CN111458208A - Display method for distinguishing cold-rolled annealed multiphase steel structure - Google Patents
Display method for distinguishing cold-rolled annealed multiphase steel structure Download PDFInfo
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- CN111458208A CN111458208A CN202010218519.2A CN202010218519A CN111458208A CN 111458208 A CN111458208 A CN 111458208A CN 202010218519 A CN202010218519 A CN 202010218519A CN 111458208 A CN111458208 A CN 111458208A
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- 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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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
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Abstract
The invention discloses a display method for distinguishing cold-rolled annealed multiphase steel structures, which comprises the following steps: (1) coarse grinding; (2) fine grinding; (3) polishing; (4) corrosion of a first reagent: rapidly wiping the polished surface of the sample for 1-2 seconds by using a first reagent, wherein the first reagent is nital with the volume concentration of 2%; (5) and (3) corrosion of a reagent II: directly immersing the sample corroded by the first reagent into the second reagent for coloring the surface of the sample, wherein the coloring time is 10-15 seconds, and the second reagent is 8-12gNa2S2O5And 80-120ml of distilled water; (6) and (3) sample detection: and washing and drying the sample corroded by the reagent II by absolute ethyl alcohol, and observing the sample under a color optical microscope. The method has the advantages of simple operation method, easy mastering, avoidance of the processes of repeated polishing and corrosion of the sample, clean surface, clear and recognizable tissue, suitability for field use and reasonable control of the sample and the production fieldThe manufacturing process parameters and the guarantee of the product performance can play important roles.
Description
Technical Field
The invention belongs to the technical field of metallurgy, and particularly relates to a display method for distinguishing tissues in cold-rolled annealed multi-phase steel.
Background
In order to reduce the weight of the vehicle body without impairing the safety performance of the vehicle body, cold-rolled annealed advanced high-strength steels, such as dual-phase steels (ferrite + martensite), transformation induced plasticity steels (ferrite + bainite + retained austenite) and quench-distributed steels in third-generation automotive steels (ferrite + bainite + retained austenite + martensite), are increasingly used in the manufacture of automotive vehicle bodies, and because these steel grades have good strength and form-fit, are suitable for machining complicated parts, and are increasingly used in automotive parts, particularly structural parts and reinforcing parts.
At present, in order to distinguish phases in multi-phase steel and relative proportions of the phases, the phases in the steel can be effectively distinguished and the phase proportions can be determined by comprehensively utilizing a plurality of methods such as an optical microscope, a scanning electron microscope and the like sometimes in combination with a projection electron microscope and X-ray diffraction and the like after the nitric acid alcohol solution is corroded, the method is long in time and high in cost, and particularly under a transmission electron microscope, due to the fact that an observation visual field is too small, multi-field observation is needed, the workload is too large, and the cost is high. At present, corrosion methods can be used for distinguishing ferrite and martensite in dual-phase steel, such as a patent dual-phase steel color metallographic staining agent and a color display method thereof, but a display method capable of rapidly and accurately distinguishing a multi-phase steel structure is lacked.
Disclosure of Invention
The invention aims to solve the problem of overcoming the defects in the existing corrosion method and provide a metallographic structure display method which is simpler to operate and can clearly display and distinguish each phase in steel.
The problem to be solved by the present invention is solved by the following etching method:
a display method for distinguishing cold-rolled annealed multiphase steel structures comprises the following steps:
(1) coarse grinding: after embedding the sample, carrying out coarse grinding and flat grinding on a plane polishing machine;
(2) fine grinding: sequentially polishing the rough-ground test sample on 280# -320# -400# -600# -800# sand paper;
(3) polishing: polishing the panne polishing cloth with diamond polishing paste with particles of 1.0-2.5um to form a mirror surface without scratches;
(4) corrosion of a first reagent: rapidly wiping the polished surface of the sample for 1-4 seconds by using a first reagent, wherein the first reagent is nital with the volume concentration of 2-5%;
(5) and (3) corrosion of a reagent II: directly immersing the sample corroded by the first reagent into the second reagent for coloring the surface of the sample, wherein the coloring time is 10-15 seconds, and the second reagent is prepared from 8-12gNa2S2O5And 80-120ml of distilled water;
(6) and (3) sample detection: and washing the sample corroded by the reagent II with absolute ethyl alcohol, drying the sample by blowing, and observing each phase in the tissue under a color optical microscope.
In the above display method for distinguishing the structure of the cold-rolled annealed multiphase steel, the reagent II is prepared in step (5).
According to the display method for distinguishing the cold-rolled annealed multi-phase steel structure, the reagent II in the step (5) can be prepared and then placed in a sealed opaque reagent bottle for use within a week.
