CN105973970B - A method of detection austenitic stainless steel corrosion susceptibility - Google Patents
A method of detection austenitic stainless steel corrosion susceptibility Download PDFInfo
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- CN105973970B CN105973970B CN201610283611.0A CN201610283611A CN105973970B CN 105973970 B CN105973970 B CN 105973970B CN 201610283611 A CN201610283611 A CN 201610283611A CN 105973970 B CN105973970 B CN 105973970B
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Abstract
The present invention provides a kind of method for detecting austenitic stainless steel corrosion susceptibility, this method acquires the reactivation peak current density of austenitic stainless steel using EPR method, so that it is determined that the relationship between reactivation peak current density and extent of corrosion, and then judge the extent of corrosion of austenitic stainless steel to be measured, the more accurate stabilization of testing result.
Description
Technical field
The present invention relates to a kind of methods for detecting austenitic stainless steel corrosion susceptibility, belong to electrochemical technology field.
Background technique
Through the austenitic stainless steel of solution treatment, crystal boundary understands carbide precipitate after sensitized treatment, causes crystal boundary chromium depleted existing
As the austenitic stainless steel of heavy corrosion actual use.It is caused using the equipment of austenite stainless steel making due to corrosion failure
Loss it is serious, the increasingly extensive application of stainless steel causes to study its etching problem very urgent.
EPR, i.e. electrochemistry reactivation are answered in the various methods of existing evaluation stainless steel intercrystalline corrosion sensibility
With extensive and mature method, has the characteristics that quick, lossless and quantify, be able to satisfy industry spot examination requirements.EPR Fa Changcai
Use H2SO4 + KSCN electrolyte, KSCN medium main function acts as reacting movable agent, i.e., during the reactivation of EPR method
Accelerate the dissolution of the imperfect passivating film of Cr depletion zone.
Summary of the invention
The present invention provides a kind of detection austenite stainless to solve drawbacks described above and deficiency existing in the prior art
The method of steel corrosion sensibility, this method acquire the reactivation peak current density of austenitic stainless steel by EPR method, and then sentence
Break its extent of corrosion, as a result precise and stable.
In order to solve the above technical problems, the present invention provides a kind of method for detecting austenitic stainless steel corrosion susceptibility, adopt
With electrochemistry reactivation, i.e. EPR method obtains reactivation peak current densityI r, according to reactivation peak current densityI rJudge the extent of corrosion of stainless steel, specifically includes the following steps:
Step 1 determines detection device, prepares standard sample, carries out under the conditions of different sensitizations to austenitic stainless steel quick
Change processing, obtains the different standard sample of extent of corrosion；Sensitized treatment process is, by austenitic stainless steel in 950 DEG C of heat preservation 2h
Water quenching afterwards is then placed in chamber type electric resistance furnace and is sensitized under 600 DEG C, 650 DEG C, 700 DEG C, 750 DEG C and 800 DEG C sensitizing temperatures respectively
Quickly cooling after different time obtains the different standard sample of extent of corrosion, for use；
Step 2, optimizing detection parameter, using field mouthful method optimizing detection device parameter and electrolyte parameter；
Step 3 obtains standard sample using EPR method and is re-activated peak current densityI r, and to activation peak current densityI rIt is analyzed and processed, obtains reactivation peak current densityI rRelationship between extent of corrosion；
Step 4, to austenitic stainless steel to be measured repeat step 3 the step of, obtain living again for austenitic stainless steel to be measured
Change peak current densityI o；
Step 5, by the reactivation peak current density of austenitic stainless steel to be measuredI oBring the curve graph in step 3 into,
Obtain the extent of corrosion of austenitic stainless steel to be measured.
Wherein, in the step 1, detection device is three-electrode cell PS-268A type electrochemical meter, austenite
Stainless steel is 304 stainless steels, is encapsulated after sensitized treatment through epoxy resin, working face is polished to SiC waterproof abrasive paper from No. 300 step by step
No. 2000, dehydrated alcohol oil removing is used after water cleaning, is dried up after deionized water cleaning stand-by.
