CN103543097A - Electrochemical method for determining inter-crystalline corrosion sensibility of austenitic stainless steel - Google Patents
Electrochemical method for determining inter-crystalline corrosion sensibility of austenitic stainless steel Download PDFInfo
- Publication number
- CN103543097A CN103543097A CN201310543201.1A CN201310543201A CN103543097A CN 103543097 A CN103543097 A CN 103543097A CN 201310543201 A CN201310543201 A CN 201310543201A CN 103543097 A CN103543097 A CN 103543097A
- Authority
- CN
- China
- Prior art keywords
- stainless steel
- austenitic stainless
- electrochemical
- impedance spectroscopy
- electrochemical impedance
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
- Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
Abstract
The invention discloses an electrochemical method for determining the inter-crystalline corrosion sensibility of austenitic stainless steel. The electrochemical method comprises the following steps: (1) carrying out passivating treatment; (2) measuring an electrochemical impedance spectroscopy; and (3) fitting and analyzing the measured electrochemical impedance spectroscopy and evaluating the inter-crystalline corrosion sensibility of the austenitic stainless steel. According to the method, the change of the inter-crystalline corrosion sensibility of the austenitic stainless steel can be judged rapidly and accurately by the electrochemical impedance spectroscopy and the impedance spectroscopy is further analyzed and the inter-crystalline corrosion degree can be evaluated quantitatively by through an equivalent circuit.
Description
Technical field
The present invention relates to metal material field, be specifically related to a kind of electrochemical method of measuring Intergranular Corrosion of Austenitic Stainless Steel susceptibility.
Background technology
The austenitic stainless steel of widespread use at present is generally applied in harsh corrosion environment, and intercrystalline corrosion is a kind of main Corrosion Types.Intercrystalline corrosion can cause its mechanical property to decline rapidly.The corrosion among crystalline grains research of austenitic stainless steel is one of research emphasis in recent years.
At present, stainless intercrystalline corrosion evaluation method mainly comprises copper-copper sulphate-sulfuric acid process, oxalic acid etch method, iron sulfate-sulfuric acid etch method etc., and these methods all have the shortcomings such as length destructive or consuming time.
Galvanochemistry reactivation (EPR) be generally acknowledge at present a kind of fast, the electrochemical method of Nondestructive Evaluation stainless steel intercrystalline corrosion susceptibility, there is the feature of accurate quantitative analysis.The general reactivation rate R that adopts
a=I
r/ I
aevaluate Susceptibility To Intergranular Corrosion.Reactivation rate R
abe worth greatlyr, Susceptibility To Intergranular Corrosion is higher.
Summary of the invention
For solving the problems of the technologies described above, the present invention aims to provide a kind of electrochemical method of measuring Intergranular Corrosion of Austenitic Stainless Steel susceptibility.
Principle of the present invention is: according to " the poor chromium of crystal boundary that Carbide Precipitation causes " theory, and heating or Slow cooling in sensitizing temperature (450-900 ℃) scope, carbon tends to chromium and iron in conjunction with forming complicated carbonide (CrFe)
23c
6, from oversaturated austenite, separate out and be distributed on crystal boundary, easily there is intercrystalline corrosion.Electrochemical impedance spectroscopy belongs to galvanochemistry transient test technology, is a kind of effective ways of measuring material and surface property thereof.At austenitic stainless steel grain boundaries, do not exist or only have a small amount of chromium to separate out (as the stainless steel of solid solution state), the passivating film that can generate through Passivation Treatment rear surface is complete, and matrix is had to protectiveness.After Ageing Treatment, the poor chromium of the grain boundaries of austenitic stainless steel, chromium content is lower than 12% time, and the passivating film after Passivation Treatment is imperfect.Electrochemical impedance spectroscopy can accurately, promptly reflect the passivating film information of stainless steel surfaces.When surperficial passivating film is complete, in etchant solution, impedance spectrum shows as a time constant; When causing due to the poor chromium of grain boundaries that passivating film is imperfect or unstable to be caused intercrystalline corrosion occurs, impedance spectrum shows as two time constants, and wherein the resistance value of low frequency end can further react intercrystalline corrosion degree.
