CN108344679A - A method of characterization cast austenitic-ferritic stainless steel pitting corrosion - Google Patents
A method of characterization cast austenitic-ferritic stainless steel pitting corrosion Download PDFInfo
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Abstract
A method of cast austenitic ferritic stainless steel pitting corrosion is characterized by passivating film, belongs to corrosion technology field.Z3CN20.09M cast austenitics ferritic stainless steel is cut into 10mm × 10mm × 4mm samples after 475 DEG C of heat ageing different times, cleaning polishing is prepared into electrochemical sample, electrode is connected to immerse in the sulfuric acid solution of 0.5mol/L later, apply negative potential first and removes the passivating film formed in sample preparation, apply positive potential 0.5V again, 0.5~1 hour to prepare passivating film.After the sample that Passivation Treatment is crossed connects electrode, 30 minutes open circuit potential with acquisition stabilization in 3.5% sodium chloride solution are immersed.The case where test passivation membrane impedance is with potential change, it is 0.1~0.6V that electrochemical workstation, which scans potential range, and current potential increment is 0.01V, frequency 1000Hz.After the completion of test, calculates and draw Mott Schottky curves.According to formulaThe point defect concentration of austenite ferrite stainless steel surface passivated membrane is calculated by the slope of curve.Point defect concentration is bigger, shows that cast austenitic ferritic stainless steel pitting resistance is poorer.
Description
Technical field
The invention belongs to Corrosion of Stainless Steel technical fields, are related to a kind of by passivating film characterization cast austenitic-ferrite
The method of stainless steel pitting corrosion.
Background technology
Today's society energy shortage, problem of environmental pollution become increasingly conspicuous.Nuclear energy be acknowledged as reality, can replace on a large scale
For fossil energy, not only clean but also the economic energy.One loop of nuclear power station main pipeline is one of seven big key equipment of nuclear island, is referred to as
" aorta " of nuclear power station.Two generation Fortschrittlicher Druckwasser Reaktor Nuclear power plant main pipelines use Z3CN20.09M cast austenitics-ferrite
Heat ageing phenomenon can occur for stainless steel, high comprehensive performance, but the ferritic phase therein long service under high temperature and high pressure environment,
Lead to the performance for deteriorating material resistance to spot corrosion while material embrittlement.
Spot corrosion is most important failure mode outside cast austenitic-ferritic stainless steel de-stress corrosion cracking, borrosion hole one
Denier is formed, and the power with " deep-cutting " has prodigious hidden danger and destructiveness.Currently, main the having of pitting test for stainless steel method
Learn immersion and electrochemical method.Chemical immersion method impregnates stainless steel curved beam with the ferric trichloride that mass fraction is 6%, to bill of materials
Pitting number, borrosion hole size and depth etc. in plane product are evaluated.This method testing time is long, has destructiveness, and
Early stage spot corrosion can not be detected.Electrochemical method have many advantages, such as it is simple, quick, be widely used in material corrosion detection in, including
Constant potential critical pitting temperature method and dynamic potential scanning pitting potential method.But both electrochemical methods are all by obtaining stable state
The pitting corrosion of spot corrosion information evaluation material, and steady state point pit size majority is more than 100 microns.When materials microstructure occurs
When changing, spot corrosion being caused to germinate, electrochemical method is difficult to the relevant information of accurate evaluation spot corrosion generation.For example, Z3CN20.09M
Spinodal decomposition occurs for ferritic phase in cast austenitic-ferritic stainless steel Heat Ageing, generates nanoscale precipitated phase, occurs
Spot corrosion be just difficult to Conventional electrochemical method detect.
It is that formation that surface can spontaneous is one layer very thin and performance stabilization that stainless steel, which has the reason of excellent anticorrosive performance,
Passivating film.The local failure of passivating film easily causes spot corrosion.We have found previous research work, extend with thermal aging time,
Z3CN20.09M cast austenitics-ferritic stainless steel pitting resistance is remarkably decreased.By studying cast austenitic-ferrite
The characteristic of passivation film on stainless steel surface analyzes Z3CN20.09M cast austenitics-ferritic stainless steel caused by heat ageing degree difference
The difference of surface passivation film component, structure and chemical property helps to disclose cast austenitic-ferritic stainless steel heat ageing
The mechanism that nanocrystal induction spot corrosion occurs afterwards.
