CN112501681B - Preparation method of electrochemical polishing sample of high-low carbon martensitic stainless steel - Google Patents
Preparation method of electrochemical polishing sample of high-low carbon martensitic stainless steel Download PDFInfo
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- 238000005498 polishing Methods 0.000 title claims abstract description 47
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 19
- 229910001105 martensitic stainless steel Inorganic materials 0.000 title claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000003792 electrolyte Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 238000005520 cutting process Methods 0.000 claims abstract description 4
- 238000007517 polishing process Methods 0.000 claims abstract description 4
- 238000004519 manufacturing process Methods 0.000 claims abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 229940028356 diethylene glycol monobutyl ether Drugs 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 claims description 3
- 238000004806 packaging method and process Methods 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 244000137852 Petrea volubilis Species 0.000 claims description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims 1
- 239000002390 adhesive tape Substances 0.000 claims 1
- 229910052804 chromium Inorganic materials 0.000 claims 1
- 239000011651 chromium Substances 0.000 claims 1
- 239000010941 cobalt Substances 0.000 claims 1
- 229910017052 cobalt Inorganic materials 0.000 claims 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims 1
- 229910052750 molybdenum Inorganic materials 0.000 claims 1
- 239000011733 molybdenum Substances 0.000 claims 1
- 229910052759 nickel Inorganic materials 0.000 claims 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims 1
- 229910052721 tungsten Inorganic materials 0.000 claims 1
- 239000010937 tungsten Substances 0.000 claims 1
- 229910052720 vanadium Inorganic materials 0.000 claims 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 14
- 238000000034 method Methods 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 7
- 238000001887 electron backscatter diffraction Methods 0.000 abstract description 6
- 229910001220 stainless steel Inorganic materials 0.000 abstract description 5
- 238000004458 analytical method Methods 0.000 abstract description 4
- 239000010935 stainless steel Substances 0.000 abstract description 4
- 238000007789 sealing Methods 0.000 abstract 1
- 229910000831 Steel Inorganic materials 0.000 description 11
- 239000010959 steel Substances 0.000 description 11
- 238000009826 distribution Methods 0.000 description 6
- 229910000734 martensite Inorganic materials 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 229910001566 austenite Inorganic materials 0.000 description 3
- 238000003384 imaging method Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 2
- 238000010884 ion-beam technique Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 229910020630 Co Ni Inorganic materials 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910001039 duplex stainless steel Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000000992 sputter etching Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a preparation method of a high-low carbon martensitic stainless steel electrochemical polishing sample, and belongs to the technical field of material analysis and test. The method of the invention comprises the following steps: cutting a sample to be tested from an original sample by using linear cutting, polishing the cut sample step by using water-abrasive paper with different meshes, polishing the cut sample on a polishing machine until the cut sample is smooth and has no scratch, and cleaning and drying the cut sample; sealing the edge of the polished sample by using colorless nail polish to expose the part to be polished; after the nail polish is semi-dried, the sample is fixed on the outer side wall of the electrolytic cell, and electrochemical polishing is carried out. The electrolytic polishing method for stainless steel is quite stable in electrolytic polishing of stainless steel by using the electrolyte, the polishing process can be carried out at normal temperature without manufacturing a low-temperature environment, the polished surface of the polished sample is good in flatness, the residual stress on the surface of the sample can be well removed, and the analysis rate is high in the EBSD test process.
Description
Technical Field
The invention relates to a preparation method of an electrochemical polishing sample of high-low carbon martensitic stainless steel, and belongs to the technical field of material analysis and test.
Background
Other phases than the matrix phase often exist in martensitic stainless steels, including austenite, carbides, and intermetallic compounds, among others. These phases are dispersed between matrix phases and can have important effects on the properties of materials mechanics, corrosion, etc. The phases in steel materials can now be analyzed by electron microscopy, and in particular matrix organization and carbide secondary phases can be distinguished easily using back-scattered electron imaging. Since the size and distribution of the second phase in the steel material have a great influence on the mechanical properties of the material, effective statistics on the size, distribution and the like of the second phase in the steel are often required in the research. And once the metallographic specimen is corroded by the corrosive liquid, part of the second phase particles can fall off, so that the statistical result is inaccurate, and if the specimen is polished on a polishing machine only, polishing scratches and polishing pits can be left, so that the observation is affected.