The electrochemical method of mensuration Intergranular Corrosion of Austenitic Stainless Steel susceptibility provided by the invention, comprises the steps:
1) austenitic stainless steel to be measured is carried out to Passivation Treatment;
2) measuring process 1) austenitic stainless steel electrochemical impedance spectroscopy after processing;
3) to step 2) electrochemical impedance spectroscopy that records carries out matching and parsing, evaluates Intergranular Corrosion of Austenitic Stainless Steel susceptibility.
Wherein, described in step 1), Passivation Treatment can be chemical passivation processing or electrochemical passivation processing.Described chemical passivation is treated to and in passivating dip, is incubated 30min by being immersed at 80 ℃ of austenitic stainless steels to be measured.Described passivating dip is 10ml/LH
2sO
4+ 20g/LKNO
3aqueous solution.
Wherein, step 2) condition of described Using Electrochemical Impedance Spectroscopy is: containing Cl
-etchant solution in, working electrode is austenitic stainless steel, auxiliary electrode is platinized platinum, contrast electrode is saturated calomel electrode (SCE), carries out electrochemical impedance spectroscopy measurement after system reaches steady state (SS), frequency range is 10
5hz～10mHz, ac-excited signal amplitude is 10mV, measures and carries out under open circuit potential.
The described Cl that contains
-etchant solution be preferably the NaCl aqueous solution of quality percentage composition 3.5%.
The time that described system reaches steady state (SS) is preferably 1 hour.
The application of the electrochemical method that the present invention also provides described mensuration Intergranular Corrosion of Austenitic Stainless Steel susceptibility in evaluating stainless steel intercrystalline corrosion susceptibility.
Advantage of the present invention is:
The present invention can judge the variation of the Susceptibility To Intergranular Corrosion of austenitic stainless steel quickly and accurately by Eis Characteristics, and by equivalent electrical circuit, the further parsing of impedance spectrum is evaluated to intercrystalline corrosion degree quantitatively.
Accompanying drawing explanation
Fig. 1 is that the Super304H of solid solution state and Sensitized soaks the electrochemical impedance spectroscopy after 1h in solution.
Fig. 2 is the equivalent electrical circuit of matching solid solution state (a) and Sensitized (b) Super304H electrochemical impedance spectroscopy.
Fig. 3 is the metallographic structure after solid solution state (a) and Sensitized (b) Super304H EPR experiment.
Fig. 4 is the electrochemical impedance spectroscopy of the HR3C of 700 ℃ of sensitization 1h, 3h.
Embodiment
Following examples are used for illustrating the present invention, but are not used for limiting the scope of the invention.The present invention's chemical reagent used is all commercially available.
Embodiment 1
Measure solid solution state Super304H and 650 ℃ of sensitizations, process the corrosion among crystalline grains of the Super304H of 50h.Super304H is the Super304H of power plant.
1, stainless chemical passivation is processed: at 80 ℃, in passivating dip, be incubated 30min and carry out chemical passivation processing.Described passivating dip is 10ml/LH
2sO
4(be that every liter of passivating dip is containing the 98%H of 10ml
2sO
4)+20g/L KNO
3aqueous solution.
2, electrochemical impedance spectrometry: in etchant solution 3.5%NaCl aqueous solution, working electrode is Super304H austenitic stainless steel to be measured, and auxiliary electrode is platinized platinum, and contrast electrode is saturated calomel electrode (SCE).For making system reach steady state (SS), carry out electrochemical impedance spectroscopy measurement (the German Zahner Zennium of company electrochemical workstation) soak 1h in etchant solution after, frequency range is 10
5hz～10mHz, ac-excited signal amplitude is 10mV, measures and carries out under open circuit potential.Fig. 1 is that the Super304H of solid solution state and Sensitized soaks the electrochemical impedance spectroscopy after 1h in solution.
