CN101762454B - Dual-ring electrochemical dynamic potential reactivating evaluating method for diphase stainless steel intercrystalline corrosion sensitivity - Google Patents
Dual-ring electrochemical dynamic potential reactivating evaluating method for diphase stainless steel intercrystalline corrosion sensitivity Download PDFInfo
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Abstract
The invention discloses a dual-ring electrochemical dynamic potential reactivating evaluating method for diphase stainless steel intercrystalline corrosion sensitivity, which comprises the following steps: first, pre-treating specimen; second, preparing electrochemical evaluating solution;third, establishing electrochemical evaluating system; fourth, DL-EPR testing; fifth, judging intercrystalline corrosion sensitivity. The invention adopts mixture-solution of sulphuric and hydrochloric acids as the evaluating solution, can solve the technical problems of passive potential and corrosion potential, separate the passive potential and corrosion potential according to the concrete specimen of a diphase stainless steel, thereby realizing effective and accurate judgment about the diphase stainless steel intercrystalline corrosion sensitivity, establishing the dual-ring electrochemical dynamic potential reactivating evaluating method for diphase stainless steel intercrystalline corrosion sensitivity according to the diphase stainless steel features, and further obtaining judging criterion for diphase stainless steel intercrystalline corrosion sensitivity. The method has simple process, high sensitivity, good stability, high operability, economic property and environmental-protection.
Description
Technical field
The invention belongs to two phase stainless steel Susceptibility To Intergranular Corrosion assessment technique field, be specifically related to a kind of dicyclo galvanochemistry potentiokinetic reactivation evaluation assessment for the two phase stainless steel Susceptibility To Intergranular Corrosion.
Background technology
Two phase stainless steel (Duplex Stainless Steel, be abbreviated as DSS) have the advantage of austenite and ferritic stainless steel concurrently, good corrosion-resistant and mechanical property is arranged, therefore in oil, chemical industry, synthon and Petroleum refining with the [S.Bernhardsson that is widely used in the corrosivity commercial production such as transport, in:Proceedings of the Conference Duplex Stainless steel ' s91, Beaune, Les editions dephysique, 1991, pp.185.].Yet, unsuitable thermal treatment and welding technology can make two phase stainless steel separate out a large amount of σ mutually, the secondary phase such as nitride and carbonide, the appearance meeting of these secondary phases makes a big impact to its Susceptibility To Intergranular Corrosion.σ separates out mutually particularly fast and precipitate size is large, has a strong impact on corrosive nature [J.O.Nilsson, Mater.Sci.Technol., 8 (1992) 685. of material; N.Lopez, M.Cid, M.Puiggali, Corros.Sci., 41 (1999) 1615.; M.E.Wilms, V.J.Gadgil, J.M.Krougmen, F.P.Ijsseling, Corros.Sci., 36 (1994) 871.].Therefore need the content of research σ phase and the relation of heat treatment time, and seek a kind of standard that can estimate σ relative material corrosion resistance influence degree.
Stainless steel may strictly not cause sensitization phenomenon owing to controlling of production process in process of production.Austenitic stainless steel whether the evaluation of sensitization general what adopt is GB 4334.1 " stainless steel 10% oxalic acid etch test method ", but this method is only for austenitic stainless steel, for two phase stainless steel and inapplicable.Two phase stainless steel is the stainless steel grade that upgrades than austenitic stainless steel, has the advantage of austenite and ferritic stainless steel concurrently, and good corrosion-resistant and mechanical property is arranged, but does not have the accurately method of inspection of the sensitization problem of two phase stainless steel at present.
DL-EPR test system in the past is mainly for developing at single austenitic stainless steel, and the general main medium that adopts is the dilute acid soln that contains thiocyanate ion.Present stage does not have the detection method for two phase stainless steel
Summary of the invention
The objective of the invention is in order to solve the detection of two phase stainless steel sensitization sensitive question, a kind of dicyclo galvanochemistry potentiokinetic reactivation evaluation assessment of two phase stainless steel Susceptibility To Intergranular Corrosion is provided, the method technique is simple, economic environmental protection.