In the step 2, detection device parameter is specifically, flyback current potentialE=300mV and scanning speedV=100mV·
min-1；Electrolyte needed for EPR is tested be 0.5mol/L sulfuric acid and 0.01mol/L potassium rhodanate aqueous solution or 1.0mol/L sulfuric acid and
0.5mol/L sodium-chloride water solution, test temperature are 25 ± 1 DEG C.
Working electrode is placed in electrolytic cell before starting and stands 10min by step 3, after instrument open circuit potential is stablized with
100mV·min-1Sweep speed forward direction is swept at passivation region 300mV, then with phase same rate reverse scan to take-off potential, examination
Testing data sampling period is 5s.
After EPR test, after working electrode is cleaned with deionized water, the ultrasonication 5min in dehydrated alcohol, drying
The erosion profile of austenitic stainless steel is tested using metallography microscope sem observation afterwards.
Present invention advantageous effects achieved: the present invention provides a kind of detection austenitic stainless steel corrosion susceptibility
Method, this method acquire the reactivation peak current density of austenitic stainless steel using EPR method, so that it is determined that reactivation peak value electricity
Relationship between current density and extent of corrosion, and then judge the extent of corrosion of austenitic stainless steel to be measured, testing result is more smart
Really stablize.
Detailed description of the invention
The reactivation peak of the standard sample of sensitized treatment different time when Fig. 1 sensitizing temperature of the embodiment of the present invention is 700 DEG C
It is worth the graph of relation of current density Ir and sensitization time t；
The sensitization degree DOS of the standard sample of sensitized treatment different time when Fig. 2 sensitizing temperature of the embodiment of the present invention is 700 DEG C
With the graph of relation of sensitization time t；
Fig. 3 sensitizing temperature of the embodiment of the present invention is the erosion profile figure of 650 DEG C of sensitized treatment different times；
Fig. 4 sensitizing temperature of the embodiment of the present invention is the erosion profile figure of 700 DEG C of sensitized treatment different times；
Fig. 5 sensitizing temperature of the embodiment of the present invention is the erosion profile figure of 750 DEG C of sensitized treatment different times.
Specific embodiment
The invention will be further described below in conjunction with the accompanying drawings.Following embodiment is only used for clearly illustrating the present invention
Technical solution, and not intended to limit the protection scope of the present invention.
The present invention provides a kind of method for detecting austenitic stainless steel corrosion susceptibility, using electrochemistry potentiokinetic reactivation
Method, i.e. EPR method obtain reactivation peak current densityI r, according to reactivation peak current densityI rJudge the corrosion journey of stainless steel
Degree, specifically includes the following steps:
Step 1 determines detection device, prepares standard sample, carries out under the conditions of different sensitizations to austenitic stainless steel quick
Change processing, obtains the different standard sample of extent of corrosion；Sensitized treatment process is, by austenitic stainless steel in 950 DEG C of heat preservation 2h
Water quenching afterwards is then placed in chamber type electric resistance furnace and is sensitized under 600 DEG C, 650 DEG C, 700 DEG C, 750 DEG C and 800 DEG C sensitizing temperatures respectively
Quickly cooling after different time obtains the different standard sample of extent of corrosion, then encapsulates through epoxy resin, working face SiC water sand
Paper is polished to No. 2000 from No. 300 step by step, and dehydrated alcohol oil removing is used after water cleaning, is dried up after deionized water cleaning stand-by.
Detection device uses three-electrode cell PS-268A type electrochemical meter, and austenitic stainless steel is stainless using 304
Steel.
Step 2, optimizing detection parameter, using field mouthful method optimizing detection device parameter and electrolyte parameter；
Detection device parameter is specifically, flyback current potentialE=300mV and scanning speedV=100mV·min-1；Needed for EPR test
Electrolyte is 0.5mol/L sulfuric acid and 0.01mol/L potassium rhodanate aqueous solution or 1.0mol/L sulfuric acid and 0.5mol/L sodium chloride water
Solution, test temperature are 25 ± 1 DEG C.
