CN114791456A - Lossless and in-situ detectable method for predicting impact toughness change trend of Cr13 super stainless steel - Google Patents
Lossless and in-situ detectable method for predicting impact toughness change trend of Cr13 super stainless steel Download PDFInfo
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- CN114791456A CN114791456A CN202111069220.6A CN202111069220A CN114791456A CN 114791456 A CN114791456 A CN 114791456A CN 202111069220 A CN202111069220 A CN 202111069220A CN 114791456 A CN114791456 A CN 114791456A
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- 238000000034 method Methods 0.000 title claims abstract description 22
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 20
- 239000010935 stainless steel Substances 0.000 title claims abstract description 20
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 12
- 238000012360 testing method Methods 0.000 claims abstract description 58
- 238000004458 analytical method Methods 0.000 claims abstract description 13
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 claims description 13
- 230000007423 decrease Effects 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000003792 electrolyte Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 229940116357 potassium thiocyanate Drugs 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 244000137852 Petrea volubilis Species 0.000 claims 1
- 230000003247 decreasing effect Effects 0.000 claims 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 claims 1
- 229910001105 martensitic stainless steel Inorganic materials 0.000 abstract description 22
- 238000001514 detection method Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000032683 aging Effects 0.000 abstract description 2
- 238000005496 tempering Methods 0.000 abstract description 2
- 238000011282 treatment Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 25
- 239000000243 solution Substances 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 6
- 238000001453 impedance spectrum Methods 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000002161 passivation Methods 0.000 description 3
- 230000004075 alteration Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000157 electrochemical-induced impedance spectroscopy Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910000734 martensite Inorganic materials 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
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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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Abstract
The invention provides a method for predicting the impact toughness change trend of Cr13 super stainless steel by nondestructive and in-situ detection, which comprises the step of carrying out electrochemical impedance analysis test on a test sample to obtain the impact toughness of the test sample after the open-circuit potential is stabilized and a charge transfer resistance R corresponding to the impact toughness t (ii) a By charge transfer resistance R t And the impact toughness of the test sample, and predicting the impact toughness change trend of Cr13 super stainless steel. The method utilizes an electrochemical impedance technology to predict the impact toughness change trend of Cr13 super martensitic stainless steel, particularly Cr13 super martensitic stainless steel after tempering or long-time aging treatment, and the method predicts the charge transfer resistance R t As a prediction index, carbide and other precipitated phases in Cr13 super martensitic stainless steel are detected, and the change of the impact toughness of the material is evaluated, so that the safety of corresponding production is guided.
Description
Technical Field
The invention relates to the technical field of stainless steel electrochemical testing, in particular to a method for predicting the impact toughness change trend of Cr13 super stainless steel in a nondestructive and in-situ detection manner.
Background
The Cr13 super martensitic stainless steel has higher strength and hardness and good corrosion resistance, and has wider application in the fields of petroleum pipelines, oceans, nuclear industry and the like. However, during long-term aging and tempering treatment or at the welding seam of the stainless steel, Cr-rich carbide is easily precipitated, which can reduce the mechanical property and corrosion resistance of Cr13 super martensitic stainless steel, and particularly, when the carbide is coarsened along grain boundaries, the ductility and toughness of the material are obviously reduced, thus causing accidents. Therefore, it is important to detect the precipitated phase 000 such as carbide in the Cr13 super martensitic stainless steel.
The traditional carbide analysis method is a Scanning Electron Microscope (SEM) method, a Transmission Electron Microscope (TEM) method and other methods, and the methods have high requirements on equipment, samples and personnel, can be generally carried out only in a scientific laboratory and are limited to microscopic qualitative or semi-quantitative detection, so that macroscopic quantitative detection of carbides in stainless steel cannot be realized.
Disclosure of Invention
The invention overcomes the defects in the prior art, the existing carbide analysis method can not realize macroscopic quantitative detection of carbide in stainless steel, and provides a method for predicting the impact toughness change trend of Cr13 super stainless steel, which can not be damaged and can be detected in situ t As a prediction index, Cr13 super martensitic stainless steel was examined for precipitated phases such as carbide and the impact toughness of the material was evaluatedAnd changing to guide the safe operation of corresponding production.