In order to realize the foregoing invention purpose, technical scheme of the present invention is as follows:
A kind of dicyclo galvanochemistry potentiokinetic reactivation evaluation assessment may further comprise the steps:
1) sample pretreatment: with two phase stainless steel sample polishing to be measured, then through mechanical buffing and oil removal treatment;
2) preparation of electrochemical evaluation solution: the sulfuric acid of preparing at ambient temperature and the mixed solution of hydrochloric acid;
3) foundation of electrochemical evaluation system: in step 2) set up the standard three-electrode system that is consisted of by auxiliary electrode, contrast electrode, working electrode in the evaluation solution of preparation;
4) DL-EPR test: control electric potential scanning with electrochemical workstation, from corrosion potential, make the anode polarization electric potential scanning with certain speed, after sweeping to passivation potential 400mV, make to be scanned up to corrosion potential in the other direction with same sweep speed, thereby measure activation electric current I a and reactivation electric current I r;
5) Susceptibility To Intergranular Corrosion is judged: judge the sample Susceptibility To Intergranular Corrosion with ratio R a=Ir/Ia * 100%.
Polishing is with 180～1500 model sand paper the two phase stainless steel specimen surface to be polished in the above-mentioned step (1), makes the roughness of this two phase stainless steel specimen surface consistent with the roughness of described sand paper.
Sulfuric acid solution concentration in the evaluation solution of above-mentioned step (2) is 1～3mol/L, and concentration of hydrochloric acid solution is 0.1～2mol/L, and the preferably sulfuric acid solution concentration is 2mol/L, and concentration of hydrochloric acid solution is 1mol/L.
Auxiliary electrode is platinized platinum in the above-mentioned step (3), and contrast electrode is saturated calomel electrode, and working electrode is sample.Step (3) electrochemical evaluation system is the technology that those skilled in the art commonly uses.In addition, the present invention.Step (3) electrochemical evaluation system also connects wire to sample and inlays insulation processing through epoxy resin, and the slit prevents crevice corrosion with the silica gel sealing of hole between stainless steel and the epoxy resin.Sample is used washed with de-ionized water before test.
Above-mentioned step (4) Anodic polarized potential sweep speed is 0.5～5mv/s, preferred 1.66mv/s; Current potential when passivation potential is forward scan during maximum anode current, such as 400mV, the current potential when corrosion potential is reverse scan during maximum anode current.
The temperature of DL-EPR test electrochemical evaluation solution is 20～40 ℃ in the above-mentioned step (4), preferred 30 ℃.
Two phase stainless steel Susceptibility To Intergranular Corrosion dicyclo galvanochemistry potentiokinetic reactivation evaluation assessment of the present invention is used for estimating 2205 two phase stainless steel Susceptibility To Intergranular Corrosions.
The present invention adopts sulfuric acid (H
2SO
4) and the mixed solution of hydrochloric acid (HCl) as estimating solution, can solve passivation potential and corrosion potential technical barrier, can be according to a concrete sample of two phase stainless steel, passivation potential and corrosion potential are well separated, thereby reach the effect of effectively and accurately judging two phase stainless steel intercrystalline corrosion power, the two phase stainless steel Susceptibility To Intergranular Corrosion dicyclo galvanochemistry potentiokinetic reactivation evaluation assessment of setting up according to the two phase stainless steel characteristic simultaneously, obtain two phase stainless steel Susceptibility To Intergranular Corrosion criterion, the method technique is simple, highly sensitive, good stability, workable, and economic environmental protection.
Description of drawings
Fig. 1 is the SEM figure of the different sensitization of standard 2205 two phase stainless steels: (a) process 5h, (c) 800 ℃ of sensitizations processing 4h, (d) 800 ℃ of sensitizations processing 11h without sensitization sample, (b) 800 ℃ of sensitizations;
Fig. 2 is the DL-EPR test result of 2205 test materials of different sensitization: (a) without sensitization material, (b) slight sensitization material, (c) serious sensitization material;
Fig. 3 is the pattern result after the DL-EPR of 2205 test materials of different sensitization tests: (a) without sensitization material, (b) slight sensitization material, (c) serious sensitization material, (d) serious sensitization material.
Embodiment
In order to make the technical problem to be solved in the present invention, technical scheme and beneficial effect clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.
