CN100374845C - Method for evaluating pitting resistance performance of material - Google Patents
Method for evaluating pitting resistance performance of material Download PDFInfo
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- CN100374845C CN100374845C CNB2005100293323A CN200510029332A CN100374845C CN 100374845 C CN100374845 C CN 100374845C CN B2005100293323 A CNB2005100293323 A CN B2005100293323A CN 200510029332 A CN200510029332 A CN 200510029332A CN 100374845 C CN100374845 C CN 100374845C
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Abstract
The present invention belongs to the technical field of the evaluation of metallic corrosion, particularly to an evaluation method for the pitting corrosion resistant performance of materials. A parameter-re-passivation temperature for evaluating the pitting corrosion resistant performance of the materials is introduced into the present invention, a standard three-electrode system is used in terms of electrochemistry, and the re-passivation temperature and the critical pitting corrosion temperature of the materials are measured through corrosion current density under constant externally applied electric potential and the temperature in a temperature cycling scanning method. The parameter of the re-passivation temperature can actually and objectively reflect the pitting corrosion resistant performance and the pitting corrosion re-passivation performance of the materials and has important study value, and the cycling scanning method can quickly, directly and accurately measure the critical pitting corrosion temperature, the re-passivation temperature and other evaluating parameters of the materials and has important application value.
Description
Technical field
The invention belongs to metal erosion assessment technique field, be specifically related to a kind of method of evaluating pitting resistance performance of material, comprise and introduce an evaluating material parameter and a kind of new method of measuring this parameter and material critical spot corrosion temperature of inactivating performance again.
Background technology
Spot corrosion is one of modal corrosion form in easy passive metal or the alloy.This corrosion is extremely strong because of disguise, greatly destructive, and is extensively paid attention to and further investigate.One of research emphasis is exactly the sign of material spot corrosion behavior and the evaluation of pitting resistance performance of material.
The evaluating of pitting resistance performance of material mainly contains pit number, material weightlessness, pit size and the degree of depth, critical pitting temperature ([1] Brigham R J, Tozer E W, Corrosion-NACE, 1973,29 on the material unit area; 33), spot corrosion feature current potential etc.Wherein critical pitting temperature and spot corrosion feature current potential be because be easy to quantitative measurment, and pitting resistance that can objective direct reaction material and be widely used in scientific research and industrial application.
Pitting potential is one of the important parameter of the spot corrosion susceptibility of characterizing metal and alloy, and measuring method has a lot, can be divided into potential control and electric current control method, and wherein using is at most electrokinetic potential polarization curve scan method in the potential control the most widely.This method places chemical mediator with material, and anode potential reaches a certain current potential of passivation region ([2] Wei Baoming, Hao Ling towards positive dirction scanning, China's corrosion and protection journal, 1988, in the time of 8:87) because spot corrosion takes place, current density increases rapidly suddenly, and this current potential is called the spot corrosion disruptive potential.After spot corrosion takes place, again with the current potential reverse scanning, if record another feature current potential that electric current is descended owing to pit passivation again at passivation region, then be called again passivation potential ([3] Szklarska-SmialowskaZ.Pitting Corrosion of Metals.NACE, 1986).
Critical pitting temperature is that the material passivating film begins to break, and the minimum temperature of correspondence can be relative critical pitting temperature when spot corrosion took place, and also can be absolute critical pitting temperature.Critical pitting temperature is meant the critical pitting temperature when the material externally-applied potential is lower than a certain value relatively, and this temperature reduces along with the increase of externally-applied potential, shows the certain dependence to the material externally-applied potential.Absolute critical pitting temperature ([4] Arnvig P E, Bisgard A D, COORROSION/96-NACEPublication, Denver, 1996,437) be meant when the material externally-applied potential and surpass a certain particular value measured critical pitting temperature before reaching material transpassivation current potential the time that this parameter is a steady state value, the variation with externally-applied potential does not change.The American National Standard regulation, when constant potential was 700mV, the critical pitting temperature that records was absolute critical pitting temperature.The critical pitting temperature measuring method mainly contains corrosion electric current density under chemical immersion method and the constant externally-applied potential-temperature scanning method ([5] Qvarfort R, Corrosion Science, 1989,29; 987).
Yet the improvement that is similar to the cyclic polarization curve method does not but occur in stainless steel spot corrosion temperature survey field, and material this notion of passivation temperature does not again see that the someone proposes yet, and becomes a blank in metal erosion assessment technique field.
Summary of the invention
The objective of the invention is to propose a kind of can be comprehensively, the method for evaluating pitting resistance performance of material exactly.
The method of the evaluating pitting resistance performance of material that the present invention proposes, comprise the parameter of introducing an evaluating pitting resistance performance of material---passivation temperature again, galvanochemistry adopts the three-electrode system of standard, and utilize corrosion current under the constant externally-applied potential-temperature cycles scan method to measure the passivation temperature again and the critical pitting temperature of material, thereby the pitting resistance of material is made an appraisal; Concrete steps are as follows:
1. the pre-passivation of sample
Adopt dense HNO
3Solution carries out pre-passivation to avoid the interference of crevice corrosion to sample surfaces, and treatment temperature is 50-60 ℃, time 80-100 minute.