The purpose of the invention is realized by the following technical scheme.
A method for predicting the impact toughness change trend of Cr13 super stainless steel without damage and capable of in-situ detection is carried out according to the following steps:
In the step 1, connecting a lead to the back of the test surface of the sample to be tested, sealing the back into epoxy resin, and exposing the test surface of the sample to be tested only to ensure that the area of the test surface of the sample to be tested is equal to the exposed area of the sample to be tested;
in the step 1, grinding the test surface of a sample to be tested to 2000 meshes from coarse to fine by using SiC abrasive paper, mechanically polishing, washing by using deionized water and absolute ethyl alcohol, and drying to obtain a test sample;
in step 1, a test sample is placed in a mixed electrolyte aqueous solution for electrochemical impedance analysis test, wherein in the mixed electrolyte aqueous solution, the mass percent of sulfuric acid is 5%, and the mass percent of potassium thiocyanate is 0.02%;
in step 1, after the open circuit potential is stabilized, an electrochemical impedance analysis test is carried out at the potential, and the test frequency is 10 5 -10 -2 Hz, the test amplitude is 10 mV;
the resistance of the carbide Cr-poor region is much lower than that of the carbide non Cr-poor region, so R t The magnitude of (A) is mainly determined by the resistance of the carbide Cr-poor region, i.e. the more severe the carbide Cr-poor region is, the R t The lower the value, i.e. R t The smaller the tendency for the impact toughness of the test specimen to decrease, the greater the need for safety protection or replacement of the test specimen.
In practical application, can be usedObtaining R of the tested sample material under a certain condition through the over-control variable t When fitting the obtained R t When the value is lower than the warning value, the impact toughness of the test sample material is sharply reduced; in the examples when R t Less than 351.9 (omega cm) 2 ) The impact toughness of Cr13 super martensitic stainless steel decreases sharply, so that under such conditions the value can be defined as the warning value for the impact toughness of Cr13 super martensitic stainless steel, when R is t Below this value, the material runs the risk of brittle fracture under impact load and requires replacement or other corresponding measures for protection.
The beneficial effects of the invention are as follows: the Cr13 super martensitic stainless steel sample is at 5% H 2 SO 4 Carrying out electrochemical impedance test in electrolyte solution of + 0.02% KSCN, fitting impedance spectrum with fitting software to obtain parameters with practical physical significance, and using charge transfer resistor R t The change of the impact toughness of the Cr13 super martensitic stainless steel is predicted as a new index; KSCN is a depolarizer which can locally destroy the passive film, and its carbide and its adjacent region are the weak regions of passive film, so it is more easily destroyed in corrosion process t The method can be used for rapidly, quantitatively and nondestructively predicting the change of the impact toughness of the Cr13 super martensitic stainless steel in an in-situ detection manner and guiding the safe production.
Drawings
FIG. 1 shows that the Cr13 super martensitic stainless steel after different heat treatments in the hot rolled state samples are at 5 wt.% H 2 SO 4 A Nyquist plot in +0.02 wt.% KSCN solution;
FIG. 2 shows Cr13 super martensitic stainless steel after different heat treatments in the hot rolled state at 5 wt.% H 2 SO 4 +0.02 wt.% Bode plot in KSCN solution;
FIG. 3 is a Cr13 super martensitic stainless steel solution treated specimen at 5 wt.% H after various heat treatments 2 SO 4 A Nyquist plot in +0.02 wt.% KSCN solution;
FIG. 4 is a Cr13 super martensitic stainless steel solution treated specimen at 5 wt.% H after various heat treatments 2 SO 4 Bode plot in +0.02 wt.% KSCN solution;
FIG. 5 is an equivalent circuit diagram used in a Zsimwin fit using electrochemical impedance spectroscopy software;
FIG. 6 shows impact toughness and charge transfer resistance R of Cr13 super martensitic stainless steel quenched and tempered sample t The relationship of (1).
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
The instrument used to perform the electrochemical impedance analysis test was the princeton VersaSTAT 3 electrochemical workstation.