The invention improves the operation method for distinguishing phases in the current two-phase and multi-phase high-strength steel structure. The corrosion method needs two corrosion reagents to be used in sequence, wherein the reagent I is low-concentration nital, and the reagent II is Na2S2O5And distilled water. After polishing, a sample is quickly corroded by a first reagent; then quickly immerging into the second reagent to color the surface,and then washing the surface of the corrosion sample by using absolute ethyl alcohol, and drying by blowing to obtain a structure with clear phases.
The phases in the steel can be distinguished under a color optical microscope through the color difference, wherein ferrite is grey white, residual austenite is white, martensite is black, and bainite is dark gray.
The method is simple in operation and easy to master, avoids the processes of repeated polishing and corrosion of the sample, obtains a clean surface, has clear and recognizable tissues, is very suitable for field use, and plays an important role in reasonably controlling process parameters and ensuring product performance in a production field.
Description of the drawings:
fig. 1 is a picture of a structure etched with a 4% nital solution.
Fig. 2 is a photograph of a structure etched with an L epera etchant.
FIG. 3 is a photograph of a structure etched with the etchant of the present invention.
Detailed Description
The method is obtained by improving the corrosion test of the cold-rolled annealed multiphase steel, does not need to repeatedly polish and corrode a sample, does not need strict reagent proportioning, and quickly wipes the sample for 1 to 4 seconds by using a 2 to 5 percent nitric acid alcohol solution (reagent I); direct immersion of the solution in a bath of 8-12g Na2S2O5And (3) coloring the surface of the sample in a solution (reagent II) mixed with 80-120ml of distilled water for 10-15s, washing the surface of the corroded sample by absolute ethyl alcohol, and drying the corroded sample by blowing to observe the sample. The action mechanism is as follows: the polished sample is quickly wiped by using a reagent I, and the following reaction occurs: fe +2H+-Fe+++H2Then directly immerging into the second reagent, the residual nitric acid on the surface can promote Na in the second reagent2S2O5Decomposition occurs to release SO2、H2S and H2Fe generated by the first etching++Can be reacted with H2S reacts to form FeS precipitate phase, which is used for coloring corrosion surface and finally usedAnd washing the surface with water and ethanol, and drying the surface to observe tissues.
In order to ensure the corrosion effect, the second reagent is preferably prepared and used immediately, and can also be placed in a sealed opaque reagent bottle for use within one week.
The following specific examples are given:
example 1
Preparing a metallographic specimen from a multiphase steel (C0.22, Mn 2.27, S0.002, P0.019, Si 1.71, Als 0.048, Nb 0.048, Ti0.056 and Cr 0.038) material; after the samples are inlaid, the samples are subjected to rough grinding and smoothing on a plane grinder, then the samples are sequentially ground on 280# -320# -600# -800# abrasive paper, diamond polishing paste with the particle size of 2.5um is used for polishing on velveteen polishing cloth, and no scratch is formed on the polished mirror surface; rapidly wiping the polished surface of the sample for 2 seconds by using a first reagent, wherein the first reagent is nitric acid alcohol with the volume concentration of 2%; directly immersing the sample corroded by the first reagent into the second reagent for coloring the surface of the sample, wherein the coloring time is 10 seconds, and the second reagent is 100mlH2O+10gNa2S2O5A solution; and washing the sample corroded by the reagent II with absolute ethyl alcohol, drying the sample by blowing, and observing each phase in the tissue under a color optical microscope.
Example 2
Preparing a metallographic specimen from a multiphase steel (C0.21, Mn 2.26, S0.002, P0.019, Si 1.68, Als 0.048, Nb 0.046, Ti0.054 and Cr 0.038) material; after the samples are inlaid, the samples are subjected to rough grinding and smoothing on a plane grinder, then the samples are sequentially ground on 280# -320# -600# -800# abrasive paper, diamond polishing paste with the particle size of 1.0um is used for polishing on velveteen polishing cloth, and no scratch is formed on the polished mirror surface; rapidly wiping the polished surface of the sample for 1 second by using a first reagent, wherein the first reagent is nitric acid alcohol with the volume concentration of 4%; directly immersing the sample corroded by the first reagent into the second reagent for coloring the surface of the sample, wherein the coloring time is 12 seconds, and the second reagent is 80mlH2O+12gNa2S2O5A solution; and washing the sample corroded by the reagent II with absolute ethyl alcohol, drying the sample by blowing, and observing each phase in the tissue under a color optical microscope.
