CN114791456B - Nondestructive and in-situ detection method for predicting impact toughness change trend of Cr13 super stainless steel - Google Patents
Nondestructive and in-situ detection method for predicting impact toughness change trend of Cr13 super stainless steel Download PDFInfo
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- CN114791456B CN114791456B CN202111069220.6A CN202111069220A CN114791456B CN 114791456 B CN114791456 B CN 114791456B CN 202111069220 A CN202111069220 A CN 202111069220A CN 114791456 B CN114791456 B CN 114791456B
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- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 21
- 239000010935 stainless steel Substances 0.000 title claims abstract description 21
- 238000001514 detection method Methods 0.000 title claims abstract description 11
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 11
- 238000012360 testing method Methods 0.000 claims abstract description 64
- 238000004458 analytical method Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 230000007423 decrease Effects 0.000 claims description 6
- 239000003792 electrolyte Substances 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 244000137852 Petrea volubilis Species 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 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
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 230000001066 destructive effect Effects 0.000 claims 1
- 229910001105 martensitic stainless steel Inorganic materials 0.000 abstract description 27
- 239000000463 material Substances 0.000 abstract description 6
- 238000011282 treatment Methods 0.000 abstract description 4
- 230000032683 aging Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000005496 tempering Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 28
- 238000002161 passivation Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- 238000001453 impedance spectrum Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient 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
- 239000011159 matrix material Substances 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
- 238000007789 sealing Methods 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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- General Physics & Mathematics (AREA)
- Immunology (AREA)
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Abstract
The invention provides a nondestructive and in-situ detection method for predicting the impact toughness change trend of Cr13 super stainless steel, which comprises the steps 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 resistor R corresponding to the impact toughness t The method comprises the steps of carrying out a first treatment on the surface of the With charge transfer resistance R t And testing the relation between the impact toughness of the sample, and predicting the impact toughness change trend of the Cr13 super stainless steel. The invention predicts the impact toughness change trend of Cr13 super martensitic stainless steel, in particular Cr13 super martensitic stainless steel after tempering or long-time aging treatment by using electrochemical impedance technology, and the invention predicts the charge transfer resistor R t As a prediction index, detecting precipitated phases such as carbide in Cr13 super martensitic stainless steel, and evaluating the change of impact toughness of the material, thereby guiding the safe progress of corresponding production.
Description
Technical Field
The invention relates to the technical field of stainless steel electrochemical testing, in particular to a nondestructive and in-situ detection method for predicting the impact toughness change trend of Cr13 super stainless steel.
Background
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 easy to separate out, so that the mechanical property and corrosion resistance of Cr13 super martensitic stainless steel are reduced, and particularly, after the carbide is coarsened along a grain boundary, the plasticity and toughness of the material are obviously reduced, and accidents are caused. Therefore, it is particularly important to detect the precipitated phase 000 such as carbide in the Cr13 super martensitic stainless steel.
The traditional carbide analysis method is to use Scanning Electron Microscope (SEM) and Transmission Electron Microscope (TEM) and the like, and the method has high requirements on equipment, samples and personnel, is usually only carried out in a scientific laboratory, is limited to microcosmic qualitative or semi-quantitative detection, and cannot realize macroscopic quantitative detection of the carbide in the stainless steel.
Disclosure of Invention
The invention overcomes the defects in the prior art, the prior carbide analysis method can not realize macroscopic quantitative detection of carbide in stainless steel, and provides a nondestructive and in-situ-detectable method for predicting the impact toughness change trend of Cr13 super stainless steel, the invention predicts the impact toughness change trend of Cr13 super martensitic stainless steel by utilizing electrochemical impedance technology based on the principle that corrosion usually occurs preferentially in the area and the adjacent area of the area because the precipitated phase such as carbide belongs to the second phase in the stainless steel and the structure and the components of the precipitated phase are greatly different from the matrix, and the invention predicts the impact toughness change trend of Cr13 super martensitic stainless steel, especially Cr13 super martensitic stainless steel after tempering or long-time aging treatment t As a prediction index, detecting precipitated phases such as carbide in Cr13 super martensitic stainless steel, and evaluating the change of impact toughness of the material, thereby guiding the safe progress of corresponding production.