The invention provides a kind of two phase stainless steel Susceptibility To Intergranular Corrosion dicyclo galvanochemistry potentiokinetic reactivation evaluation assessment, may further comprise the steps:
1) sample pretreatment: two phase stainless steel sample to be measured is polished step by step through sand paper first, then through mechanical buffing to 1.5 μ m and oil removal treatment;
2) preparation of electrochemical evaluation solution: the mixed solution of preparing at ambient temperature sulfuric acid and hydrochloric acid, sulfuric acid solution concentration is 1～3mol/L in this mixed solution, concentration of hydrochloric acid solution is 0.1～2mol/L, and the preferably sulfuric acid solution concentration is 2mol/L, and concentration of hydrochloric acid solution is 1mol/L;
3) foundation of electrochemical evaluation system: in step 2) set up the standard three-electrode system that is consisted of by auxiliary electrode, contrast electrode, working electrode in the evaluation solution of preparation, wherein, auxiliary electrode is platinized platinum, contrast electrode is saturated calomel electrode, working electrode is sample, the temperature of estimating solution is 20～40 ℃, preferred 30 ℃;
4) DL-EPR test: control electric potential scanning with electrochemical workstation, from corrosion potential, make the anode polarization electric potential scanning with certain speed, after sweeping to passivation potential 400mV, make to be scanned up to corrosion potential in the other direction with same sweep speed, thereby measure activation electric current I a and reactivation electric current I r, wherein, anode polarization electric potential scanning speed is 0.5～5mv/s, preferred 1.66mv/s; Maximum anode current when activation electric current I a is forward scan, maximum anode current when reactivation electric current I r is reverse scan;
5) Susceptibility To Intergranular Corrosion is judged: judge the sample Susceptibility To Intergranular Corrosion with ratio R a=Ir/Ia * 100%.
Above-mentioned two phase stainless steel Susceptibility To Intergranular Corrosion dicyclo galvanochemistry potentiokinetic reactivation evaluation assessment the 4th) in the step DL-EPR test, at first be from corrosion potential, make the anode polarization electric potential scanning with certain speed, after sweeping to passivation potential 400mV, have automatically and make to be scanned up to corrosion potential in the other direction with same sweep speed, in the forward scan process, a maximum anode current can occur namely is activation electric current I a, in the reverse scan process, a maximum anode current also can occur namely is reactivation electric current I r, be designed into the concrete experimental implementation from this inventive method, activation electric current I a does not overlap with reactivation electric current I r, thereby has effectively guaranteed the reliability of the inventive method, stability and high sensitivity.
Dicyclo galvanochemistry potentiokinetic reactivation evaluation assessment of the present invention is used for estimating 2205 two phase stainless steel Susceptibility To Intergranular Corrosions.
The definition of one term
Dicyclo galvanochemistry reactivation (DL-EPR): be a kind of electrochemical test method of quantitative fast detecting stainless steel sensitization, can be used for the Susceptibility To Intergranular Corrosion of industry spot experimental material.Its principle is to utilize the content of the bulk alloy element in stainless passivation-reactivation characteristic and the passivating film and relevant these characteristics of characteristic of film, studies stainless sensitization behavior.Under the passive state, the state of passivating film depends on the content of Cr in the solid solution, Mo to a great extent.Therefore, apply volta potential in the particular medium, can form the intact passivating film at stainless steel surfaces.Yet the stainless steel of sensitization state can not form complete passivating film because of the poor chromium in subregion (Cr).So the volta potential flyback is to being again stainless steel surfaces when activation, the passivating film defective locations is optimum solvation, and characterizing out is that the measuring current of electro-chemical test increases.So, just, can quantitatively detect stainless sensitization.Usually, in the past DL-EPR test system is mainly at single austenitic stainless steel.Yet two phase stainless steel has austenite+ferrite two-phase, and the test system that needs exploitation to make new advances comprises and estimates medium, evaluation procedure, location parameter etc.
Sensitization: be to instigate one or more materials (as adding sensitizer or changing processing technology etc.) under certain external influence, the process that the reaction sensitivity increases.Stay for some time or Slow cooling 450～800 ℃ of temperature ranges such as stainless steel, thereby cause crystal boundary to be separated out with Cr
23C
6It is the process of the carbonide of main chromium.Sensitization makes the chromium content of crystal boundary near zone, and corrosion stability descends, and the susceptibility that intercrystalline corrosion in use occurs increases.
