape, components and microstructure of the sample which is not corroded in a location area are tested; repeating the process of taking out and retesting after the corrosion to obtain the corrosion appearance of the surface of the material and the time sequence data of the product; and finally, positioning, tracking and analyzing the microstructure by using image processing software and taking the indentation as an anchor point.
2. The method of claim 1, comprising the steps of:
(1) preparing a metal material experimental sample for corrosion research;
(2) manufacturing a hardness indentation on the surface of a sample by using a micro Vickers hardness tester as a mark for positioning, tracking and observing;
(3) recording the position of the positioning indentation on the surface of the sample, carrying out scanning electron microscope shooting on the surface of the sample to obtain the non-corroded surface appearance of the positioning area of the sample, carrying out electron back scattering diffraction test to obtain the microstructure information of the area, and carrying out energy spectrum test to obtain the element component information of the area;
(4) simulating a corrosion environment to corrode the sample;
(5) taking out a sample, observing the sample by using a scanning electron microscope, shooting the corrosion characteristics of the sample at the corrosion stage, and measuring the element content of a corrosion product by using an EDS (electronic discharge spectroscopy) test;
(6) repeating the steps (4) and (5) to obtain the surface corrosion morphology of the sample and the time sequence data of the product;
(7) and covering the electron back scattering diffraction test result on a scanning electron microscope morphology picture by using image processing software, taking the positioning indentation as an anchor point of overlapping operation, and simultaneously combining morphology and component information to realize the combined analysis of SEM + EDS + EBSD.
3. The method according to claim 2, wherein an electron back-scattering diffraction sample preparation technique is used to prepare the metal material experimental sample for corrosion research.
4. The method of location tracking characterization for corrosion research according to claim 3, wherein: when preparing a metal material experimental sample for corrosion research, obtaining a sample with a proper size by cutting; after inlaying, polishing the surface by five sand papers from coarse to fine; sequentially spraying diamond spraying polishing paste with the particle sizes of 2.5 mu m and 1.0 mu m for mechanical polishing; performing electrolytic polishing in a polishing solution of 70% phosphoric acid and 30% absolute ethyl alcohol by using an 8V direct-current power supply; washing residual stains with distilled water and absolute ethyl alcohol in sequence, and drying by using a blower.
5. The method of location tracking characterization for corrosion research according to claim 2, wherein: several hardness indentations were made on the sample surface, of which the clearest, intact 1 was taken as a positioning mark.
6. The method of location tracking characterization for corrosion research according to claim 2, wherein: and covering the grain orientation distribution map and the grain boundary characteristic distribution map obtained by the EBSD test on the SEM topography picture by using image processing software and taking the positioning indentation as an anchor point of the overlapping operation.
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Cited By (2)
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| CN117250216A (en) * | 2023-11-17 | 2023-12-19 | 北京首钢股份有限公司 | Analysis method of alloyed hot dip galvanized steel sheet |
| CN117250216B (en) * | 2023-11-17 | 2024-04-26 | 北京首钢股份有限公司 | Analysis method of alloyed hot dip galvanized steel sheet |
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