The aim of the invention is achieved by the following technical scheme.
A nondestructive and in-situ detection method for predicting impact toughness change trend of Cr13 super stainless steel is carried out according to the following steps:
step 1, performing electrochemical impedance analysis test on a test sample to obtain impact toughness of the test sample with stable open circuit potential and a charge transfer resistor R corresponding to the impact toughness t ；
In the step 1, the back surface of the test sample is sealed in epoxy resin after being connected with a wire, and only the test surface of the test sample is exposed, so that the area of the test surface of the test sample is ensured to be equal to the exposed area of the test sample;
in the step 1, polishing the test surface of a sample to be tested to 2000 meshes from coarse to fine by using SiC sand paper, mechanically polishing, washing with deionized water and absolute ethyl alcohol, and drying to obtain a test sample;
in the step 1, a test sample is placed in a mixed electrolyte aqueous solution for electrochemical impedance analysis test, wherein the mass percentage of sulfuric acid in the mixed electrolyte aqueous solution is 5%, and the mass percentage of potassium thiocyanate is 0.02%;
in step 1, after the open circuit potential is stabilized, electrochemical impedance analysis test is performed at the potential with a test frequency of 10 5 -10 -2 Hz, test amplitude is 10mV;
step 2, using the charge transfer resistor R obtained in step 1 t And testing the relation between the impact toughness of the sample, and predicting the impact toughness change trend of Cr13 super stainless steel;
the resistance of the carbide Cr-depleted region is much less than the resistance of the carbide non-Cr-depleted region, so R t The size of (2) is mainly determined by the resistance of the carbide-depleted Cr region, i.e., the more severe the carbide-depleted Cr region, R t The lower the value, i.e. R t The smaller the test specimen, the greater the propensity for impact toughness to decrease, requiring safety protection or replacement of the test specimen.
In practical application, R of the test sample material under certain conditions can be obtained by controlling variables 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 reduced sharply; in the example when R t Below 351.9 (Ω cm) 2 ) The impact toughness of Cr13 super martensitic stainless steel is drastically reduced, so that the value can be defined as the guard value of the impact toughness of Cr13 super martensitic stainless steel under such conditions, when R t Below this value, the material is at risk of brittle fracture under impact load, and needs to be replaced or otherwise protected.
The inventionThe beneficial effects are that: cr13 super martensitic stainless steel sample at 5%H 2 SO 4 Electrochemical impedance test is carried out in electrolyte solution with +0.02% of KSCN, impedance spectrum is fitted by fitting software, parameters with practical physical significance are obtained, and charge transfer resistance R is utilized t As a new index, predicting the change of the impact toughness of Cr13 super martensitic stainless steel; KSCN is a depolarizer which can locally destroy the passivation film, and because carbide and its adjacent area are weak areas of the passivation film, it is more easily destroyed in the course of corrosion, and by using this principle, the invention uses the charge transfer resistor R t As a new index, the method detects precipitated phases such as carbide in Cr13 super martensitic stainless steel and evaluates the change of impact toughness of the material, and the method can rapidly and quantitatively predict the change of impact toughness of Cr13 super martensitic stainless steel in a nondestructive and in-situ detection manner, thereby guiding the safe production.