A method for predicting the impact toughness change trend of Cr13 super stainless steel without damage and capable of being detected in situ is carried out according to the following steps:
step 3, the test sample is placed in 5% sulfuric acid (H) 2 SO 4 ) Performing electrochemical impedance analysis test with 0.02% potassium thiocyanate (KSCN) in mixed electrolyte water solution to obtain impact toughness of the test sample after open-circuit potential stabilization and corresponding charge transfer resistance R t Namely, after the open circuit potential is stabilized, the electrochemical impedance analysis test is carried out under the potential, and the test frequency is 10 5 -10 -2 Hz, the test amplitude is 10 mV;
the resistance of the carbide Cr-poor region is much lower than that of the carbide non Cr-poor region, so R t The size of (A) is mainly determined by the resistance of the carbide Cr-poor region, i.e. the more severe the carbide Cr-poor region is, R t The lower the value, i.e. R t The smaller the tendency for the impact toughness of the test specimen to decrease, the greater the need for safety protection or replacement of the test specimen.
Electrochemical impedance analysis tests were performed by taking the impact toughness change trend of Cr13 super martensitic stainless steel under different heat treatment conditions as an example, and the results of tables 1 and 2 were obtained as follows:
table 1: heat treatment system, impact toughness value and R of Cr13 super martensitic stainless steel t
TABLE 2 parameters of the impedance spectra after circuit fitting
It can be seen from Table 1 and FIG. 6 that the charge transfer resistance R is the same as that of the charge transfer resistor R t At lower levels, the impact toughness of Cr13 super martensitic stainless steel is very low, with R t The value is increased, the impact toughness is rapidly increased, and a relatively high platform is maintained; when R is t Less than 351.9 (omega cm) 2 ) The impact toughness of Cr13 super martensitic stainless steel decreases sharply, so that under this condition this value can be defined as the warning value for the impact toughness of Cr13 super martensitic stainless steel, when R t Below this value, the material runs the risk of brittle fracture under impact load and requires replacement or other corresponding measures for protection.
Wherein R is t Determination of the critical value: subjecting a super martensitic stainless steelThe steel is aged or tempered for a long time to simulate the actual working environment or working conditions and then 5 wt.% H is selected 2 SO 4 +0.02 wt.% KSCN aqueous solution as reaction medium, with 10mV amplitude from 10 using Princeton VersaSTAT 3 electrochemical workstation 5 -10 -2 Electrochemical impedance testing was performed at Hz, and the samples were at 5 wt.% H, as shown in FIGS. 1-4 2 SO 4 +0.02 wt.% electrochemical impedance spectrum in KSCN water solution, analyzing the obtained electrochemical impedance data with electrochemical impedance spectrum data analysis software Zsimwin, and fitting the electrochemical impedance spectrum with equivalent circuit as shown in FIG. 5 to obtain parameter values of each equivalent element, due to SCN in KSCN - Can form a complex with the passivation film to cause the weak part of the passivation film to be damaged preferentially, and the mass transfer resistance R obtained by fitting t Is the result of the parallel connection of the complete passive film surface of the sample and the weak part of the passive film, therefore R t The value of (A) is mainly determined by the resistance value of the weaker part of the smaller passivation film, so that the coarser the precipitated carbide, the larger the Cr-poor region, and the fitted R t The smaller the decrease and the greater the tendency of the impact toughness to decrease, and accordingly, R was established by electrochemical impedance spectroscopy fitting of different heat-treated samples t The relationship between the values and the impact toughness is shown in FIG. 6. it can be seen from FIG. 6 that there is a critical R t Value 351.9(Ω. cm) 2 ) R when fitting electrochemical impedance t Above this value, the impact toughness of the test specimens exhibits a high plateau when R is t Below this value, the impact toughness decreases rapidly.
The invention being thus described by way of example, it should be understood that any simple alterations, modifications or other equivalent alterations as would be within the skill of the art without the exercise of inventive faculty, are within the scope of the invention.