Two standard two phase stainless steels are separated out σ and are observed mutually
Test is 10mm * 10mm * 3mm with the standard 2205 two phase stainless steel specimen sizes of abundant solid solution attitude, principal ingredient such as table 1.For obtaining the precipitated phase of different content, 800 ℃ of lower high-purity N
2Sensitization 5min is carried out in protection, 4h, and 11h processes.Under 800 ℃, the content of σ phase is high more a lot of than the content of other secondary phase, and therefore the stainless Susceptibility To Intergranular Corrosion of research under this temperature is mainly considered the impact of σ phase, and other factor can be ignored.
Table 1. standard 2205 two phase stainless steel sample part composition (units: wt.%)
| C | Mn | P | Si | S | Cr | Ni | N | Mo |
| 0.03 | 1.5 | 0.25 | 0.5 | 0.28 | 22 | 5.5 | 0.18 | 3.2 |
Such as Fig. 1, do not only have two-phase in the tissue of sensitization processing Fig. 1 (a) and 800 ℃ of sensitization processing 5min Fig. 1 (b), ferrite (black) and austenite (white), and precipitated phase has appearred among sensitization 4h Fig. 1 (c) and 11h Fig. 1 (d), the brightest position is the σ phase among the figure, and it is evident that from figure σ is distributed in the ferrite mutually, voxel volume can decompose after this had also proved the sensitization processing, can find out also that in addition the content of σ phase can increase along with the increase of sensitization time.
Determining of three technological parameters
1, sweep speed determines
Solution temperature T=25 ℃, solution medium is 2Mol/L H
2SO
4+ 1Mol/L HCl, sweep speed is respectively 0.5mV/s, 1.66mV/s, 2.5mV/s, 5mV/s tests.The result shows, sweep speed is very large for the impact of the stainless reactivation rate Ra that processes through sensitization.Ra between the too fast different precipitated phase content of electric potential scanning distinguishes not obvious; And sweep speed is lower, and Ra more can show differentiation, sees Table 2.This explanation sweep speed is lower, and the DL-EPR measuring accuracy is better.It is longer that but the lower test of speed expends time in, therefore preferred 1.66mV/s electric potential scanning speed.
2, estimate choosing of solution temperature
Be 2Mol/L H at solution medium
2SO
4+ 1Mol/L HCl, sweep speed is under the condition of 1.66mV/s, adopt respectively 20 ℃, 25 ℃, 30 ℃, 40 ℃ four solution temperatures that sample is estimated, the result shows the more high Susceptibility To Intergranular Corrosion of more easily distinguishing two phase stainless steel of system temperature, sees Table 2.Same for preferred 30 ℃ of the consideration of measuring accuracy and test condition operability is estimated.
3, the selection of HCL concentration
Solution temperature T=30 ℃, sweep speed is 1.66mV/s, H
2SO
4Concentration be fixed as 2Mol/L, the concentration of HCl is when 0.1Mol/L, 0.5Mol/L, 2Mol/L, the otherness of Susceptibility To Intergranular Corrosion criterion Ra value is not obvious, the results are shown in Table 2, so the solution that adopts is 2Mol/L H
2SO
4+ 1Mol/L HCl.
4, the impact of specimen surface roughness
Sample surfaces is adopted 4 kinds of processing, and liquid honing is polished to 1.5 μ m to 180#, 1000#, 1500#.Acquired results shows that specimen surface roughness is little on the impact of Ra value, sees Table 2, and this shows that the EPR test is less demanding to the surface treatment of sample.Wherein, aforesaid " 180#, 1000#, 1500# " refers to the sand paper model, the art generally represents the roughness of sample with the sand paper model, that is to say the sand papering two phase stainless steel specimen surface of using respectively 180#, 1000#, 1500#, with this specimen surface polishing, make the roughness of this two phase stainless steel specimen surface consistent with the roughness of described sand paper.The present embodiment preferably uses 1500# sand paper with the specimen surface sanding and polishing.