Step 3 obtains standard sample using EPR method and is re-activated peak current densityI r, and to activation peak current densityI rIt is analyzed and processed, obtains reactivation peak current densityI rRelationship between extent of corrosion；
Working electrode was placed in electrolytic cell before EPR on-test and stands 10min, after instrument open circuit potential stablize after with
100mV·min-1Sweep speed forward direction is swept at passivation region 300mV, then with phase same rate reverse scan to take-off potential, examination
Testing data sampling period is 5s.
Step 4, to austenitic stainless steel to be measured repeat step 3 the step of, obtain living again for austenitic stainless steel to be measured
Change peak current densityI o；
Step 5, by the reactivation peak current density of austenitic stainless steel to be measuredI oBring the curve graph in step 3 into,
Obtain the extent of corrosion of austenitic stainless steel to be measured.
After EPR test, after working electrode is cleaned with deionized water, the ultrasonication 5min in dehydrated alcohol, drying
The erosion profile of austenitic stainless steel is tested using metallography microscope sem observation afterwards.
Embodiment
In order to illustrate technical effect of the invention, now sensitizing temperature being selected to be 700 DEG C, treated in different sensitization times
One group of standard sample obtains the graph of relation of the reactivation peak current density and sensitization time of standard sample, such as Fig. 1 institute
Show, is as can be seen from Figure 1 re-activated peak current density Ir and positive correlation is presented in sensitization time, that is, when reactivation peak
When being worth current density Ir increase, Cr depletion zone corrosion is also stronger, as can be seen that austenitic stainless steel intergranular is rotten from erosion profile figure
Lose sensibility with sensitization time correlation, as shown in Figure 3-Figure 5, wherein 3- (a), 3- (b), 3- (c) in Fig. 3
, to respectively indicate sensitization time be 5min, 10min, 1h, 10h to 3- (d), 4- (a), 4- (b), 4- (c) are respectively indicated quick in Fig. 4
Changing the time is 1min, 10min, 3h, in Fig. 5 5- (a), 5- (b), 5- (c), 5- (d) respectively indicate sensitization time be 1min,
5min, 30min, 3h, thus it is more smart to evaluate Intergranular Corrosion of Austenitic Stainless Steel sensibility with reactivation peak current density Ir
Really stablize.
In the prior art, generally using judge index of the sensitization degree DOS as Intergranular Corrosion of Austenitic Stainless Steel, but from quick
From the point of view of change degree DOS and the relation curve of sensitization time, as shown in Fig. 2, sensitization degree DOS is relatively quick with the increase of sensitization time
The slope for changing the time reduces instead, this illustrates that sensitization degree DOS evaluation Intergranular Corrosion of Austenitic Stainless Steel sensibility exists centainly
Limitation.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, several improvement and deformations can also be made, these improvement and deformations
Also it should be regarded as protection scope of the present invention.
Claims (4)
1. a kind of method for detecting austenitic stainless steel corrosion susceptibility, it is characterised in that: use electrochemistry potentiokinetic reactivation
Method, i.e. EPR method obtain reactivation peak current density Ir, according to reactivation peak current density IrJudge the corrosion journey of stainless steel
Degree, specifically includes the following steps:
Step 1 determines detection device, prepares standard sample, carries out at sensitization under the conditions of different sensitizations to austenitic stainless steel
Reason, obtains the different standard sample of extent of corrosion；Sensitized treatment process is, by austenitic stainless steel after 950 DEG C of heat preservation 2h water
It quenches, is then placed in chamber type electric resistance furnace and is sensitized difference under 600 DEG C, 650 DEG C, 700 DEG C, 750 DEG C and 800 DEG C sensitizing temperatures respectively
Quickly cooling after time obtains the different standard sample of extent of corrosion, for use；
Step 2, optimizing detection parameter, using field mouthful method optimizing detection device parameter and electrolyte parameter；
Detection device parameter is specifically, flyback current potential E=300mV and scan velocity V=100mVmin-1；Electricity needed for EPR test
Solving liquid is 0.5mol/L sulfuric acid and 0.01mol/L potassium rhodanate aqueous solution or 1.0mol/L sulfuric acid and 0.5mol/L aqueous sodium chloride
Liquid, test temperature are 25 ± 1 DEG C；
Step 3 obtains standard sample using EPR method and is re-activated peak current density Ir, and to activation peak current density IrInto
Row analysis processing obtains reactivation peak current density IrRelationship between extent of corrosion；
Step 4, to austenitic stainless steel to be measured repeat step 3 the step of, obtain the reactivation peak of austenitic stainless steel to be measured
It is worth current density Io；
Step 5, by the reactivation peak current density I of austenitic stainless steel to be measuredoBring the curve graph in step 3 into, obtain to
Survey the extent of corrosion of austenitic stainless steel.