When researching duplex stainless steel, it is often necessary to study the crystal structure, orientation relation, interface relation between two phases, and the like of the phases by an electron back scattering diffraction technique. The electron back scattering diffraction test has extremely high requirements on the sample, and the sample surface is required to be flat and free of residual stress. Such sample processing includes mechanical shock polishing, chemical etching polishing, ion etching, focused ion beam in situ processing, and the like. However, these methods have corresponding disadvantages, such as vibration polishing can generate residual stress on the surface of the sample, so that the resolution ratio is not high in the test process; chemical polishing tends to produce selective corrosion, which removes some of the phases and interfaces that need to be observed, from affecting the test results, while focused ion beam processing (FIB), while producing the best samples, is inefficient and expensive.
Electrolytic polishing is a cheaper and simpler sample preparation method. For steel materials, the formulation of the electrolyte is generally that ethanol and perchloric acid are mixed in a certain proportion, and polishing is often performed at a low temperature because perchloric acid is a strong oxidizing acid, which results in complicating the polishing apparatus. In addition, the typical electropolishing apparatus is one in which the sample is completely immersed in the electrolyte, which limits the apparatus to the size of the sample, especially the preparation of the sample preparation polish after encapsulation with the epoxy resin; the invention provides a simple, efficient and stable electrochemical polishing method for a low-carbon martensitic stainless steel sample by adopting an improved electrolyte and a polishing device.
Disclosure of Invention
The invention aims to provide a method for electrochemical polishing of a low-carbon martensitic stainless steel sample, which has the advantages of simple process, high efficiency, good flatness of the obtained sample, effective removal of residual stress on the surface of the sample, and quick and mass preparation of the electrochemical polished sample; the sample prepared by the method not only can carry out the size and distribution statistics of carbide and the pretreatment of the sample pitting test, but also can carry out EBSD observation, and the preparation process specifically comprises the following steps:
(1) A Bao Kuaizhuang sample is cut from high-low carbon martensitic stainless steel by using a wire cutting machine, the sample is stuck on a flat iron block, and the sample is polished step by step in water-abrasive paper with different meshes and polished on a polishing machine until the surface is bright and free of scratches.
(2) Immersing the iron block adhered with the thin block-shaped sample in the step (1) in acetone, carrying out ultrasonic vibration until the thin sheet naturally drops, taking out, washing and drying.
(3) Packaging the polished edge of the sample with colorless nail polish to expose the region to be corroded in the middle of the sample, and adhering the thin block to the outer side wall of an electrolytic cell of an electrochemical polishing device when the nail polish is semi-dry, wherein small holes are correspondingly formed in the side wall of the electrolytic cell, and the region to be corroded is just exposed at the small holes; the test pieces were then fixed using a hole-digging double sided tape.
(4) Pouring electrolyte, contacting the electrolyte with the to-be-corroded area, connecting positive and negative electrode wires, and regulating voltage to switch on a power supply; the electrolyte comprises the following components: in every 1500ml of solution, 1063ml of absolute ethyl alcohol, 152ml of diethylene glycol monobutyl ether, 167ml of distilled water and 118ml of perchloric acid, the voltage is 15-20V in the polishing process, the current is 60-80mA, and the polishing time is 75s.
(5) And (3) washing the sample subjected to electrochemical polishing by using deionized water to remove electrolyte, cleaning the sample in alcohol and deionized water, and drying and preserving the sample.
Preferably, the number of sandpaper used in step (2) of the present invention is 600, 800, 1000, 1500, 2000, 3000 mesh, respectively.
The invention has the beneficial effects that:
(1) The device is simple in equipment, can be realized only by a plastic beaker and a direct-current conversion power supply, can be used for electrolytic polishing of samples with various sizes, is packaged by using nail polish, has no pollution to the surfaces of the samples, is well removed after a corrosion experiment is finished, and is quite short in solidification time, so that the solidification time is greatly shortened, and the flatness of the obtained samples is quite good; the epoxy encapsulated samples may also be encapsulated with nail polish.