Invention content
The purpose of the present invention is to provide one kind characterizing cast austenitic-ferritic stainless steel pitting corrosion by passivating film
Method.Point caused by nanocrystalline phase is precipitated after can characterizing cast austenitic-ferritic stainless steel heat ageing using this method
Erosion, increases the confidence level of test.
A method of characterization cast austenitic-ferritic stainless steel pitting corrosion, it is characterised in that first in casting Ovshinsky
Body-ferrite stainless steel surface prepares passivating film, and cast austenitic-iron element is characterized by calculating the point defect concentration of passivating film
The pitting resistance of body stainless steel, is as follows:
1) test sample is prepared:By cast austenitic-ferritic stainless steel 475 DEG C of difference heat ageings 0,500,1000,
The sample of 10mm × 10mm × 4mm is cut into after 2000 hours, cleaning polishing is prepared into electrochemical sample;
2) electrochemical evaluation solution is prepared:The sulfuric acid solution and quality point that compound concentration is 0.5mol/L at ambient temperature
The sodium chloride solution that number is 3.5%;
3) Passivation Treatment:Prepared sulfuric acid solution is put into 25 DEG C of thermostat water baths and is kept the temperature, sample connects electrode
Immerse in solution later, the negative potential of application -1V first 5~10 minutes to remove the passivating film formed in sample preparation,
Apply positive potential 0.5V again, anodic oxidation 0.5~1 hour is to prepare passivating film.
4) Impedance measurement-current potential:The sodium chloride solution of preparation is put into 25 DEG C of thermostat water bath and is kept the temperature.It will be above-mentioned blunt
Change processed sample connection electrode, immerses 30 minutes open circuit potential with acquisition stabilization in solution.It is surveyed with electrochemical workstation
The case where examination passivation membrane impedance is with potential change, scanning range is -0.1~0.6V, and current potential increment is 0.01V, and frequency is
1000Hz;
5) point defect concentration of passivating film is calculated:Mott-Schottky curves are drawn, according to formulaThe point that austenite-ferrite stainless steel surface passivated membrane is calculated by the slope of curve lacks
Fall into concentration.In formula, C represents space charge interlayer capacitance, and ε is the relative dielectric constant of passivating film, ε0For permittivity of vacuum
(8.654×10-12F/m), e is electron charge (1.602 × 10-19C), NDFor donor concentration, E is externally-applied potential, EfbFor flat rubber belting
Current potential, k are Boltzmann (Boltzmann) constant (1.38066 × 10-23J/K), T is thermodynamic temperature.Point defect concentration is got over
Greatly, passivating film is more more easily damaged, and pitting resistance of stainless steel is poorer.
Further, ferrite content is 13% in above-mentioned cast austenitic-ferritic stainless steel.
The present invention is had the following advantages that compared with existing spot corrosion measuring technology and effect:
1. sample constant potential polarization rear surface in sulfuric acid is passivated, crevice corrosion occurs when avoiding electro-chemical test
Possibility, can more accurately characterize the pitting corrosion of cast austenitic-ferritic stainless steel.
2. damage of the electro-chemical test to sample can be reduced after sample to be tested surface passivating treatment, cast austenitic-is tested
Ferritic stainless steel passivation film properties can not only characterize the variation of pitting corrosion, and can further disclose the machine of spot corrosion generation
Reason.
3. can rapidly and accurately characterize cast austenitic-ferritic stainless steel heat ageing is precipitated nanometer crystalline phase induction spot corrosion hair
Raw phenomenon, it is with a high credibility.
Description of the drawings
Fig. 1 shows the Mott- of heat ageing different time (embodiment 1-4) cast austenitic-ferritic stainless steel passivating film
Schottky curves.As it can be seen that increasing with thermal aging time, passivating film point defects concentration increases, and shows that Z3CN20.09M is cast
Austenite-ferrite stainless steel pitting resistance declines.
Fig. 2 indicates heat ageing different time (embodiment 1-4) Z3CN20.09M cast austenitics-ferritic stainless steel passivation
The case where film spot defect density changes.