2. the method for detection austenitic stainless steel corrosion susceptibility according to claim 1, it is characterised in that: the step
In one, detection device is three-electrode cell PS-268A type electrochemical meter, and austenitic stainless steel is 304 stainless steels, sensitization
It is encapsulated after processing through epoxy resin, working face is polished to No. 2000 from No. 300 with SiC waterproof abrasive paper step by step, with anhydrous after water cleaning
Ethyl alcohol oil removing dries up stand-by after deionized water cleaning.
3. the method for detection austenitic stainless steel corrosion susceptibility according to claim 1, it is characterised in that: step 3 is opened
Working electrode is placed in electrolytic cell before beginning and stands 10min, with 100mVmin after instrument open circuit potential is stablized-1Sweep speed
Forward direction is swept at passivation region 300mV, and then with phase same rate reverse scan to take-off potential, the test data sampling period is 5s.
4. the method for detection austenitic stainless steel corrosion susceptibility according to claim 1, it is characterised in that: EPR test
Afterwards, after working electrode being cleaned with deionized water, the ultrasonication 5min in dehydrated alcohol uses metallographic microscope after drying
Observe the erosion profile of tested austenitic stainless steel.
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| CN105929011B (en) * | 2016-04-29 | 2018-10-26 | 河海大学常州校区 | A kind of spot corrosion detection method of stainless steel intercrystalline corrosion |
| RU2702796C1 (en) * | 2019-01-22 | 2019-10-11 | Российская Федерация, от имени которой выступает Государственная корпорация по атомной энергии "Росатом" | Electrochemical cell for determination of steels resistance against intergranular corrosion |
| CN112683766A (en) * | 2020-12-22 | 2021-04-20 | 重庆市食品药品检验检测研究院 | Method for detecting fluorine resistance of tantalum and titanium materials |
| 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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| JPH1026598A (en) * | 1996-07-10 | 1998-01-27 | Hitachi Ltd | Method and apparatus for evaluating sensitization of cr-containing austenite alloy |
| CN1438478A (en) * | 2003-03-20 | 2003-08-27 | 上海交通大学 | Method for detecting corrosion of concrete bar in reinforced concrete |
| CN101762454A (en) * | 2010-02-03 | 2010-06-30 | 海洋王照明科技股份有限公司 | Dual-ring electrochemical dynamic potential reactivating evaluating method for diphase stainless steel intercrystalline corrosion sensitivity |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1026598A (en) * | 1996-07-10 | 1998-01-27 | Hitachi Ltd | Method and apparatus for evaluating sensitization of cr-containing austenite alloy |
| CN1438478A (en) * | 2003-03-20 | 2003-08-27 | 上海交通大学 | Method for detecting corrosion of concrete bar in reinforced concrete |
| CN101762454A (en) * | 2010-02-03 | 2010-06-30 | 海洋王照明科技股份有限公司 | Dual-ring electrochemical dynamic potential reactivating evaluating method for diphase stainless steel intercrystalline corrosion sensitivity |
Non-Patent Citations (2)
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| EPR法评价晶间腐蚀敏感性的各种判据的比较;高中平等;《中国腐蚀与防护学报》;20000831;第20卷(第4期);第2、3节及表1 |
| 在Ｈ2ＳＯ4＋ＮaＣl电解液中采用ＥＰＲ法评价304不锈钢晶间腐蚀敏化度的变化;熊佳龙等;《腐蚀与防护》;20150131;第36卷(第1期);全文 |
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