The constituency Specific Principles of the various Testing factors of table 2 is seen following Susceptibility To Intergranular Corrosion criterion Ra mark sheet
Annotate: the explanation of the Ra property distinguished:--, very poor;-, poor; +, good; ++, fine
Therefore the solution medium that adopts DL-EPR to estimate 2205 two phase stainless steel Susceptibility To Intergranular Corrosion recommend adoptions is 2M H
2SO
4+ 1M HCl, sweep speed is 1.66mV/s, solution temperature is 30 ℃.
For the DL-EPR test system that designs at single austenitic stainless steel, the main medium that this system adopts was the dilute acid soln that contains thiocyanate ion in the past.Because this test system is not that to set up dicyclo galvanochemistry potentiokinetic reactivation evaluation assessment be theory, therefore the method need not relate to passivation potential and corrosion potential technical barrier, if when testing the corrosion susceptibility of two phase stainless steel with existing DL-EPR test system, the potential diagram of passivation potential and corrosion potential is two level and smooth rectilinears that overlap fully, also just can't test the corrosion susceptibility of two phase stainless steel.And the inventive method is the characteristic that has according to two phase stainless steel, selects sulfuric acid (H
2SO
4) and the mixed solution of hydrochloric acid (HCl) as estimating solution, again with the standard three-electrode system, be that auxiliary platinized platinum helps electrode, saturated calomel reference electrode, the sample working electrode inserts by art methods and estimates in the solution, can solve passivation potential and corrosion potential technical barrier, can be according to the concrete various kinds of two phase stainless steel, passivation potential and corrosion potential are well separated, judge that effectively and accurately the two phase stainless steel intercrystalline corrosion is strong and weak thereby reach.
The passivation potential of above-mentioned 400mV is stainless essential attribute, and this passivation potential numerical value all remains unchanged when making the anode polarization electric potential scanning and do to be scanned up to corrosion potential in the other direction.
Above-mentioned judgement two phase stainless steel intercrystalline corrosion power is to judge according to Ra=Ir/Ia * 100%, and when the numerical value of reactivation rate Ra was higher, Susceptibility To Intergranular Corrosion was also just stronger.When Ra＜0.5%, Susceptibility To Intergranular Corrosion is very little, can ignore, shown in Fig. 2 (a) among the embodiment 3; 0.5%≤Ra＜5%, two phase stainless steel is the intercrystalline corrosion tendency slightly, shown in Fig. 2 (b) among the embodiment 4; 5%≤Ra, the Susceptibility To Intergranular Corrosion of two phase stainless steel is large, shown in Fig. 2 (c) among the embodiment 5.
2205 two phase stainless steels after adopting two phase stainless steel Susceptibility To Intergranular Corrosion dicyclo galvanochemistry potentiokinetic reactivation evaluation assessment to sensitization carry out the Susceptibility To Intergranular Corrosion evaluation, comprise that step is:
1) sample pretreatment: two phase stainless steel sample to be measured is polished to 180# step by step through sand paper first, then through mechanical buffing to 1.5 μ m and oil removal treatment;
2) preparation of electrochemical evaluation solution: prepare at ambient temperature sulfuric acid solution and hydrochloric acid solution, this sulfuric acid solution concentration is 1mol/L, and concentration of hydrochloric acid solution is 0.1mol/L;
3) foundation of electrochemical evaluation system: in step 2) set up the standard three-electrode system that is consisted of by auxiliary electrode, contrast electrode, working electrode in the evaluation solution of preparation, wherein, auxiliary electrode is platinized platinum, contrast electrode is saturated calomel electrode, working electrode is sample, and the temperature of estimating solution is 20 ℃;
4) DL-EPR test: control electric potential scanning with electrochemical workstation, from corrosion potential, make the anode polarization electric potential scanning with certain speed, after sweeping to passivation potential 400mV, make to be scanned up to corrosion potential in the other direction with same sweep speed, thereby measure activation electric current I a and reactivation electric current I r, wherein, anode polarization electric potential scanning speed is 0.5mv/s;
5) Susceptibility To Intergranular Corrosion is judged: judge the sample Susceptibility To Intergranular Corrosion with ratio R a=Ir/Ia * 100%.