2. corrosion electric current density-temperature scanning
At first feed high pure nitrogen (more than 99.99%) 25-40 minute with deoxygenation, continue logical nitrogen deoxygenation in the test process to medium solution; Galvanochemistry adopts the three-electrode system of standard: auxiliary electrode is the metal platinum electrode, and contrast electrode is a saturated calomel electrode, and sample is a working electrode; Constant externally-applied potential, elevated temperature scans the material corrosion electric current with the variation of temperature curve gradually, and the control rate of heat addition is 1 ± 0.3 ℃/min, and until the critical pitting temperature that scans material, promptly the material corrosion current density increases to 1 * 10
-4A/cm
2Corresponding temperature writes down this temperature;
3. corrosion electric current density-temperature flyback
The corrosion electric current density of material arrives 5 * 10
-3A/cm
2After, stop heating, cooling gradually, the trip temperature reverse scanning of going forward side by side, the control rate of temperature fall is 1 ± 0.3 ℃/min, until the passivation temperature again that scans material, promptly the material corrosion current density reaches 1 * 10 once more
-4A/cm
2The time correspondence temperature, write down this temperature.
In the said method, constant externally-applied potential value is decided according to material concrete environment of living in and research needs, but is no more than 1V.
In the said method, the temperature that described passivation temperature again can objective effectively evaluating material is inactivating performance again, and important academic using value is arranged.Its meaning is the material pit pairing maximum temperature of passivation again.This parameter is also relevant with the pairing corrosion electric current density of beginning reverse scanning, reverse scanning speed etc. itself influencing except being subjected to material and media environment.Therefore, for ease of accurate objective evaluation material temperature inactivating performance again, adopted following standard: reach 5 * 10 in the material corrosion current density
-3A/cm
2After begin the temperature reverse scanning, control cooling velocity 1 ± 0.3 ℃/min in the scanning process.Final prescribed material corrosion electric current density reaches 1 * 10 once more
-4A/cm
2Corresponding temperature is the passivation temperature again of material.
Description of drawings
Fig. 1 is an Experimental equipment.
Fig. 2 is corrosion current under the constant externally-applied potential of OCr25Ni7Mo4 stainless steel-temperature cycles scanning curve.
Fig. 3 is the surface topography photo of sample under 100 times of metaloscopes, and wherein Fig. 3 (a) is for spot corrosion material surface pattern in the past takes place, and Fig. 3 (b) is the spot corrosion pattern.
Fig. 4 is the polarization curve of sample under different temperatures.Wherein curve a is the following polarization curve of material critical spot corrosion temperature, and curve b is the above polarization curve of material critical spot corrosion temperature, and curve c is for the spot corrosion sample taking place at the following polarization curve of passivation temperature again.
Symbol among the figure: A is a water inlet, and B is a thermofin, and C is a heating jacket, and D is a water delivering orifice, and E is a water, F is a medium solution, and G is a temperature controller, and H is saturated KCl solution, and I is a contrast electrode, and J is a salt bridge, K is the gas outlet, and L is a working electrode, and M is an auxiliary electrode, and N is a thermometer, and O is an air intake
Embodiment
Step 1: the square coupons of 20mm * 20mm * 3mm at first is processed into sample in the preparation of sample.After clean surface was removed greasy dirt, sample was placed in 55 ℃ dense HNO
3Pre-passivation 90min is to avoid the interference of crevice corrosion in the solution.Use the epoxy encapsulation non-working surface behind the welding lead of the passivation sample back side, only reserve the surface of about 15mm * 15mm passivation, and progressively carefully be polished to sand paper No. 1000, only expose the workplace of 10mm * 10mm.
Step 2: the packaged sample drying at room temperature of corrosion current-temperature scanning was placed 1 hour, treated that current potential begins scan test after stable.Before the experiment, at first in medium solution, feed high pure nitrogen (more than 99.99%) 30 minutes, continue the ventilation deoxygenation in the test process with deoxygenation.Galvanochemistry adopts the three-electrode system of standard: auxiliary electrode adopts the metal platinum electrode; The contrast electrode system is a saturated calomel electrode; Packaged sample is a working electrode.The experiment concrete grammar is: constant externally-applied potential, scanning material corrosion current density is with the variation of temperature curve.For preventing the accuracy of material intensification lagging influence experimental result, thermometer mercury bubble present position should be the temperature field symmetry with sample, and the strict simultaneously control rate of heat addition is at 1 ± 0.3 ℃/min.Note current density and reach 1 * 10 first
-4A/cm
2Temperature, i.e. the absolute critical pitting temperature of material.
Step 3: corrosion current-temperature flyback reaches 5 * 10 in the material corrosion current density
-3A/cm
2After begin the temperature reverse scanning, in the scanning process control cooling velocity at 1 ± 0.3 ℃/min.And note the material corrosion current density and reach 1 * 10 once more
-4A/cm
2Corresponding temperature, the i.e. passivation temperature again of material.