Claims (4)
1. A lossless and in-situ detectable method for predicting the impact toughness change trend of Cr13 super stainless steel is characterized by comprising the following steps: the method comprises the following steps:
step 1, subjecting the test sample to electric fieldChemical impedance analysis and test are carried out to obtain the impact toughness of the test sample after the open-circuit potential is stabilized and the charge transfer resistance R corresponding to the impact toughness t The method comprises the following steps of placing a test sample in a mixed electrolyte aqueous solution for electrochemical impedance analysis test, wherein in the mixed electrolyte aqueous solution, the mass percent of sulfuric acid is 5%, and the mass percent of potassium thiocyanate is 0.02%;
step 2, the charge transfer resistor R obtained in the step 1 t And the impact toughness of a test sample, and predicting the impact toughness change trend of Cr13 super stainless steel, wherein after the open circuit potential is stabilized, an electrochemical impedance analysis test is carried out under the open circuit potential, and the test frequency is 10 5 -10 -2 Hz, and the test amplitude is 10 mV;
R t the smaller, the greater the tendency of the test specimen to decrease in impact toughness, R t Critical value of 351.9 omega cm 2 When R is t When the value is less than the critical value, the impact toughness is rapidly decreased.
2. The method for predicting the impact toughness change trend of Cr13 super stainless steel in a lossless and in-situ detectable manner according to claim 1, wherein: in step 1, the back surface of the test surface of the sample to be tested is connected with a lead wire and then sealed in epoxy resin, and only the test surface of the sample to be tested is exposed, so as to ensure that the area of the test surface of the sample to be tested is equal to the exposed area of the sample to be tested.
3. The method for predicting the impact toughness change trend of Cr13 super stainless steel in a lossless and in-situ detectable manner according to claim 1, wherein the method comprises the following steps: in the step 1, the test surface of the sample to be tested is ground to 2000 meshes from coarse to fine by using SiC sand paper and is mechanically polished, and then the test sample is obtained after washing and drying by using deionized water and absolute ethyl alcohol.
4. Use of a lossless and in-situ detectable method for predicting impact toughness change trend of Cr13 super stainless steel according to any one of claims 1-3 for predicting safety protection or replacement time of Cr13 super stainless steel.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01312453A (en) * | 1988-06-13 | 1989-12-18 | Res Dev Corp Of Japan | Method for evaluating deterioration and damage of material by electrode impedance measurement |
| JPH03111752A (en) * | 1989-09-27 | 1991-05-13 | Res Dev Corp Of Japan | Method for evaluating secular embrittlement and softened damage of chromium molybdenum steel by electrochemical means |
| JP2010261853A (en) * | 2009-05-08 | 2010-11-18 | Shimizu Corp | Toughness evaluation method and toughness evaluation device of steel product |
| CN104820002A (en) * | 2015-04-16 | 2015-08-05 | 山东大学 | Quenched steel machining white layer detection method based on electrochemical detection device |
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2021
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01312453A (en) * | 1988-06-13 | 1989-12-18 | Res Dev Corp Of Japan | Method for evaluating deterioration and damage of material by electrode impedance measurement |
| JPH03111752A (en) * | 1989-09-27 | 1991-05-13 | Res Dev Corp Of Japan | Method for evaluating secular embrittlement and softened damage of chromium molybdenum steel by electrochemical means |
| JP2010261853A (en) * | 2009-05-08 | 2010-11-18 | Shimizu Corp | Toughness evaluation method and toughness evaluation device of steel product |
| CN104820002A (en) * | 2015-04-16 | 2015-08-05 | 山东大学 | Quenched steel machining white layer detection method based on electrochemical detection device |
Non-Patent Citations (2)
| Title |
|---|
| ZHIHONG LIU ET AL.: "Research on the correlation between impact toughness and corrosion performance of Cr13 Super martensitic stainless steel under deferent tempering condition", MATERIALS LETTERS, vol. 283, pages 128791 * |
| 张侠洲;陈延清;王凤会;张熹;赵英建;: "耐候钢Q420qNH焊接粗晶区冲击韧性及耐电化学腐蚀性能", 电焊机, no. 10 * |
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