Specific implementation mode
Embodiment 1
Original Z3CN20.09M cast austenitics-ferritic stainless steel is cut into the sample of 10mm × 10mm × 4mm, clearly
It is prepared into electrochemical sample after washing polishing, electrode is connected and immerses in the sulfuric acid solution of 0.5mol/L later, apply negative potential-first
1V to remove the passivating film formed in sample preparation, then applies positive potential 0.5V in 5 minutes, prepares passivating film within 1 hour.It is blunt
Change after processed sample connects electrode, immerses in 3.5% sodium chloride solution 30 minutes to obtain stable open circuit electricity
Position.The case where impedance of passivating film is with potential change is tested, it is -0.1~0.6V, current potential that electrochemical workstation, which scans potential range,
Increment is 0.01V, frequency 1000Hz.After the completion of test, calculates and draw Mott-Schottky curves, according to formulaZ3CN20.09M cast austenitics-ferrite stainless is calculated by the slope of curve (Fig. 1)
The point defect concentration of steel passivating film.Z3CN20.09M cast austenitics-ferritic stainless steel point defect concentration of non-heat ageing is
1.3518×1021(Fig. 2).
Embodiment 2
Z3CN20.09M cast austenitics-ferritic stainless steel 475 DEG C of heat ageings cut into after 500 hours 10mm ×
The sample of 10mm × 4mm, cleaning polishing are prepared into electrochemical sample, connect the sulfuric acid solution of immersion 0.5mol/L after electrode
In, apply negative potential -1V first, to remove the passivating film formed in sample preparation, then apply positive potential 0.5V within 8 minutes,
Prepare passivating film within 0.5 hour.After the sample that Passivation Treatment is crossed connects electrode, 30 points are immersed in 3.5% sodium chloride solution
Clock is to obtain stable open circuit potential.The case where impedance of passivating film is with potential change is tested, electrochemical workstation scans current potential
Ranging from -0.1~0.6V, current potential increment are 0.01V, frequency 1000Hz.After the completion of test, calculates and draw Mott-
Schottky curves, according to formulaZ3CN20.09M is calculated by the slope of curve (Fig. 1)
The point defect concentration of cast austenitic-ferritic stainless steel passivating film, 500 hours Z3CN20.09M of heat ageing cast Ovshinsky
Body-ferritic stainless steel point defect concentration is 1.5135 × 1021(Fig. 2).
Embodiment 3
Z3CN20.09M cast austenitics-ferritic stainless steel 475 DEG C of heat ageings cut into after 1000 hours 10mm ×
The sample of 10mm × 4mm, cleaning polishing are prepared into electrochemical sample, connect the sulfuric acid solution of immersion 0.5mol/L after electrode
In, apply negative potential -1V first, to remove the passivating film formed in sample preparation, then apply positive potential 0.5V within 10 minutes,
Prepare passivating film within 1 hour.After the sample that Passivation Treatment is crossed connects electrode, immerse in 3.5% sodium chloride solution 30 minutes
To obtain stable open circuit potential.The case where impedance of passivating film is with potential change is tested, electrochemical workstation scans current potential model
It encloses for -0.1~0.6V, current potential increment is 0.01V, frequency 1000Hz.After the completion of test, calculates and draw Mott-
Schottky curves, according to formulaAustenite-iron element is calculated by the slope of curve (Fig. 1)
The point defect concentration of body stainless steel surface passivating film, 1000 hours Z3CN20.09M of heat ageing cast austenitics-ferrite is not
The steel point defect concentration that becomes rusty is 1.6243 × 1021(Fig. 2).
