CN113899682A - Method for detecting corrosion sensitivity of duplex stainless steel - Google Patents
Method for detecting corrosion sensitivity of duplex stainless steel Download PDFInfo
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- CN113899682A CN113899682A CN202111002342.3A CN202111002342A CN113899682A CN 113899682 A CN113899682 A CN 113899682A CN 202111002342 A CN202111002342 A CN 202111002342A CN 113899682 A CN113899682 A CN 113899682A
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- 238000005260 corrosion Methods 0.000 title claims abstract description 64
- 230000007797 corrosion Effects 0.000 title claims abstract description 58
- 229910001039 duplex stainless steel Inorganic materials 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 32
- 230000035945 sensitivity Effects 0.000 title claims abstract description 25
- 239000000523 sample Substances 0.000 claims abstract description 22
- 206010070834 Sensitisation Diseases 0.000 claims abstract description 15
- 230000008313 sensitization Effects 0.000 claims abstract description 15
- 238000012360 testing method Methods 0.000 claims abstract description 14
- 230000004913 activation Effects 0.000 claims abstract description 13
- 238000002474 experimental method Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 3
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 238000002161 passivation Methods 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 230000007420 reactivation Effects 0.000 abstract description 6
- 238000001514 detection method Methods 0.000 abstract description 5
- 230000003213 activating effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 16
- 238000003466 welding Methods 0.000 description 6
- 230000032683 aging Effects 0.000 description 4
- 238000012876 topography Methods 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 229910000963 austenitic stainless steel Inorganic materials 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 244000137852 Petrea volubilis Species 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229940116357 potassium thiocyanate Drugs 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
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- G01—MEASURING; TESTING
- 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
- G01—MEASURING; TESTING
- 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
- G01N17/02—Electrochemical measuring systems for weathering, corrosion or corrosion-protection measurement
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Abstract
The invention relates to a method for detecting corrosion sensitivity of duplex stainless steel, which comprises the steps of firstly preparing a sample, putting the duplex stainless steel into a box-type resistance furnace at 800 ℃, and respectively carrying out sensitization treatment for different times so as to obtain samples with different corrosion degrees; then preparing H with the concentration of 1 mol/L2SO4In solution, and in H2SO4Adding 1.5mol/L HCl solution into the solution, then performing ERP test, and obtaining the maximum current I corresponding to the active state under positive electrokinetic potential scanning through experimentsaWith maximum current I reactivated during the reverse scanrCalculating DOS = Ir/IaCharacterizing the intergranular corrosion susceptibility of the sample material by 100%; and finally, observing the surface appearance of each sample, and comprehensively judging the corrosion sensitivity of the material by combining the DOS value. The invention adopts an EPR method to collect the current density of an activation peak and a reactivation peak of the duplex stainless steel, and the current density of the reactivation peak are comparedThe sensitivity degree of intergranular corrosion of the duplex stainless steel is judged by activating the ratio of the peak current density and the corrosion morphology, and the detection result is accurate and reliable.
Description
Technical Field
The invention relates to the technical field of stainless steel corrosion detection, in particular to a method for detecting corrosion sensitivity of duplex stainless steel.
Background
The duplex stainless steel has good mechanical property and corrosion resistance, particularly has good pitting corrosion resistance in a medium environment containing chloride ions, and is applied to the marine environment along with the rapid development of marine engineering equipment and high-technology ship industry in China. The main connection mode of the duplex stainless steel in engineering application is welding modes such as manual arc welding, argon tungsten-arc welding, submerged arc welding and the like, however, the heat cycle action of local heating and cooling inherent in the welding process and the expansion and contraction phenomena of the material can cause sensitization of a welding joint area, so that the performance of the stainless steel is obviously changed, and particularly the corrosion resistance is seriously deteriorated.
EPR, namely an electrochemical potentiodynamic reactivation method, is a widely applied and mature method in various methods for evaluating the sensitivity of stainless steel intergranular corrosion, and has the characteristics of rapidness, no damage, quantification and the like. EPR method usually employs H2SO4+ KSCN electrolyte, which is developed mainly for single austenitic stainless steel and can not detect the sensitization of duplex stainless steel accurately, for example, an electrochemical method for detecting intergranular corrosion of 316LN austenitic stainless steel is disclosed in the patent with the publication number of CN104849204B, in which a sulfuric acid solution is used, and potassium thiocyanate and sodium chloride are added into the solution, so that the intergranular corrosion performance of austenitic stainless steel can be detected accurately, but the method is not suitable for detecting the corrosion sensitivity of duplex stainless steelTherefore, it is necessary to provide a method suitable for detecting the corrosion sensitivity of duplex stainless steel.
