CN106918545B - Corrosion test method and device for rapidly realizing occurrence and development of stainless steel pitting corrosion - Google Patents
Corrosion test method and device for rapidly realizing occurrence and development of stainless steel pitting corrosion Download PDFInfo
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- CN106918545B CN106918545B CN201510999424.8A CN201510999424A CN106918545B CN 106918545 B CN106918545 B CN 106918545B CN 201510999424 A CN201510999424 A CN 201510999424A CN 106918545 B CN106918545 B CN 106918545B
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- 238000005260 corrosion Methods 0.000 title claims abstract description 117
- 230000007797 corrosion Effects 0.000 title claims abstract description 116
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 79
- 239000010935 stainless steel Substances 0.000 title claims abstract description 79
- 238000011161 development Methods 0.000 title claims abstract description 26
- 238000010998 test method Methods 0.000 title claims abstract description 16
- 238000012360 testing method Methods 0.000 claims abstract description 56
- 230000010287 polarization Effects 0.000 claims abstract description 39
- 239000000463 material Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000005259 measurement Methods 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 4
- 238000000840 electrochemical analysis Methods 0.000 claims description 4
- 238000005530 etching Methods 0.000 claims description 3
- 238000002474 experimental method Methods 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 2
- 239000001301 oxygen Substances 0.000 claims 2
- 229910052760 oxygen Inorganic materials 0.000 claims 2
- 230000018109 developmental process Effects 0.000 description 16
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 230000012010 growth Effects 0.000 description 4
- 238000002161 passivation Methods 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 2
- 230000003698 anagen phase Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 229910001105 martensitic stainless steel Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- G01N17/006—Investigating resistance of materials to the weather, to corrosion, or to light of metals
-
- 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
Abstract
The invention relates to the field of corrosion pitting test, in particular to a corrosion test method and device for rapidly realizing the occurrence and development of stainless steel pitting. The test method comprises the steps of firstly measuring corrosion potential of a stainless steel working electrode by using an electrochemical workstation open-circuit potential measurement mode, then measuring pitting potential and repassivation potential of the stainless steel working electrode by using a dynamic potential scanning mode, then selecting a potential value between the measured pitting potential and repassivation potential as polarization potential, and applying the selected polarization potential to the stainless steel working electrode by using an electrochemical workstation constant potential polarization mode, so that pitting corrosion generated by the stainless steel working electrode in the dynamic potential scanning stage continues to grow, and pitting pits with different depths are obtained in different polarization time. The method has simple structure and convenient operation, can rapidly realize the occurrence and development of the pitting corrosion of the stainless steel under the indoor simulated natural environment, and can compare the pitting corrosion resistance of the stainless steel with different materials.
Description
Technical Field
The invention relates to the field of corrosion pitting test, in particular to a corrosion test method and device for rapidly realizing the occurrence and development of stainless steel pitting.
Background
Pitting corrosion is the most common local corrosion of stainless steel, and a passivation film of the stainless steel is easily damaged in a corrosion environment (particularly a medium containing Cl < - >) to generate active points, so that the pitting corrosion accelerates growth under the action of a corrosion medium, and serious local corrosion is caused on the stainless steel. Scientific researchers have studied for decades to recognize that the pitting process can be divided into the following steps: pitting, pitting metastable growth, pitting stable growth and pitting occurrence and re-passivation terminate the growth phase. In the electrochemical theory, when the external potential of the stainless steel sample exceeds the pitting corrosion starting potential, pitting corrosion is generated, and the pitting corrosion starts to grow along with the reduction of the potential; however, when the potential drops below the repassivation potential, the formation of the passivation film may terminate the pitting growth.