Embodiment 2
2205 two phase stainless steels after adopting two phase stainless steel Susceptibility To Intergranular Corrosion dicyclo galvanochemistry potentiokinetic reactivation evaluation assessment to sensitization carry out the Susceptibility To Intergranular Corrosion evaluation, comprise that step is:
1) sample pretreatment: two phase stainless steel sample to be measured is polished to 1500# step by step through sand paper first, then through mechanical buffing to 3 μ m and oil removal treatment;
2) preparation of electrochemical evaluation solution: prepare at ambient temperature sulfuric acid solution and hydrochloric acid solution, this sulfuric acid solution concentration is 3mol/L, and concentration of hydrochloric acid solution is 2mol/L;
3) foundation of electrochemical evaluation system: in step 2) set up the standard three-electrode system that is consisted of by auxiliary electrode, contrast electrode, working electrode in the evaluation solution of preparation, wherein, auxiliary electrode is platinized platinum, contrast electrode is saturated calomel electrode, working electrode is sample, and the temperature of estimating solution is 40 ℃;
4) DL-EPR test: control electric potential scanning with electrochemical workstation, from corrosion potential, make the anode polarization electric potential scanning with certain speed, after sweeping to passivation potential 400mV, make to be scanned up to corrosion potential in the other direction with same sweep speed, thereby measure activation electric current I a and reactivation electric current I r, wherein, anode polarization electric potential scanning speed is 5mv/s;
5) Susceptibility To Intergranular Corrosion is judged: judge the sample Susceptibility To Intergranular Corrosion with ratio R a=Ir/Ia * 100%.
Embodiment 3
Adopt two phase stainless steel Susceptibility To Intergranular Corrosion dicyclo galvanochemistry potentiokinetic reactivation evaluation assessment to carrying out the Susceptibility To Intergranular Corrosion evaluation without 2205 two phase stainless steels after the sensitization, comprise that step is:
1) sample pretreatment: two phase stainless steel sample to be measured is polished to 1500# step by step through sand paper first, then through mechanical buffing to 2 μ m and oil removal treatment;
2) preparation of electrochemical evaluation solution: prepare at ambient temperature sulfuric acid solution and hydrochloric acid solution, sulfuric acid solution concentration is 2mol/L, and concentration of hydrochloric acid solution is 1mol/L;
3) foundation of electrochemical evaluation system: in step 2) set up the standard three-electrode system that is consisted of by auxiliary electrode, contrast electrode, working electrode in the evaluation solution of preparation, wherein, auxiliary electrode is platinized platinum, contrast electrode is saturated calomel electrode, working electrode is sample, and the temperature of estimating solution is 30 ℃;
4) DL-EPR test: control electric potential scanning with electrochemical workstation, from corrosion potential, make the anode polarization electric potential scanning with certain speed, after sweeping to passivation potential 400mV, make to be scanned up to corrosion potential in the other direction with same sweep speed, thereby measure activation electric current I a and reactivation electric current I r, wherein, anode polarization electric potential scanning speed is 1.66mv/s;
5) Susceptibility To Intergranular Corrosion is judged: judge the sample Susceptibility To Intergranular Corrosion with ratio R a=Ir/Ia * 100%.
Carry out DL-EPR test, the curve that its result obtains such as Fig. 2 (a) without 2205 two phase stainless steel materials of sensitization.Survey Ir very little, so the Susceptibility To Intergranular Corrosion factor R a=Ir/Ia of material * 100 are very little, this characterizes a little less than the Susceptibility To Intergranular Corrosion of this material.Fig. 3 (a) is the surface topography after testing.
Embodiment 4
2205 two phase stainless steels after adopting two phase stainless steel Susceptibility To Intergranular Corrosion dicyclo galvanochemistry potentiokinetic reactivation evaluation assessment to slight sensitization carry out the Susceptibility To Intergranular Corrosion evaluation, comprise that step is:
1) sample pretreatment: two phase stainless steel sample to be measured is polished to 1500# step by step through sand paper first, then through mechanical buffing to 1 μ m and oil removal treatment;
2) preparation of electrochemical evaluation solution: prepare at ambient temperature sulfuric acid solution and hydrochloric acid solution, sulfuric acid solution concentration is 2mol/L, and concentration of hydrochloric acid solution is 1mol/L;
3) foundation of electrochemical evaluation system: in step 2) set up the standard three-electrode system that is consisted of by auxiliary electrode, contrast electrode, working electrode in the evaluation solution of preparation, wherein, auxiliary electrode is platinized platinum, contrast electrode is saturated calomel electrode, working electrode is sample, and the temperature of estimating solution is 30 ℃;
4) DL-EPR test: control electric potential scanning with electrochemical workstation, from corrosion potential, make the anode polarization electric potential scanning with certain speed, after sweeping to passivation potential 400mV, make to be scanned up to corrosion potential in the other direction with same sweep speed, thereby measure activation electric current I a and reactivation electric current I r, wherein, anode polarization electric potential scanning speed is 1.66mv/s;
5) Susceptibility To Intergranular Corrosion is judged: judge the sample Susceptibility To Intergranular Corrosion with ratio R a=Ir/Ia * 100%.