3, impedance spectrum is carried out to matching and parsing.Because of the Super304H austenitic stainless steel of solid solution state in passivating dip, can generate the passivating film of even compact, thereby impedance spectrum shows a time constant.And Super304H after sensitization is due to the poor chromium of crystal boundary, the imperfect densification of the passivating film of grain boundaries, stainless steel generation intercrystalline corrosion.Impedance spectrum shows as two time constants.The Super304H of solid solution state adopts equivalent electrical circuit as shown in Figure 2 (a) shows to carry out matching; The Super304H of Sensitized adopts equivalent electrical circuit as shown in Fig. 2 (b) to carry out matching.Fitting result is as shown in table 1.
The Super304H electrochemical impedance spectroscopy fitting result of table 1 solid solution state and Sensitized
Fig. 3 is for adopting the rear solid solution state of galvanochemistry reactivation test and the stainless metallographic structure of Sensitized Super304.
Embodiment 2
With 700 ℃ of sensitizations of method electrochemical impedance spectroscopy test of the present invention, process the corrosion among crystalline grains of the HR3C austenitic stainless steel of 1h and 3h.HR3C austenitic stainless steel is commercially available.
1, stainless passivation: 10ml/LH
2sO
4(98%)+20g/L KNO
3in solution, at 80 ℃, be incubated 30min and carry out chemical passivation processing.
2, electrochemical impedance spectrometry: in 3.5%NaCl solution, working electrode is HR3C stainless steel to be measured, and auxiliary electrode is platinized platinum, and contrast electrode is saturated calomel electrode (SCE).For making system reach steady state (SS), carry out electrochemical impedance spectroscopy measurement (the German Zahner Zennium of company electrochemical workstation) soak 1h in etchant solution after, frequency range is 10
5hz～10mHz, ac-excited signal amplitude is 10mV, measures and carries out under open circuit potential.Fig. 4 is 700 ℃ of sensitization 1h, the electrochemical impedance spectroscopy of the HR3C of 3h.
3, impedance spectrum is resolved.Adopt the equivalent electrical circuit as shown in Fig. 2 (b) to carry out matching.Fitting result is as shown in table 2.
The electrochemical impedance spectroscopy fitting result of the HR3C of table 2700 ℃ sensitization 1h and 3h
Galvanochemistry reactivation is measured the R that the HR3C austenitic stainless steel of 1h and 3h is processed in 700 ℃ of sensitizations
avalue is respectively 0.40 and 0.66, and the latter's intergranular susceptibility is higher than the former.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, do not departing under the prerequisite of the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (8)
1. an electrochemical method of measuring Intergranular Corrosion of Austenitic Stainless Steel susceptibility, comprises the steps:
1) austenitic stainless steel to be measured is carried out to Passivation Treatment;
2) measuring process 1) austenitic stainless steel electrochemical impedance spectroscopy after processing;
3) to step 2) electrochemical impedance spectroscopy that records carries out matching and parsing, evaluates Intergranular Corrosion of Austenitic Stainless Steel susceptibility.
2. method according to claim 1, is characterized in that, Passivation Treatment can be chemical passivation processing or electrochemical passivation is processed described in step 1).
3. method according to claim 2, is characterized in that, described chemical passivation is treated to and in passivating dip, is incubated 30min by being immersed at 80 ℃ of austenitic stainless steels to be measured.
4. method according to claim 3, is characterized in that, described passivating dip is 10ml/LH
2sO
4+ 20g/LKNO
3aqueous solution.
5. method according to claim 1, is characterized in that step 2) condition of described Using Electrochemical Impedance Spectroscopy is: containing Cl
-etchant solution in, working electrode is austenitic stainless steel, auxiliary electrode is platinized platinum, contrast electrode is saturated calomel electrode (SCE), carries out electrochemical impedance spectroscopy measurement after system reaches steady state (SS), frequency range is 10
5hz～10mHz, ac-excited signal amplitude is 10mV, measures and carries out under open circuit potential.
6. method according to claim 5, is characterized in that, described in contain Cl
-etchant solution be preferably the NaCl aqueous solution of quality percentage composition 3.5%.