In natural environment (such as stratum water environment), because corrosiveness of a corrosive medium is small, and a certain induction period exists in the occurrence of stainless steel pitting, the stainless steel pitting under the condition needs longer time, and a common corrosion test method is an indoor soaking test in order to evaluate and compare the pitting resistance of stainless steel with different materials under the environment, but the required test period is longer, and a test result cannot be obtained quickly. The electrochemical polarization corrosion test method can not only shorten the test period and quickly lead the stainless steel to generate pitting corrosion, but also lead the pitting corrosion to grow quickly, and can evaluate and compare the pitting corrosion resistance of the stainless steel with different materials in a designated corrosion medium in a short time.
Disclosure of Invention
The invention aims to provide a corrosion test method and a corrosion test device for rapidly realizing the occurrence and the development of stainless steel pitting corrosion, which can rapidly realize the occurrence and the development of the stainless steel pitting corrosion in a corrosion medium under the indoor simulated natural environment condition, and evaluate and compare the pitting corrosion resistance of the stainless steel with different materials in a short time.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
a corrosion test apparatus for rapidly effecting the onset and progression of pitting corrosion in stainless steel, the apparatus comprising: the electrochemical workstation, the corrosion electrolytic cell, the test medium solution, the auxiliary electrode, the reference electrode, the working electrode and the vent pipe have the following specific structures:
a test medium solution is filled in the corrosion electrolytic cell, an auxiliary electrode, a reference electrode and a working electrode are arranged in the test medium solution, and a vent pipe of nitrogen is inserted in the test medium solution; the electrochemical workstation is provided with four binding clips, and is respectively connected with the auxiliary electrode, the reference electrode, the working electrode and the grounding wire through the four binding clips.
The corrosion test device for rapidly realizing the occurrence and development of stainless steel pitting corrosion is characterized in that the auxiliary electrode is a platinum electrode, the reference electrode is a saturated calomel electrode, and the working electrode is a stainless steel electrode.
The corrosion test device for rapidly realizing the occurrence and development of stainless steel pitting corrosion is characterized in that a working electrode binding clip WE, an auxiliary electrode binding clip CE, a reference electrode binding clip RE and a grounding wire clip GOUND of an electrochemical workstation are respectively and correspondingly connected with a working electrode, an auxiliary electrode, a reference electrode and a grounding wire, and the working electrode, the auxiliary electrode and the reference electrode are arranged in a corrosion electrolytic cell special for an electrochemical test experiment and are completely immersed below the liquid level of a test medium solution to form an electrochemical workstation and an electrochemical three-electrode system test system.
The corrosion test method for rapidly realizing the occurrence and development of the stainless steel pitting corrosion of the device comprises the steps of firstly measuring the corrosion potential of a stainless steel working electrode by using an open-circuit potential measurement mode of an electrochemical working station, then measuring the pitting corrosion potential and the repassivation potential of the stainless steel working electrode by using a dynamic potential scanning mode, then selecting a potential value between the measured pitting corrosion potential and the repassivation potential as a polarization potential, and applying the selected polarization potential on the stainless steel working electrode by using a constant potential polarization mode of the electrochemical working station, so that the pitting corrosion generated by the stainless steel working electrode in the dynamic potential scanning stage continues to grow, and pitting corrosion pits with different depths are obtained in different polarization time, and evaluating and comparing the pitting corrosion resistance of stainless steel with different materials according to the result.
The corrosion test method for rapidly realizing the occurrence and development of stainless steel pitting corrosion comprises the following specific steps:
(1) Preparing corresponding test medium solution according to test requirements, and placing the test medium solution into a corrosion electrolytic cell;
(2) Placing the working electrode, the auxiliary electrode and the reference electrode which are connected with the lead in a corrosion electrolytic cell, and requiring all the electrodes to be completely immersed below the liquid level;
(3) After the working electrode is placed in the corrosion electrolytic cell for 15min, the open-circuit potential of the working electrode, namely the corrosion potential, is measured by using an electrochemical workstation open-circuit potential measurement mode;
(4) Anodic polarization was performed at a potential scan rate of 20mV/min from the corrosion potential using an electrochemical workstation potentiodynamic scan mode when the anodic current reached 500. Mu.A/cm 2 Then, retrace is carried out, and the scanning is stopped after the etching potential is returned;
(5) With a corresponding current density of 10 μA/cm on the anodic polarization curve 2 The potential value is used as the pitting potential of the stainless steel electrode, the intersection point of the retrace curve and the anodic polarization curve is used as the repassivation potential of the stainless steel electrode, and the pitting potential and the repassivation potential are read according to the two requirements;
(6) And selecting a potential value as a polarization potential in the range from the measured repassivation potential to the pitting potential, and carrying out constant potential polarization on the working electrode by adopting a constant potential polarization mode of the electrochemical workstation so as to enable pitting corrosion generated by the working electrode in a potentiodynamic scanning stage to continue growing.