Disclosure of Invention
The present invention is directed to overcoming the above-mentioned disadvantages of the prior art and providing a method for detecting corrosion sensitivity of duplex stainless steel by collecting maximum current in active state I of duplex stainless steel under forward potentiodynamic scanning by EPR methodaWith maximum current I reactivated during the reverse scanrBy using Ir/ IaThe method is characterized in that not only can the subtle difference of the intercrystalline corrosion sensitivity between samples with different sensitization degrees be quantitatively compared, but also the intercrystalline corrosion morphology can be qualitatively observed, and the method is very sensitive to the detection of chromium-poor areas.
The technical scheme adopted by the invention for solving the problems is as follows: a method for detecting corrosion sensitivity of duplex stainless steel is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: sample preparation: putting the duplex stainless steel into a box-type resistance furnace at 800 ℃, and performing sensitization treatment for 5min, 10min, 20min and 30min respectively to obtain samples with different corrosion degrees;
step two: determination of electrochemical parameters: preparation of H at a concentration of 1 mol/L2SO4In solution, and in H2SO4Adding HCl solution with concentration of 1.5mol/L into the solution to obtain solution containing H2SO4And HCl, electrochemical testing equipment selects a CHI600 electrochemical tester, electrochemical testing is carried out in a three-electrode electrolytic cell, saturated calomel is used as a reference electrode, and a Pt electrode is used as an auxiliary electrode;
step three: performing ERP test: firstly, the working electrode is put into the mixed acid solution prepared in the second step, the experimental temperature is 30 +/-1 ℃, after the corrosion potential is stable, the working electrode starts to scan from the self-corrosion potential of-0.3V to the anode direction at the scanning speed of 1.66mV/s and an activation peak appears, and when the potential enters a passivation area to be +0.3V, the working electrode is instantly swept back at the same scanning speed and appearsThe activation peak stops the experiment when the potential returns to the self-corrosion potential, and the experiment can obtain the maximum current I corresponding to the activation state under positive electrokinetic potential scanningaWith maximum current I reactivated during the reverse scanrCalculating DOS = Ir/ IaCharacterizing the intergranular corrosion susceptibility of the sample material by 100%;
step four: and observing the surface appearance of each sample, and comprehensively judging the corrosion sensitivity of the material by combining the DOS value.
Preferably, 2205 duplex stainless steel is selected as the duplex stainless steel.
Preferably, in the first step, after the samples with different corrosion degrees are obtained, the samples are cut into 10 × 6mm, six surfaces of the samples are polished to 1000 # by SiC sand paper, the samples are packaged by epoxy resin and the working surfaces are exposed, before use, the working electrodes are polished to 1000 # by SiC sand paper, and the surfaces are cleaned by acetone and deionized water.
Preferably, in the fourth step, after the experiment is finished, the working electrode is dried after being cleaned by deionized water, the appearance of the duplex stainless steel microstructure of each sample is observed by adopting a scanning electron microscope, and the corrosion degree is judged by combining with the DOS value.
Compared with the prior art, the invention has the following advantages and effects: according to the invention, the current densities of an activation peak and a reactivation peak of the duplex stainless steel are collected by adopting an EPR method, the intergranular corrosion sensitivity of the duplex stainless steel is judged by the ratio of the current density of the reactivation peak to the current density of the activation peak and the corrosion morphology, and the detection result is accurate and reliable.
Drawings
In order to illustrate the embodiments of the present invention or the solutions in the prior art more clearly, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without inventive effort.
FIG. 1 is a graph showing the relationship between aging time and sensitivity to intergranular corrosion of a sensitized sample in an example of the present invention.
FIG. 2 is a Scanning Electron Microscope (SEM) morphology of an unsensitized sample EPR after testing in the example of the invention.
FIG. 3 is a scanning electron microscope topography after a sample EPR test with a sensitization time of 5min in the embodiment of the invention.
FIG. 4 is a scanning electron microscope topography after a sample EPR test with a sensitization time of 10min in the embodiment of the invention.