(2) The electrolytic polishing method for stainless steel is quite stable in electrolytic polishing of stainless steel by using the electrolyte, the polishing process can be carried out at normal temperature without manufacturing a low-temperature environment, the polished surface of the polished sample is good in flatness, the residual stress on the surface of the sample can be well removed, and the analysis rate is high in the EBSD test process.
Drawings
FIG. 1 is a front view of an electropolishing apparatus in accordance with the present invention;
FIG. 2 is a side view of an electropolishing apparatus in accordance with the present invention;
FIG. 3 is a photograph showing the second phase distribution obtained by back-scattered electron imaging under a field emission scanning electron microscope after electrochemical polishing of the low carbon martensitic bearing steel described in example 1;
FIG. 4 is a pitting morphology induced by inclusions in the steel after corrosion resistance testing of the low carbon super martensitic stainless steel described in example 1;
Fig. 5 is an EBSD picture of the martensite and the contravariant austenite of the low-carbon super martensitic stainless steel described in example 1.
Detailed Description
The invention will be described in further detail with reference to the drawings and the specific embodiments, but the scope of the invention is not limited to the description.
The electrolytic polishing device used in the embodiment of the invention is shown in figures 1 and 2, and comprises an electrolytic tank, a platinum sheet and a power supply, wherein the side wall of the electrolytic tank is provided with a small hole for adhering a sample.
Table 1 shows the composition of the test steel (wt.%)
TABLE 1
| C | Cr | Mo | Co | Ni | V | W | Fe |
| 0.1～0.15 | 13～15 | 4～5 | 12～13 | 1.5～2.5 | 0.5～1 | 0.5～1 | Bal. |
The preparation method of the low-carbon martensitic stainless bearing steel sample specifically comprises the following steps:
(1) A thin block specimen having a gauge of 10X 10mm and a thickness of 2mm was cut from the high and low carbon martensitic stainless steel using a wire cutter.
(2) And (3) adhering the sample obtained in the step (1) to a flat iron block, polishing the sample step by using water-grinding sand paper with 600, 800, 1000, 1500, 2000 and 3000 meshes respectively, and polishing the sample on a polishing machine until the sample is bright and has no scratches.
(3) Immersing the iron block adhered with the thin block sample in the step (2) in acetone, carrying out ultrasonic vibration until the thin sheet naturally drops, taking out, washing and drying.
(4) Packaging the polished edge of the sample with colorless nail polish to expose the region to be corroded in the middle of the sample, adhering the thin block to the outer side wall of an electrolytic cell of the electrochemical polishing device when the nail polish is semi-dry, and correspondingly arranging small holes (the diameter of the holes is the same as the exposed region of the sample) on the side wall of the electrolytic cell, wherein the small holes just expose the region to be corroded; the test pieces were then fixed using a hole-digging double sided tape.
(6) And (5) switching on a power supply, regulating voltage and performing electrochemical polishing.
① The formula of the double spray liquid in the step (6) is as follows: in every 1500ml of solution, 1063ml of absolute ethyl alcohol, 152ml of diethylene glycol monobutyl ether, 167ml of distilled water and 118ml of perchloric acid are added.
② The parameters of the electrolysis double spraying in the step (6) are as follows: the voltage is 15-20V, the current is ensured to be 60-80mA, and the polishing time is 75s.
(7) And (3) ultrasonically cleaning the sample obtained in the step (6) in absolute ethyl alcohol twice, and then drying and preserving.
FIG. 3 is a photograph showing the second phase distribution obtained by back-scattered electron imaging under a field emission scanning electron microscope after electrochemical polishing of the low carbon martensitic bearing steel described in example 1; FIG. 4 is a pitting morphology induced by inclusions in the steel after corrosion resistance testing of the low carbon super martensitic stainless steel described in example 1; fig. 5 is an EBSD picture of the martensite and the contravariant austenite of the low-carbon super martensitic stainless steel described in example 1. The image can be seen that the back scattering electron image under the field emission scanning electron microscope is clear, the surface evenness of the sample is good, and the second phase distribution is obvious; compared with the common mechanical grinding and polishing, the method has small influence on inclusions in steel and high resolution in an EBSD test.