According to the corrosion test method for rapidly realizing the occurrence and development of stainless steel pitting corrosion, when the requirement of deoxidizing is met in the step (1), a nitrogen oxygen-expelling mode is adopted for deoxidizing.
The invention has the advantages and beneficial effects that:
1. the test method of the invention is to firstly measure the corrosion potential of the stainless steel working electrode, then measure the pitting potential and the repassivation potential of the stainless steel working electrode, then select a potential value between the measured pitting potential and the repassivation potential as the polarization potential, and apply the selected polarization potential on the working electrode, so that the pitting corrosion generated by the stainless steel working electrode in the dynamic potential scanning stage continues to grow, and pitting corrosion with different depths is obtained in different time.
2. The invention can rapidly realize the occurrence and development of stainless steel pitting corrosion under the indoor simulated natural environment, evaluate and compare the pitting corrosion resistance of stainless steel with different materials, and shorten the test period for the occurrence and development of stainless steel pitting corrosion by adopting an indoor soaking test.
Drawings
FIG. 1 is a diagram of an electrochemical test apparatus according to the present invention.
In the figure: 1-electrochemical workstation, 2-corrosion electrolytic cell, 3-test medium solution, 4-auxiliary electrode, 5-reference electrode (saturated calomel electrode), 6-working electrode (stainless steel electrode) and 7-vent pipe.
FIG. 2 is a plot of depth of pitting as a function of time for the present invention.
Detailed Description
The invention is further described with reference to the accompanying drawings:
as shown in FIG. 1, the corrosion test device for rapidly realizing the occurrence and development of stainless steel pitting corrosion mainly comprises: the electrochemical workstation 1, the corrosion electrolytic cell 2, the test medium solution 3, the auxiliary electrode 4 (platinum electrode), the reference electrode 5 (saturated calomel electrode), the working electrode 6 (stainless steel electrode), the vent pipe 7 and the like have the following specific structures:
the corrosion electrolytic cell 2 is filled with a test medium solution 3, an auxiliary electrode 4, a reference electrode 5 and a working electrode 6 are arranged in the test medium solution 3, and a vent pipe 7 of nitrogen is inserted into the test medium solution 3; the electrochemical workstation 1 is provided with four binding clips, and is correspondingly connected with the auxiliary electrode 4, the reference electrode 5, the working electrode 6 and the grounding wire through the four binding clips, so that the types of test medium solutions contained in the corrosion electrolytic cell 2 can be determined according to test requirements.
Before the test, the working electrode binding clips (WE), the auxiliary electrode binding Clips (CE), the reference electrode binding clips (RE) and the grounding wire clips (GOUND) of the electrochemical workstation are correspondingly connected with the working electrode 6, the auxiliary electrode 4, the reference electrode 5 and the grounding wire respectively, and the working electrode, the auxiliary electrode and the reference electrode are placed in the corrosion electrolytic cell 2 special for the electrochemical test experiment, and all the electrodes are required to be completely immersed below the liquid level during the test, so that the electrochemical workstation and the electrochemical three-electrode system test system are formed.