7. method according to claim 5, is characterized in that, the time that described system reaches steady state (SS) is preferably 1 hour.
8. the application of the method described in claim 1-7 any one in evaluating stainless steel intercrystalline corrosion susceptibility.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310543201.1A CN103543097A (en) | 2013-11-05 | 2013-11-05 | Electrochemical method for determining inter-crystalline corrosion sensibility of austenitic stainless steel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310543201.1A CN103543097A (en) | 2013-11-05 | 2013-11-05 | Electrochemical method for determining inter-crystalline corrosion sensibility of austenitic stainless steel |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103543097A true CN103543097A (en) | 2014-01-29 |
Family
ID=49966766
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310543201.1A Pending CN103543097A (en) | 2013-11-05 | 2013-11-05 | Electrochemical method for determining inter-crystalline corrosion sensibility of austenitic stainless steel |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103543097A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104567657A (en) * | 2014-12-23 | 2015-04-29 | 天津大学 | Method for representing metal surface corrosion roughness based on electrochemical impedance spectra |
| CN107462513A (en) * | 2017-07-03 | 2017-12-12 | 岭东核电有限公司 | The decision method and decision-making system of the intergranular stress corrosion of nuclear power station steam generator |
| CN108344679A (en) * | 2018-01-18 | 2018-07-31 | 北京科技大学 | A method of characterization cast austenitic-ferritic stainless steel pitting corrosion |
| CN109030338A (en) * | 2018-09-18 | 2018-12-18 | 西安交通大学 | A kind of method of electro-catalysis chemical attack original austenite grain |
| CN109632916A (en) * | 2018-12-20 | 2019-04-16 | 西安铂力特增材技术股份有限公司 | A method of measurement increasing material manufacturing titanium alloy surface Stability of Passive Film |
| CN110987786A (en) * | 2019-12-26 | 2020-04-10 | 国网四川省电力公司电力科学研究院 | Power transformer and metal corrosion state judgment method of support framework of power transformer |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101334353A (en) * | 2008-08-01 | 2008-12-31 | 厦门大学 | Multifunctional sensor for monitoring reinforced concrete structure erosion |
| CN101571473A (en) * | 2008-04-30 | 2009-11-04 | 中国科学院金属研究所 | Test method for stimulating corrosion process of stainless steel in atmospheric environment in salt lake |
| CN102590298A (en) * | 2012-01-20 | 2012-07-18 | 中国科学院金属研究所 | Method for testing microbiological corrosion resisting performance of antibacterial stainless steel by electrochemical method |
-
2013
- 2013-11-05 CN CN201310543201.1A patent/CN103543097A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101571473A (en) * | 2008-04-30 | 2009-11-04 | 中国科学院金属研究所 | Test method for stimulating corrosion process of stainless steel in atmospheric environment in salt lake |
| CN101334353A (en) * | 2008-08-01 | 2008-12-31 | 厦门大学 | Multifunctional sensor for monitoring reinforced concrete structure erosion |
| CN102590298A (en) * | 2012-01-20 | 2012-07-18 | 中国科学院金属研究所 | Method for testing microbiological corrosion resisting performance of antibacterial stainless steel by electrochemical method |
Non-Patent Citations (5)
| Title |
|---|
| CHING-AN HUANG ET AL: "The electrochemical behavior of austenitic stainless steel with different degrees of sensitization in the transpassive potential region in 1 M H2SO4 containing chloride", 《CORROSION SCIENCE》 * |
| 张春雷等: "Super304H奥氏体不锈钢晶间腐蚀的研究进展", 《特殊钢》 * |
| 张春雷等: "Super304H奥氏体不锈钢的晶间腐蚀性能", 《长沙理工大学学报(自然科学版)》 * |
| 查小琴等: "不锈钢晶间腐蚀测试方法", 《材料开发与应用》 * |
| 秦丽雁等: "304不锈钢晶间腐蚀过程中的电化学阻抗谱特征", 《中国腐蚀与防护学报》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104567657A (en) * | 2014-12-23 | 2015-04-29 | 天津大学 | Method for representing metal surface corrosion roughness based on electrochemical impedance spectra |