Claims (2)
1. The preparation method of the electrochemical polishing sample of the low-carbon martensitic stainless steel is characterized by comprising the following steps of:
(1) Cutting Bao Kuaizhuang a sample from low-carbon martensitic stainless steel by using a wire cutting machine, adhering the sample to a flat iron block, polishing step by step in water-abrasive paper with different meshes, and polishing on a polishing machine until the surface is bright and free of scratches;
The low-carbon martensitic stainless steel comprises the following components in percentage by weight: carbon: 0.1% -0.15%, chromium: 13% -15%, molybdenum: 4% -5%, cobalt: 12% -13%, nickel: 1.5% -2.5%, vanadium: 0.5% -1%, tungsten: 0.5% -1%, and the balance being iron;
(2) Immersing the iron block adhered with the thin block-shaped sample in the step (1) in acetone, carrying out ultrasonic vibration until the thin sheet naturally drops, taking out, washing and drying;
(3) Packaging the polished edge of the sample with colorless nail polish to expose the region to be corroded in the middle of the sample, and adhering the thin block to the outer side wall of an electrolytic cell of an electrochemical polishing device when the nail polish is semi-dry, wherein small holes are correspondingly formed in the side wall of the electrolytic cell, and the region to be corroded is just exposed at the small holes; then fixing the sample by using a hole digging double faced adhesive tape;
(4) Pouring electrolyte, contacting the electrolyte with the to-be-corroded area, connecting positive and negative electrode wires, and regulating voltage to switch on a power supply; the electrolyte comprises the following components: in every 1500ml of solution, 1063ml of absolute ethyl alcohol, 152ml of diethylene glycol monobutyl ether, 167ml of distilled water and 118ml of perchloric acid, the voltage is 15-20V in the polishing process, the current is 60-80mA, and the polishing time is 75s;
(5) And (3) washing the sample subjected to electrochemical polishing by using deionized water to remove electrolyte, cleaning the sample in alcohol and deionized water, and drying and preserving the sample.
2. The method of manufacturing according to claim 1, characterized in that: the number of sand paper used in the step (1) is 600, 800, 1000, 1500, 2000 and 3000 meshes respectively.
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| CN113670699A (en) * | 2021-08-18 | 2021-11-19 | 西安建筑科技大学 | Ferrite heat-resistant stainless steel EBSD sample and preparation method thereof |
| CN115406918A (en) * | 2022-07-18 | 2022-11-29 | 成都先进金属材料产业技术研究院股份有限公司 | Martensite high-strength steel EBSD sample preparation method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101736393A (en) * | 2008-11-06 | 2010-06-16 | 上海工程技术大学 | Fixing device of electrolytic polishing sample |
| CN106435709A (en) * | 2016-10-27 | 2017-02-22 | 南京钢铁股份有限公司 | Electrolytic polishing device allowing real-time observation of polishing effect and method thereof |
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| CN103398892B (en) * | 2013-08-23 | 2015-05-13 | 北京科技大学 | Method for displaying prior austenite crystal boundary of martensite heat-resistant steel |
| CN111910244B (en) * | 2020-07-07 | 2023-05-05 | 甘肃酒钢集团宏兴钢铁股份有限公司 | Method for preparing dual-phase stainless steel EBSD sample by pulse wave electrolytic polishing |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101736393A (en) * | 2008-11-06 | 2010-06-16 | 上海工程技术大学 | Fixing device of electrolytic polishing sample |
| CN106435709A (en) * | 2016-10-27 | 2017-02-22 | 南京钢铁股份有限公司 | Electrolytic polishing device allowing real-time observation of polishing effect and method thereof |
Non-Patent Citations (1)
| Title |
|---|
| Hydrogen embrittlement in heat affected zone of a welded sheet of precipitation hardening martensitic stainless steel;S.SAHAWAT等;2009国际博士研讨会论文集;第234-242页 * |
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