The corrosion test method for rapidly realizing the occurrence and development of the stainless steel pitting corrosion by adopting the test device comprises the steps of firstly measuring the corrosion potential of a stainless steel working electrode by using an open-circuit potential measurement mode of an electrochemical working station, then measuring the pitting corrosion potential and the repassivation potential of the stainless steel working electrode by using a dynamic potential scanning mode, then selecting a potential value between the measured pitting corrosion potential and the repassivation potential as a polarization potential, and applying the selected polarization potential on the stainless steel working electrode by using a constant potential polarization mode of the electrochemical working station, so that the pitting corrosion generated by the stainless steel working electrode in the dynamic potential scanning stage continues to grow, and pitting corrosion pits with different depths are obtained in different polarization time, and evaluating and comparing the pitting corrosion resistance of stainless steel with different materials according to the result. The method comprises the following specific steps:
(1) Preparing corresponding test medium solution according to test requirements, and placing the test medium solution into a corrosion electrolytic cell, and deoxidizing the test medium solution by adopting a nitrogen oxygen-driving mode if the deoxidization requirements exist;
(2) Placing the stainless steel working electrode, the auxiliary electrode and the reference electrode which are connected with the lead wire in a corrosion electrolytic cell, and requiring all the electrodes to be completely immersed below the liquid level;
(3) After the stainless steel working electrode is placed in the corrosion electrolytic cell for 15min, the open-circuit potential of the stainless steel working electrode, namely the corrosion potential, is measured by using an electrochemical workstation open-circuit potential measurement mode;
(4) Anodic polarization was performed at a potential scan rate of 20mV/min from the corrosion potential using an electrochemical workstation potentiodynamic scan mode when the anodic current reached 500. Mu.A/cm 2 Then, retrace is carried out, and the scanning is stopped after the etching potential is returned;
(5) With a corresponding current density of 10 μA/cm on the anodic polarization curve 2 The potential value is used as the pitting potential of the stainless steel electrode, the intersection point of the retrace curve and the anodic polarization curve is used as the repassivation potential of the stainless steel electrode, and the pitting potential and the repassivation potential are read according to the two requirements;
(6) And selecting a potential value as a polarization potential in the range from the measured repassivation potential to the pitting potential, and carrying out constant potential polarization on the stainless steel working electrode by adopting a constant potential polarization mode of an electrochemical workstation, so that pitting corrosion generated by the stainless steel working electrode in a dynamic potential scanning stage continues to grow, and the test time can be determined according to practical conditions.
By adopting the test scheme, the occurrence and development of stainless steel pitting corrosion are rapidly realized in an indoor simulated natural corrosion environment, the pitting corrosion resistance of stainless steel made of different materials is evaluated and compared, and the test period for the occurrence and development of stainless steel pitting corrosion by adopting an indoor soaking test is shortened.
Examples:
experimental data: super 13Cr martensitic stainless steel is selected as a research object, and the method is used for testing, wherein an experimental medium is NaCl solution, the temperature is 50 ℃, and the constant potential polarization experimental period is 3h, 6h, 9h, 12h, 24h and 48h respectively. The maximum pitting depth data of the 13Cr test specimens measured after the test are shown in the following table.
Table 1 table 13cr test sample maximum pitting depth data statistics
Experimental curve: and performing power function fitting on the pitting depth and time data to obtain a power function relation curve of the maximum pitting depth and time, wherein the result is shown in figure 2.
Experimental effect: the maximum pitting depth obtained by immersing the 13Cr stainless steel sample in 120 ℃ NaCl solution for 30 days is 7.42 mu m, the maximum pitting depth obtained by immersing the 13Cr stainless steel sample in the same condition for 90 days is 17.5 mu m, and compared with the experimental results, the electrochemical polarization method can rapidly realize the occurrence and development of the pitting of the 13Cr stainless steel.