| CN107462513A (en) * | 2017-07-03 | 2017-12-12 | 岭东核电有限公司 | The decision method and decision-making system of the intergranular stress corrosion of nuclear power station steam generator |
| CN108344679A (en) * | 2018-01-18 | 2018-07-31 | 北京科技大学 | A method of characterization cast austenitic-ferritic stainless steel pitting corrosion |
| CN109030338A (en) * | 2018-09-18 | 2018-12-18 | 西安交通大学 | A kind of method of electro-catalysis chemical attack original austenite grain |
| CN109632916A (en) * | 2018-12-20 | 2019-04-16 | 西安铂力特增材技术股份有限公司 | A method of measurement increasing material manufacturing titanium alloy surface Stability of Passive Film |
| CN110987786A (en) * | 2019-12-26 | 2020-04-10 | 国网四川省电力公司电力科学研究院 | Power transformer and metal corrosion state judgment method of support framework of power transformer |
| CN110987786B (en) * | 2019-12-26 | 2022-08-09 | 国网四川省电力公司电力科学研究院 | Power transformer and metal corrosion state judgment method of support framework of power transformer |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103543097A (en) | Electrochemical method for determining inter-crystalline corrosion sensibility of austenitic stainless steel | |
| CN109085213B (en) | Stress corrosion crack initiation life prediction method | |
| Zhang et al. | A new criterion to determine the critical pitting temperature (CPT) based on electrochemical noise measurement | |
| CN1800822A (en) | Method for evaluating pitting resistance performance of material | |
| Cai et al. | Comparative studies on passivation and corrosion behaviors of two types of steel bars in simulated concrete pore solution | |
| Sun et al. | A comparative study on potentiodynamic and potentiostatic critical pitting temperature of austenitic stainless steels | |
| CN100547343C (en) | A kind of method of continuously monitoring metal material corrosion depth | |
| Man et al. | Characterization of the passive film and corrosion of martensitic AM355 stainless steel | |
| CN105973970B (en) | A method of detection austenitic stainless steel corrosion susceptibility | |
| CN105372321A (en) | Uranyl ion sensor based on target molecule hairpin assembly, and preparation method and application thereof | |
| CN107367595A (en) | A kind of method that micro-parameter based on low carbon-structural steel determines its target capabilities | |
| US3428532A (en) | Method for identifying metals and alloys | |
| CN105929011A (en) | Corrosive pitting detection method for intergranular corrosion of stainless steel | |
| CN108037039A (en) | A kind of efficient, method of Accurate Determining stainless steel critical pitting temperature | |
| Li et al. | Pitting corrosion of super martensitic stainless steel 00Cr13Ni5Mo2 | |
| Bastidas et al. | A stochastic approach to study localized corrosion of AISI 304L and AISI 316L stainless steels as a function of potential scan rate | |
| Jegdić et al. | Testing of intergranular and pitting corrosion in sensitized welded joints of austenitic stainless steel | |
| Runcheng et al. | Electrochemical study on corrosion behaviors of P110 casing steel in a carbon dioxide-saturated oilfield formation water | |
| Jiao et al. | Early identification of stress corrosion cracking of P110 low alloy steel in downhole fluid by electrochemical noise measurement | |
| Bihade et al. | Analysis of electrochemical current noise from metastable pitting of SS304L in NaCl solutions | |
| CN216900315U (en) | Critical point corrosion temperature test system | |
| Huang et al. | Galvanic corrosion behavior of bainite weathering steel welded joint in simulated marine atmosphere environment based on capillary microcell | |
| Kovalenko et al. | Corrosion of the internal wall of a field gas pipeline | |
| Ivanov et al. | Use of impedance spectroscopy for evaluating pipe steel susceptibility towards hydrogenation and hydrogen cracking | |
| Kozlova et al. | Corrosion Monitoring of Pipelines of Heat-Supply Systems Based on Gravimetric and Electrochemical Methods of Analysis |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20140129 |
|
| RJ01 | Rejection of invention patent application after publication |