2205 two phase stainless steel materials of slight sensitization are carried out DL-EPR test, the curve that its result obtains such as Fig. 2 (b).Survey Ir less, so the Susceptibility To Intergranular Corrosion factor R a=Ir/Ia of material * 100 are less, calculate to be about 1.84%.This characterizes this material Susceptibility To Intergranular Corrosion slightly.Fig. 3 (b) is the surface topography after testing.
Embodiment 5
2205 two phase stainless steels after adopting two phase stainless steel Susceptibility To Intergranular Corrosion dicyclo galvanochemistry potentiokinetic reactivation evaluation assessment to serious sensitization carry out the Susceptibility To Intergranular Corrosion evaluation, comprise that step is:
1) sample pretreatment: two phase stainless steel sample to be measured is polished to 1500# step by step through sand paper first, then through mechanical buffing to 1.5 μ m and oil removal treatment;
2) preparation of electrochemical evaluation solution: prepare at ambient temperature sulfuric acid solution and hydrochloric acid solution, sulfuric acid solution concentration is 2mol/L, and concentration of hydrochloric acid solution is 1mol/L;
3) foundation of electrochemical evaluation system: in step 2) set up the standard three-electrode system that is consisted of by auxiliary electrode, contrast electrode, working electrode in the evaluation solution of preparation, wherein, auxiliary electrode is platinized platinum, contrast electrode is saturated calomel electrode, working electrode is sample, and the temperature of estimating solution is 30 ℃;
4) DL-EPR test: control electric potential scanning with electrochemical workstation, from corrosion potential, make the anode polarization electric potential scanning with certain speed, after sweeping to passivation potential 400mV, make to be scanned up to corrosion potential in the other direction with same sweep speed, thereby measure activation electric current I a and reactivation electric current I r, wherein, anode polarization electric potential scanning speed is 1.66mv/s;
5) Susceptibility To Intergranular Corrosion is judged: judge the sample Susceptibility To Intergranular Corrosion with ratio R a=Ir/Ia * 100%.
2205 two phase stainless steel materials of serious sensitization are carried out DL-EPR test, the curve that its result obtains such as Fig. 2 (c).Survey Ir very large, so the Susceptibility To Intergranular Corrosion factor R a=Ir/Ia of material * 100% is also very large, calculates to be about 21.21%.This Susceptibility To Intergranular Corrosion that characterizes this material is strong.Fig. 3 (c) and (d) for the test after surface topography.
The above only is preferred embodiment of the present invention, not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. two phase stainless steel Susceptibility To Intergranular Corrosion dicyclo galvanochemistry potentiokinetic reactivation evaluation assessment may further comprise the steps:
1) sample pretreatment: with two phase stainless steel sample polishing to be measured, then through mechanical buffing and oil removal treatment;
2) preparation of electrochemical evaluation solution: the mixed solution of preparing at ambient temperature sulfuric acid and hydrochloric acid;
3) foundation of electrochemical evaluation system: in step 2) set up the standard three-electrode system that is consisted of by auxiliary electrode, contrast electrode, working electrode in the evaluation solution of preparation;
4) DL-EPR test: control electric potential scanning with electrochemical workstation, from corrosion potential, make the anode polarization electric potential scanning with certain speed, after sweeping to passivation potential 400mV, make to be scanned up to corrosion potential in the other direction with same sweep speed, thereby measure activation electric current I a and reactivation electric current I r; Wherein, described anode polarization electric potential scanning speed is 0.5～5mv/s, and the temperature of DL-EPR test electrochemical evaluation solution is 20～40 ℃;
5) Susceptibility To Intergranular Corrosion is judged: judge the sample Susceptibility To Intergranular Corrosion with ratio R a=Ir/Ia * 100%.