Drawings
FIG. 1 shows that the Cr13 super martensitic stainless steel hot rolled sample after different heat treatments has been subjected to 5wt.% H 2 SO 4 Nyquist plot in +0.02wt.% KSCN solution;
FIG. 2 shows that the Cr13 super martensitic stainless steel hot rolled sample after different heat treatments has been subjected to 5wt.% H 2 SO 4 Bode plot in +0.02wt.% KSCN solution;
FIG. 3 shows that the Cr13 super martensitic stainless steel solution treated sample was treated with 5wt.% H after different heat treatments 2 SO 4 Nyquist plot in +0.02wt.% KSCN solution;
FIG. 4 shows that the Cr13 super martensitic stainless steel solution treated sample was treated with 5wt.% H after different heat treatments 2 SO 4 Bode plot in +0.02wt.% KSCN solution;
FIG. 5 is an equivalent circuit diagram for use in a Zsimwin fit using electrochemical impedance spectroscopy analysis software;
FIG. 6 shows the impact toughness and the charge transfer resistance R of a Cr13 super martensitic stainless steel quenched and tempered sample t Is a relationship of (2).
Detailed Description
The technical scheme of the invention is further described by specific examples.
The instrument used to conduct the electrochemical impedance analysis test was a prinston versatat 3 electrochemical workstation.
A nondestructive and in-situ detection method for predicting impact toughness change trend of Cr13 super stainless steel is carried out according to the following steps:
step 1, connecting a lead on the back of a test surface of a to-be-tested sample, sealing the lead in epoxy resin, and exposing only the test surface of the to-be-tested sample to ensure that the area of the test surface of the to-be-tested sample is equal to the exposed area of the to-be-tested sample;
step 2, polishing the test surface of the sample to be tested obtained in the step 1 from coarse to fine to 2000 meshes by using SiC sand paper, mechanically polishing, washing with deionized water and absolute ethyl alcohol, and drying to obtain a test sample;
step 3, the test sample was placed in 5% sulfuric acid (H 2 SO 4 ) Electrochemical impedance analysis test is carried out in the mixed electrolyte aqueous solution with 0.02 percent of potassium thiocyanate (KSCN) 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 That is, after the open circuit potential is stabilized, electrochemical impedance analysis test is performed at the potential with a test frequency of 10 5 -10 -2 Hz, test amplitude is 10mV;
step 4, using the charge transfer resistor R obtained in step 3 t And testing the relation between the impact toughness of the sample, and predicting the impact toughness change trend of Cr13 super stainless steel;
the resistance of the carbide Cr-depleted region is much less than the resistance of the carbide non-Cr-depleted region, so R t The size of (2) is mainly determined by the resistance of the carbide-depleted Cr region, i.e., the more severe the carbide-depleted Cr region, R t The lower the value, i.e. R t The smaller the test specimen, the greater the propensity for impact toughness to decrease, requiring safety protection or replacement of the test specimen.
Electrochemical impedance analysis tests were performed using the impact toughness variation trend of Cr13 super martensitic stainless steel under different heat treatment conditions as an example, and the results of table 1 and table 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 impedance spectra after Circuit fitting
It can be seen from Table 1 and FIG. 6 that when 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 impact toughness is rapidly increased by increasing the value, and a higher platform is maintained; when R is t Below 351.9 (Ω cm) 2 ) The impact toughness of Cr13 super martensitic stainless steel is drastically reduced at this time, so that this value can be defined as the guard value of the impact toughness of Cr13 super martensitic stainless steel under this condition, when R t Below this value, the material is at risk of brittle fracture under impact load, and needs to be replaced or otherwise protected.