For a concrete example of measuring the present invention is further described below.
Measure absolute critical pitting temperature and the again passivation temperature of OCr25Ni7Mo4 stainless steel material in the NaCl of 1mol/l solution
OCr25Ni7Mo4 stainless steel sample after encapsulation, the Passivation Treatment is put into device as shown in Figure 1, and test medium is the NaCl standard solution of 1mol/l.Constant externally-applied potential 700mV/SCE, 0 ℃ increases temperature gradually, and forward scan material corrosion electric current is with the variation of temperature curve, and the control rate of heat addition is 1 ± 0.3 ℃/min; Note current density and reach 1 * 10 first
-4A/cm
2Temperature, i.e. the absolute critical pitting temperature (CPT) of material; To corrosion electric current density to 5 * 10
-3A/cm
2Promptly begin the temperature reverse scanning, 1 ± 0.3 ℃/min of reverse scanning rate of temperature fall reaches 1 * 10 once more until the material corrosion current density
-4A/cm
2In time, finish, and obtains curve as shown in Figure 2, notes this temperature, is the passivation temperature again (Tp) of this material.Fig. 3 is a sample surfaces pattern photo, and as seen spot corrosion has taken place material behind overtesting, and the spot corrosion situation that this evaluation method can the objective evaluation material is described.For the further validity of this method of checking, successively measured the polarization curve of material, as shown in Figure 4 at T=75 ℃, 85 ℃ and 50 ℃ (respectively before the corresponding critical pitting temperature, behind the critical pitting temperature and again three states behind the passivation temperature).Spot corrosion sample (75 ℃) below critical pitting temperature does not take place to be reached sudden change that electric current do not appear in 800mV/SCE yet at externally-applied potential and spot corrosion not to take place (curve a); More than temperature is increased to critical pitting temperature when (85 ℃), externally-applied potential reaches the sudden change that electric current has taken place the 700mV/SCE material spot corrosion (curve b) has taken place; Again when (50 ℃) below the passivation temperature, do not observe the sudden change of electric current to material when externally-applied potential reaches 800mV/SCE again when temperature decline flyback, new spot corrosion (curve c) does not take place in material.What above result and Fig. 2 were dry straight has coincide, and the validity of corrosion current-temperature cycles scan method research material pitting resistance has been described.
Claims (1)
1. the method for an evaluating pitting resistance performance of material, it is characterized in that comprising the parameter of introducing an evaluating pitting resistance performance of material---passivation temperature again, galvanochemistry adopts the three-electrode system of standard, and utilize corrosion current under the constant externally-applied potential-temperature cycles scan method to measure the passivation temperature again and the critical pitting temperature of material, thereby the pitting resistance of material is made an appraisal; Concrete steps are as follows:
(1) the pre-passivation of sample
Adopt dense HNO
3Solution carries out pre-passivation to avoid the interference of crevice corrosion to sample surfaces, and treatment temperature is 50-60 ℃, time 80-100 minute;
(2) corrosion electric current density-temperature scanning
At first feed high pure nitrogen 25-40 minute with deoxygenation, continue logical nitrogen deoxygenation in the test process to the NaCl of 1mol/l solution; Galvanochemistry adopts the three-electrode system of standard: auxiliary electrode is the metal platinum electrode, and contrast electrode is a saturated calomel electrode, and sample is a working electrode; Constant externally-applied potential, the constant potential value is no more than 1V, and elevated temperature scans the material corrosion electric current with the variation of temperature curve gradually, the control rate of heat addition is 1 ± 0.3 ℃/min, and until the critical pitting temperature that scans material: the material corrosion current density increases to 1 * 10
-4A/cm
2Corresponding temperature writes down this temperature;
(3) corrosion electric current density-temperature flyback
The corrosion electric current density of material arrives 5 * 10
-3A/cm
2After, stop heating, cooling gradually, the trip temperature reverse scanning of going forward side by side, the control rate of temperature fall is 1 ± 0.3 ℃/min, until the passivation temperature again that scans material: the material corrosion current density reaches 1 * 10 once more
-4A/cm
2The time correspondence temperature, write down this temperature.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101655445B (en) * | 2009-09-10 | 2012-06-13 | 上海化工研究院 | Heat pump type metal corrosion test method and device |
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| CN111024604A (en) * | 2019-12-19 | 2020-04-17 | 韦正楠 | Corrosion and scaling experiment detection system and method for geothermal water heat exchange process |
| CN112285013A (en) * | 2020-09-28 | 2021-01-29 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | On-site rapid spot inspection method for coating quality of metal bipolar plate |
| CN112179838B (en) * | 2020-09-29 | 2023-02-07 | 复旦大学 | Method for inspecting crevice corrosion resistance of duplex stainless steel |
| CN114107735B (en) * | 2021-12-10 | 2022-10-28 | 西北工业大学 | Corrosion-resistant zirconium alloy and preparation method thereof |
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| CN101655445B (en) * | 2009-09-10 | 2012-06-13 | 上海化工研究院 | Heat pump type metal corrosion test method and device |
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