2. two phase stainless steel Susceptibility To Intergranular Corrosion dicyclo galvanochemistry potentiokinetic reactivation evaluation assessment according to claim 1, it is characterized in that: sulfuric acid solution concentration is 1～3mol/L in the evaluation solution of described step (2), and concentration of hydrochloric acid solution is 0.1～2mol/L.
3. two phase stainless steel Susceptibility To Intergranular Corrosion dicyclo galvanochemistry potentiokinetic reactivation evaluation assessment according to claim 2, it is characterized in that: sulfuric acid solution concentration is 2mol/L in the evaluation solution of described step (2), concentration of hydrochloric acid solution is 1mol/L.
4. two phase stainless steel Susceptibility To Intergranular Corrosion dicyclo galvanochemistry potentiokinetic reactivation evaluation assessment according to claim 1, it is characterized in that: polishing is with 180～1500 model sand paper the two phase stainless steel specimen surface to be polished in the described step (1), makes the roughness of this two phase stainless steel specimen surface consistent with the roughness of described sand paper.
5. two phase stainless steel Susceptibility To Intergranular Corrosion dicyclo galvanochemistry potentiokinetic reactivation evaluation assessment according to claim 1, it is characterized in that: auxiliary electrode is platinized platinum in the described step (3), contrast electrode is saturated calomel electrode, and working electrode is sample.
6. two phase stainless steel Susceptibility To Intergranular Corrosion dicyclo galvanochemistry potentiokinetic reactivation evaluation assessment according to claim 1, it is characterized in that: described step (4) Anodic polarized potential sweep speed is 1.66mv/s.
7. two phase stainless steel Susceptibility To Intergranular Corrosion dicyclo galvanochemistry potentiokinetic reactivation evaluation assessment according to claim 1 is characterized in that: the temperature of DL-EPR test electrochemical evaluation solution is 30 ℃ in the described step (4).
8. the application of the arbitrary described two phase stainless steel Susceptibility To Intergranular Corrosion dicyclo galvanochemistry potentiokinetic reactivation evaluation assessment of claim 1 to 7 in estimating the two phase stainless steel Susceptibility To Intergranular Corrosion.
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| CN101975743B (en) * | 2010-11-24 | 2012-06-20 | 山东电力研究院 | Method for testing inter-grain corrosion performance of austenitic heat-resistant steel after aging at 650 DEG C |
| CN104849204B (en) * | 2015-05-29 | 2017-11-07 | 北京科技大学 | A kind of electrochemical method of test 316LN Intergranular Corrosion of Austenitic Stainless Steel |
| CN105547974A (en) * | 2015-12-18 | 2016-05-04 | 西南铝业（集团）有限责任公司 | Determination method of sensitivity grade of intergranular corrosion of 5083 alloy sheet materials |
| CN106918545B (en) * | 2015-12-28 | 2023-11-03 | 沈阳中科腐蚀控制工程技术有限公司 | Corrosion test method and device for rapidly realizing occurrence and development of stainless steel pitting corrosion |
| NO20160373A1 (en) * | 2016-03-03 | 2017-09-04 | Vetco Gray Scandinavia As | Rapid non-destructive evaluation of the degree of sensitization in stainless steels and nickel based alloys |
| CN105973970B (en) * | 2016-04-29 | 2019-05-24 | 河海大学常州校区 | A method of detection austenitic stainless steel corrosion susceptibility |
| CN106053322A (en) * | 2016-05-17 | 2016-10-26 | 上海锅炉厂有限公司 | Method for evaluating intergranular corrosion sensitivity of elbows made of austenite steel |
| 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 |
| CN112179838B (en) * | 2020-09-29 | 2023-02-07 | 复旦大学 | Method for inspecting crevice corrosion resistance of duplex stainless steel |
| CN113899682A (en) * | 2021-08-30 | 2022-01-07 | 振石集团东方特钢有限公司 | Method for detecting corrosion sensitivity of duplex stainless steel |
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