FIG. 5 is a scanning electron microscope topography after a sample EPR test with a sensitization time of 20min in the embodiment of the invention.
FIG. 6 is a scanning electron microscope topography after a sample EPR test with a sensitization time of 30min in the embodiment of the invention.
Detailed Description
The present invention will be described in further detail below by way of examples with reference to the accompanying drawings, which are illustrative of the present invention and are not to be construed as limiting the present invention.
Examples are given.
See fig. 1-6.
The embodiment discloses a method for detecting corrosion sensitivity of duplex stainless steel, which comprises the following steps:
the method comprises the following steps: sample preparation: the method comprises the following steps that 2205 duplex stainless steel is selected as the duplex stainless steel, the 2205 duplex stainless steel is placed in a box type resistance furnace at 800 ℃, sensitization treatment is carried out for 5min, 10min, 20min and 30min respectively, samples with different corrosion degrees are obtained, after the samples with different corrosion degrees are obtained, the samples are required to be cut into 10 x 6mm, six surfaces of the samples are polished to be number 1000 through SiC abrasive paper, the samples are packaged through epoxy resin, the working surface is exposed, before the samples are used, working electrodes are polished to be number 1000 through the SiC abrasive paper, and the surfaces are cleaned through acetone and deionized water;
step two: determination of electrochemical parameters: preparation of H at a concentration of 1 mol/L2SO4In solution, and in H2SO4Adding HCl solution with concentration of 1.5mol/L into the solution to obtain solution containing H2SO4Mixed acidic solution with HCl, electrochemical measurementsSelecting a CHI600 electrochemical tester as test equipment, carrying out electrochemical test in a three-electrode electrolytic cell, and taking saturated calomel as a reference electrode and a Pt electrode as an auxiliary electrode;
step three: performing ERP test: firstly, the working electrode is placed into the mixed acid solution prepared in the second step, the experiment temperature is 30 +/-1 ℃, after the corrosion potential is stable, the working electrode starts to scan from the self-corrosion potential of-0.3V to the anode direction at the scanning speed of 1.66mV/s and generates an activation peak, when the potential enters a passivation area with +0.3V, the working electrode is instantly swept back at the same scanning speed and generates an activation peak, when the potential returns to the self-corrosion potential, the experiment is stopped, and the experiment can obtain the maximum current I in the activation state corresponding to the scanning of the forward-direction potentialaWith maximum current I reactivated during the reverse scanrCalculating DOS = Ir/ IaCharacterizing the intergranular corrosion susceptibility of the sample material by 100%;
step four: and observing the surface appearance of each sample, and comprehensively judging the corrosion sensitivity of the material by combining with the DOS value, specifically, after the experiment is finished, cleaning the surface of the working electrode by using deionized water, drying the working electrode by blowing, observing the appearance of the duplex stainless steel microstructure of each sample by using a scanning electron microscope (SEM, Hitachi S3400N), and judging the corrosion degree by combining with the DOS value.
The method for detecting the corrosion sensitivity of the duplex stainless steel judges the intercrystalline corrosion sensitivity of the duplex stainless steel through the ratio of the reactivation peak current density to the activation peak current density and the corrosion morphology, the detection result is accurate and reliable, in order to explain the technical effect of the method, a group of standard samples processed at different sensitization temperatures of 800 ℃ in different sensitization times are selected, fig. 1 is a relation graph of the aging time and the intercrystalline corrosion sensitivity of the sensitization samples, and as can be seen from the graph, the sensitivity is judged at 1 mol/L H2SO4In the mixed solution formed by the solution and the 1.5mol/L HCl solution, the intergranular corrosion sensitivity of the sample becomes larger along with the increase of the aging time, and the solution and the method are selected to accurately represent the intergranular corrosion sensitivity.
In order to more intuitively represent different corrosion degrees, the samples are observed under a scanning electron microscope, see fig. 2 to 6, and as can be seen from fig. 2, the samples without sensitization treatment do not generate intergranular corrosion, and the surfaces of the samples present a small amount of step structures. The samples aged for 5min and 10min exhibited a double structure (fig. 3 and 4), the appearance of this structure indicating the onset of intergranular corrosion, whereas the groove structure was found in the samples aged for 20min and 30min, and the density of pitting pits increased with increasing aging time (fig. 5 and 6), which indicates that the samples experienced severe intergranular corrosion.