Claims (4)
1. A corrosion test method for rapidly realizing the occurrence and development of stainless steel pitting corrosion is characterized in that the corrosion test device for rapidly realizing the occurrence and development of stainless steel pitting corrosion comprises: the electrochemical workstation, the corrosion electrolytic cell, the test medium solution, the auxiliary electrode, the reference electrode, the working electrode and the vent pipe have the following specific structures:
a test medium solution is filled in the corrosion electrolytic cell, an auxiliary electrode, a reference electrode and a working electrode are arranged in the test medium solution, and a vent pipe of nitrogen is inserted in the test medium solution; the electrochemical workstation is provided with four binding clips, and is respectively connected with the auxiliary electrode, the reference electrode, the working electrode and the grounding wire through the four binding clips;
the corrosion test method for rapidly realizing the occurrence and development of the stainless steel pitting corrosion comprises the steps of firstly measuring corrosion potential of a stainless steel working electrode by using an electrochemical workstation open-circuit potential measurement mode, then measuring pitting potential and repassivation potential of the stainless steel working electrode by using a dynamic potential scanning mode, then selecting a potential value between the measured pitting potential and repassivation potential as polarization potential, and applying the selected polarization potential on the stainless steel working electrode by using an electrochemical workstation constant potential polarization mode, so that pitting corrosion generated by the stainless steel working electrode in the dynamic potential scanning stage continues to grow, pitting corrosion pits with different depths are obtained in different polarization time, and evaluating and comparing pitting corrosion resistance of stainless steel of different materials according to the result;
the corrosion test method for rapidly realizing the occurrence and development of stainless steel pitting corrosion comprises the following specific steps:
(1) Preparing corresponding test medium solution according to test requirements, and placing the test medium solution into a corrosion electrolytic cell;
(2) Placing the working electrode, the auxiliary electrode and the reference electrode which are connected with the lead in a corrosion electrolytic cell, and requiring all the electrodes to be completely immersed below the liquid level;
(3) After the working electrode is placed in the corrosion electrolytic cell for 15min, the open-circuit potential of the working electrode, namely the corrosion potential, is measured by using an electrochemical workstation open-circuit potential measurement mode;
(4) Anodic polarization was performed at a potential scan rate of 20mV/min from the corrosion potential using an electrochemical workstation potentiodynamic scan mode when the anodic current reached 500. Mu.A/cm 2 Then, retrace is carried out, and the scanning is stopped after the etching potential is returned;
(5) With a corresponding current density of 10 μA/cm on the anodic polarization curve 2 The potential value is used as the pitting potential of the stainless steel working electrode,taking the intersection point of the retrace curve and the anodic polarization curve as the repassivation potential of the stainless steel working electrode, and reading out the pitting corrosion potential and the repassivation potential according to the two requirements;
(6) And selecting a potential value as a polarization potential in the range from the measured repassivation potential to the pitting potential, and carrying out constant potential polarization on the working electrode by adopting a constant potential polarization mode of the electrochemical workstation so as to enable pitting corrosion generated by the working electrode in a potentiodynamic scanning stage to continue growing.
2. The method for rapidly achieving the occurrence and development of the pitting corrosion of the stainless steel according to claim 1, wherein the auxiliary electrode is a platinum electrode, the reference electrode is a saturated calomel electrode, and the working electrode is a stainless steel electrode.
3. The method for rapidly realizing the corrosion test of the occurrence and the development of the stainless steel pitting corrosion according to claim 1, wherein a working electrode binding clip WE, an auxiliary electrode binding clip CE, a reference electrode binding clip RE and a ground wire clip GOUND of the electrochemical workstation are respectively and correspondingly connected with a working electrode, an auxiliary electrode, a reference electrode and a ground wire, the working electrode, the auxiliary electrode and the reference electrode are placed in a corrosion electrolytic cell special for an electrochemical test experiment and are completely immersed below the liquid level of a test medium solution, so as to form the electrochemical workstation and an electrochemical three-electrode system test system.
4. The method for rapidly achieving the occurrence and development of the pitting corrosion of the stainless steel according to claim 1, wherein the step (1) is performed with oxygen removal by adopting a nitrogen oxygen-removing mode when the oxygen removal requirement exists.
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