Embodiment 4
Z3CN20.09M cast austenitics-ferritic stainless steel 475 DEG C of heat ageings cut into after 2000 hours 10mm ×
The sample of 10mm × 4mm, cleaning polishing are prepared into electrochemical sample, connect the sulfuric acid solution of immersion 0.5mol/L after electrode
In, apply negative potential -1V first, to remove the passivating film formed in sample preparation, then apply positive potential 0.5V within 10 minutes,
Prepare passivating film within 0.5 hour.After the sample that Passivation Treatment is crossed connects electrode, 30 points are immersed in 3.5% sodium chloride solution
Clock is to obtain stable open circuit potential.The case where impedance of passivating film is with potential change is tested, electrochemical workstation scans current potential
Ranging from -0.1~0.6V, current potential increment are 0.01V, frequency 1000Hz.After the completion of test, calculates and draw Mott-
Schottky curves, according to formulaAustenite-iron element is calculated by the slope of curve (Fig. 1)
The point defect concentration of body stainless steel surface passivating film, 2000 hours Z3CN20.09M of heat ageing cast austenitics-ferrite is not
The steel point defect concentration that becomes rusty is 2.1606 × 1021(Fig. 2).
Claims (2)
1. a kind of method of characterization cast austenitic-ferritic stainless steel pitting corrosion, it is characterised in that first in cast austenitic-
Ferrite stainless steel surface prepares passivating film, and cast austenitic-ferrite is characterized by calculating the point defect concentration of passivating film
The pitting resistance of stainless steel, is as follows:
1) test sample is prepared:By cast austenitic-ferritic stainless steel in 475 DEG C of difference heat ageings 0,500,1000,2000
The sample of 10mm × 10mm × 4mm is cut into after hour, cleaning polishing is prepared into electrochemical sample;
2) electrochemical evaluation solution is prepared:The sulfuric acid solution and mass fraction that compound concentration is 0.5mol/L at ambient temperature be
3.5% sodium chloride solution;
3) Passivation Treatment:Prepared sulfuric acid solution is put into 25 DEG C of thermostat water baths and is kept the temperature, sample connects after electrode
It immerses in solution, the negative potential of application -1V first 5~10 minutes is to remove the passivating film formed in sample preparation, then applies
Add positive potential 0.5V, anodic oxidation 0.5~1 hour is to prepare passivating film;
4) Impedance measurement-current potential:The sodium chloride solution that step 2) is prepared is put into 25 DEG C of thermostat water bath and is kept the temperature;By step
3) the sample connection electrode that Passivation Treatment is crossed immerses 30 minutes open circuit potential with acquisition stabilization in solution;Use electrochemical operation
The case where test passivation membrane impedance stand with potential change, scanning range is -0.1~0.6V, and current potential increment is 0.01V, and frequency is
1000Hz;
5) point defect concentration of passivating film is calculated:Mott-Schottky curves are drawn, according to formulaThe point that austenite-ferrite stainless steel surface passivated membrane is calculated by the slope of curve lacks
Fall into concentration;In formula, C represents space charge interlayer capacitance, and ε is the relative dielectric constant of passivating film, ε0For permittivity of vacuum
(8.654×10-12F/m), e is electron charge (1.602 × 10-19C), NDFor donor concentration, E is externally-applied potential, EfbFor flat rubber belting
Current potential, k are Boltzmann constant 1.38066 × 10-23J/K, T are thermodynamic temperature;Point defect concentration is bigger, and passivating film more holds
It is easily destroyed, pitting resistance of stainless steel is poorer.
2. a kind of method of characterization cast austenitic-ferritic stainless steel pitting corrosion as described in claim 1, it is characterised in that
Ferrite content is 13% in the cast austenitic-ferritic stainless steel.
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Cited By (4)
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CN110274808A (en) * | 2019-07-05 | 2019-09-24 | 北华航天工业学院 | A kind of detection method of stainless steel point borrosion hole inside corrosion product concentration |
CN110618088A (en) * | 2019-08-12 | 2019-12-27 | 中车青岛四方机车车辆股份有限公司 | Metal material surface passive film testing device |
CN110987784A (en) * | 2019-12-06 | 2020-04-10 | 西北工业大学 | Quantitative characterization method for electrochemical corrosion resistance of nickel-based alloy |
CN113063830A (en) * | 2020-01-02 | 2021-07-02 | 中国石油化工股份有限公司 | Rapid screening method of corrosion inhibitor under high-salinity water condition |
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CN113063830A (en) * | 2020-01-02 | 2021-07-02 | 中国石油化工股份有限公司 | Rapid screening method of corrosion inhibitor under high-salinity water condition |
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