Wherein R is t Determination of the critical value: the super martensitic stainless steel is aged or tempered for a long time to simulate the actual working environment or working condition, and then 5wt.% H is selected 2 SO 4 +0.02wt.% KSCN aqueous solution as reaction medium, 10mV amplitude from 10 using a prinston versstat 3 electrochemical workstation 5 -10 -2 Hz electrochemical impedance testing was performed, as shown in FIGS. 1-4, with samples at 5wt.% H 2 SO 4 +0.02wt.% of the electrochemical impedance spectrum in the KSCN aqueous solution, analyzing the obtained electrochemical impedance data by using an electrochemical impedance spectrum data analysis software Zsimwin, and fitting the electrochemical impedance spectrum by using an equivalent circuit as shown in figure 5 to obtain various equivalent elementsDue to SCN in KSCN - Can form complex with the passivation film to lead the weak part of the passivation film to be destroyed preferentially, and the mass transfer resistor R obtained by fitting t Is the result of parallel connection of the complete passivation film surface of the sample and the weak part of the passivation film, thus R t The value of (2) is mainly determined by the resistance value of the weak part of the passivation film, so that the larger precipitated carbide is, the larger Cr-deficient area is, and R is obtained by fitting t The smaller the one, the greater the tendency to decrease impact toughness, from which R is established by fitting electrochemical impedance spectra to different heat treated samples t The relationship between the values and impact toughness gives FIG. 6, from which it can be seen that a critical R exists in FIG. 6 t Value 351.9 (Ω cm) 2 ) When the electrochemical impedance is fitted to the obtained R t Above this value, the impact toughness of the test specimen exhibits a higher plateau, when R t Below this value, the impact toughness decreases rapidly.
The foregoing has described exemplary embodiments of the invention, it being understood that any simple variations, modifications, or other equivalent arrangements which would not unduly obscure the invention may be made by those skilled in the art without departing from the spirit of the invention.
Claims (4)
1. A nondestructive and in-situ detection method for predicting impact toughness change trend of Cr13 super stainless steel is characterized by comprising the following steps: the method comprises the following steps of:
step 1, performing electrochemical impedance analysis test on a test sample to obtain impact toughness of the test sample with stable open circuit potential and a charge transfer resistor R corresponding to the impact toughness t The method comprises the steps of placing a test sample in a mixed electrolyte aqueous solution for electrochemical impedance analysis test, wherein the mass percentage of sulfuric acid in the mixed electrolyte aqueous solution is 5%, and the mass percentage of potassium thiocyanate is 0.02%;
step 2, using the charge transfer resistor R obtained in step 1 t And testing the relation between the impact toughness of the sample, and predicting the impact toughness change trend of Cr13 super stainless steel, wherein after the open circuit potential is stabilized, electrochemical is performed under the open circuit potentialImpedance analysis test with a test frequency of 10 5 -10 -2 Hz, test amplitude is 10mV;
R t the smaller the test specimen, the greater the tendency for impact toughness to decrease, R t Is 351.9 Ω cm 2 When R is t Below the critical value, the impact toughness decreases rapidly.
2. The method for predicting the impact toughness change trend of Cr13 super stainless steel, which is nondestructive and in-situ detectable, according to claim 1, wherein the method comprises the following steps: in step 1, the back of the test surface of the test sample is sealed in epoxy resin after being connected with a wire, and only the test surface of the test sample is exposed, so that the area of the test surface of the test sample is equal to the exposed area of the test sample.
3. The method for predicting the impact toughness change trend of Cr13 super stainless steel, which is nondestructive and in-situ detectable, 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 polished to 2000 meshes from coarse to fine by using SiC sand paper and mechanically polished, and then washed by deionized water and absolute ethyl alcohol and dried, thus obtaining the test sample.
4. Use of a non-destructive and in-situ detectable method for predicting the impact toughness trend of Cr13 super stainless steel according to any one of claims 1-3 for predicting Cr13 super stainless steel safety protection or replacement time.
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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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- 2021-09-13 CN CN202111069220.6A patent/CN114791456B/en active Active
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 |
|---|
| Research on the correlation between impact toughness and corrosion performance of Cr13 Super martensitic stainless steel under deferent tempering condition;Zhihong Liu et al.;Materials Letters;第283卷;128791 * |
| 耐候钢Q420qNH焊接粗晶区冲击韧性及耐电化学腐蚀性能;张侠洲;陈延清;王凤会;张熹;赵英建;;电焊机(10);全文 * |
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