Although the present invention has been described with reference to the above embodiments, it should be understood that the scope of the present invention is not limited thereto, and that various changes and modifications can be made by those skilled in the art without departing from the spirit and scope of the present invention.
Claims (4)
1. A method for detecting corrosion sensitivity of duplex stainless steel is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: sample preparation: putting the duplex stainless steel into a box-type resistance furnace at 800 ℃, and performing sensitization treatment for 5min, 10min, 20min and 30min respectively to obtain samples with different corrosion degrees;
step two: determination of electrochemical parameters: preparation of H at a concentration of 1 mol/L2SO4In solution, and in H2SO4Adding HCl solution with concentration of 1.5mol/L into the solution to obtain solution containing H2SO4And HCl, electrochemical testing equipment selects a CHI600 electrochemical tester, electrochemical testing is carried out in a three-electrode electrolytic cell, saturated calomel is used as a reference electrode, and a Pt electrode is used as an auxiliary electrode;
step three: performing ERP test: firstly, the working electrode is placed into the mixed acid solution prepared in the second step, the experiment temperature is 30 +/-1 ℃, after the corrosion potential is stable, the working electrode starts to scan from the self-corrosion potential of-0.3V to the anode direction at the scanning speed of 1.66mV/s and generates an activation peak, when the potential enters a passivation area with +0.3V, the working electrode is instantly swept back at the same scanning speed and generates an activation peak, when the potential returns to the self-corrosion potential, the experiment is stopped, and the experiment can obtain the maximum electric potential corresponding to the activation state under the positive potential scanningStream IaWith maximum current I reactivated during the reverse scanrCalculating DOS = Ir/ IaCharacterizing the intergranular corrosion susceptibility of the sample material by 100%;
step four: and observing the surface appearance of each sample, and comprehensively judging the corrosion sensitivity of the material by combining the DOS value.
2. The method of detecting corrosion susceptibility of duplex stainless steel according to claim 1, wherein: the duplex stainless steel is 2205 duplex stainless steel.
3. The method of detecting corrosion susceptibility of duplex stainless steel according to claim 1, wherein: in the first step, after the samples with different corrosion degrees are obtained, the samples are required to be cut into 10 x 6mm, six surfaces of the samples are polished to be No. 1000 through SiC abrasive paper, the samples are packaged through epoxy resin, the working surfaces are exposed, before the samples are used, the working electrodes are polished to be No. 1000 through SiC abrasive paper, and the surfaces are cleaned through acetone and deionized water.
4. The method of detecting corrosion susceptibility of duplex stainless steel according to claim 1, wherein: in the fourth step, after the experiment is finished, the working electrode is dried after being cleaned by deionized water, the appearance of the duplex stainless steel microstructure of each sample is observed by adopting a scanning electron microscope, and the corrosion degree is judged by combining with the DOS value.
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101762454A (en) * | 2010-02-03 | 2010-06-30 | 海洋王照明科技股份有限公司 | Dual-ring electrochemical dynamic potential reactivating evaluating method for diphase stainless steel intercrystalline corrosion sensitivity |
CN105973970A (en) * | 2016-04-29 | 2016-09-28 | 河海大学常州校区 | Method for detecting corrosion sensitivity of austenitic stainless steel |
CN106290140A (en) * | 2016-09-29 | 2017-01-04 | 珠海格力电器股份有限公司 | A kind of method checking Intergranular Corrosion of Austenitic Stainless Steel sensitivity |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN101762454A (en) * | 2010-02-03 | 2010-06-30 | 海洋王照明科技股份有限公司 | Dual-ring electrochemical dynamic potential reactivating evaluating method for diphase stainless steel intercrystalline corrosion sensitivity |
CN105973970A (en) * | 2016-04-29 | 2016-09-28 | 河海大学常州校区 | Method for detecting corrosion sensitivity of austenitic stainless steel |
CN106290140A (en) * | 2016-09-29 | 2017-01-04 | 珠海格力电器股份有限公司 | A kind of method checking Intergranular Corrosion of Austenitic Stainless Steel sensitivity |
Non-Patent Citations (1)
Title |
---|
徐菊良;邓博;孙涛;李劲;蒋益明;: "DL-EPR法评价2205双相不锈钢晶间腐蚀敏感性", 金属学报, no. 03 * |
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