Example 3
Preparing a metallographic specimen from a multiphase steel (C0.20, Mn 1.95, S0.002, P0.011, Si 1.28, Als 0.038, Nb 0.004, Ti0.004 and Cr 0.018) material; after the samples are inlaid, the samples are subjected to rough grinding and smoothing on a plane grinder, then the samples are sequentially ground on 280# -320# -600# -800# abrasive paper, diamond polishing paste with the particle size of 2.0um is used for polishing on velveteen polishing cloth, and no scratch is formed on the polished mirror surface; rapidly wiping the polished surface of the sample for 4 seconds by using a first reagent, wherein the first reagent is 5% nitric acid alcohol in volume concentration; directly immersing the sample corroded by the first reagent into the second reagent for coloring the surface of the sample, wherein the coloring time is 14 seconds, and the second reagent is 120mlH2O+8gNa2S2O5A solution; and washing the sample corroded by the reagent II with absolute ethyl alcohol, drying the sample by blowing, and observing each phase in the tissue under a color optical microscope.
Claims (4)
1. A display method for distinguishing a cold-rolled annealed multi-phase steel structure is characterized in that: the method comprises the following steps:
(1) coarse grinding: after embedding the sample, carrying out coarse grinding and flat grinding on a plane polishing machine;
(2) fine grinding: polishing the test sample after coarse grinding by using sand paper;
(3) polishing: polishing the panne polishing cloth with diamond polishing paste with particles of 1.0-2.5um to form a mirror surface without scratches;
(4) corrosion of a first reagent: rapidly wiping the polished surface of the sample for 1-4 seconds by using a first reagent, wherein the first reagent is nital with the volume concentration of 2-5%;
(5) and (3) corrosion of a reagent II: directly immersing the sample corroded by the first reagent into the second reagent for coloring the surface of the sample, wherein the coloring time is 10-15 seconds, and the second reagent is prepared from 8-12gNa2S2O5And 80-120ml of distilled water;
(6) and (3) sample detection: and washing the sample corroded by the reagent II with absolute ethyl alcohol, drying the sample by blowing, and observing each phase in the tissue under a color optical microscope.
2. Display method for differentiating the structure of cold-rolled annealed multi-phase steel according to claim 1, characterized in that: and (2) polishing the rough-ground test sample on 280# -320# -400# -600# -800# sandpaper in sequence.
3. Display method for differentiating the structure of cold-rolled annealed multi-phase steel according to claim 1, characterized in that: and (5) preparing the reagent II in situ.
4. Display method for differentiating the structure of cold-rolled annealed multi-phase steel according to claim 1, characterized in that: and (5) preparing the reagent II, and putting the prepared reagent II into a sealed light-tight reagent bottle for use within a week.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1167257A (en) * | 1997-02-27 | 1997-12-10 | 宝山钢铁(集团)公司 | Method for indicating metallographic texture of gap-free atom cold rolled annealed steel |
| JP2007204772A (en) * | 2006-01-31 | 2007-08-16 | Jfe Steel Kk | Coloring etchant for observing microstructure of steel, and etching method |
| CN101984334A (en) * | 2010-10-29 | 2011-03-09 | 河北钢铁股份有限公司唐山分公司 | Method for displaying metallurgical structure of ultralow-carbon cold roll annealed interstitial-free steel |
| CN107957420A (en) * | 2017-11-21 | 2018-04-24 | 攀钢集团攀枝花钢铁研究院有限公司 | The assay method of middle carbon TRIP steel retained austenites |
-
2020
- 2020-03-25 CN CN202010218519.2A patent/CN111458208A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1167257A (en) * | 1997-02-27 | 1997-12-10 | 宝山钢铁(集团)公司 | Method for indicating metallographic texture of gap-free atom cold rolled annealed steel |
| JP2007204772A (en) * | 2006-01-31 | 2007-08-16 | Jfe Steel Kk | Coloring etchant for observing microstructure of steel, and etching method |
| CN101984334A (en) * | 2010-10-29 | 2011-03-09 | 河北钢铁股份有限公司唐山分公司 | Method for displaying metallurgical structure of ultralow-carbon cold roll annealed interstitial-free steel |
| CN107957420A (en) * | 2017-11-21 | 2018-04-24 | 攀钢集团攀枝花钢铁研究院有限公司 | The assay method of middle carbon TRIP steel retained austenites |
Non-Patent Citations (3)
| Title |
|---|
| CHANG GIL LEE等: "Effects of volume fraction and stability of retained austenite on formability in a 0.1C–1.5Si–1.5Mn–0.5Cu TRIP-aided cold-rolled steel sheet", 《MATERIALS SCIENCE AND ENGINEERING》 * |
| 徐海卫等: "基于动态相变的细晶双相低碳钢组织控制", 《金属学报》 * |
| 谷秀锐等: "彩色金相在显微组织分析中的应用", 《理化检验》 * |
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Application publication date: 20200728 |