CN116678932A - Dynamic polarization electrochemical corrosion detection device and detection method - Google Patents
Dynamic polarization electrochemical corrosion detection device and detection method Download PDFInfo
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- CN116678932A CN116678932A CN202310742116.1A CN202310742116A CN116678932A CN 116678932 A CN116678932 A CN 116678932A CN 202310742116 A CN202310742116 A CN 202310742116A CN 116678932 A CN116678932 A CN 116678932A
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- 238000001514 detection method Methods 0.000 title claims abstract description 25
- 238000006056 electrooxidation reaction Methods 0.000 title claims abstract description 18
- 230000010287 polarization Effects 0.000 title claims abstract description 13
- 230000007797 corrosion Effects 0.000 claims abstract description 55
- 238000005260 corrosion Methods 0.000 claims abstract description 55
- 230000005284 excitation Effects 0.000 claims abstract description 43
- 238000012544 monitoring process Methods 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims description 11
- 238000005530 etching Methods 0.000 claims description 7
- 238000003487 electrochemical reaction Methods 0.000 claims description 5
- 239000003990 capacitor Substances 0.000 claims description 4
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 description 6
- 239000000523 sample Substances 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- VREFGVBLTWBCJP-UHFFFAOYSA-N alprazolam Chemical compound C12=CC(Cl)=CC=C2N2C(C)=NN=C2CN=C1C1=CC=CC=C1 VREFGVBLTWBCJP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000005283 ground state Effects 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
Abstract
The dynamic polarization electrochemical corrosion detection device and method are characterized in that a reference electrode, an auxiliary electrode and a working electrode are arranged in an electrolytic cell, the reference electrode and the working electrode are connected with a constant potential circuit module, the constant potential circuit module is connected with a voltage excitation module at the input end, the output end is connected with the reference electrode, the auxiliary electrode and the working electrode, the voltage excitation module is connected with a main controller at the input end, a data acquisition module is connected with the auxiliary electrode at the input end, the output end is connected with the main controller, and the main controller is used for controlling the voltage excitation module to generate excitation voltage which changes in a certain rule, monitoring the voltage of the reference electrode in real time and calibrating the pressure difference between the reference electrode and the working electrode, and simultaneously transmitting data input by the data acquisition module to a display module; and the display module is used for displaying the excitation voltage, the corresponding corrosion current and the time. The invention has the advantages of accurate detection, small volume and simple operation.
Description
Technical Field
The invention belongs to the technical field of electrochemistry, and particularly relates to a dynamic polarization electrochemical corrosion detection device and a detection method.
Background
With the development of automatic control technology, control and monitoring technologies have been widely developed, and the application fields thereof have been related to aspects in life. The electrochemical corrosion monitoring is widely applied in the fields of petroleum, aviation, automobiles, buildings and the like, the corrosion problem of an oil gas pipeline always has huge potential safety hazards and economic losses, the corrosion monitoring method still in use at present mainly comprises a corrosion hanging piece and a resistance probe, and the emerging technologies in recent years comprise a hydrogen probe, electrochemical noise, field fingerprint monitoring and ultrasonic thickness measuring method, the resistance probe technology published by 2021 in 6 th month 15 in a journal of material protection and the monitoring method of the corrosion hanging piece are simultaneously provided in the comparative analysis of the corrosion monitoring result of the hanging piece weightless method, the corrosion hanging piece is most widely used in the existing corrosion monitoring method, and the hanging piece which is the same as the pipeline material is required to be installed in the same corrosion environment, and the material is required to be taken out and weighed after a certain period, so that the corrosion rate is calculated. The detection method has low cost and long period, and can not realize real-time online monitoring.
The method for monitoring the resistance probe utilizes two groups of electrodes with the same materials, one electrode is placed in a corrosive medium, the other electrode is placed in a protection state, the two materials have different resistance values along with the aggravation of corrosion, and the method has larger volume and is not suitable for a long-term complex corrosion monitoring environment. The hydrogen probe technology can only be used for hydrogen evolution phenomenon in corrosion, and has poor applicability. The ultrasonic on-line monitoring technology published in the material protection journal in the year 2020 of 1 and 15 is described and tested in the application research of general light gas fields, the monitoring method can realize on-line real-time monitoring, the precision can directly meet the industrial requirements, but the phenomenon of inaccurate positioning and disorder of data can be caused for the part of a pipeline, and equipment monitoring and long-term test are required to be installed in advance.
In the existing corrosion monitoring method, the problem of long period exists in direct measurement, and the problem that online corrosion monitoring can not be realized in indirect measurement exists in large volume. Therefore, there is a need for an electrochemical test system that is compact, simple in circuitry, and low in power consumption, and that is packaged for corrosion monitoring of the pipeline. The corrosion condition of different materials in solutions with different concentrations can be detected in the laboratory at present, an electrochemical workstation is needed, and the electrochemical workstation used at present is large in size and weight and cannot realize underground corrosion on-line monitoring, so that development of a portable small-sized device with the same function as constant potential detection in the electrochemical workstation is extremely important.
Disclosure of Invention
The invention aims to overcome the defects of the existing electrochemical corrosion monitoring and provides a dynamic polarization electrochemical corrosion detection device and a detection method which have small volume and simple structure and can efficiently and accurately detect the corrosion condition of materials.
The technical scheme adopted for solving the technical problems is as follows: a dynamic polarized electrochemical corrosion detection apparatus comprising: the device comprises a main controller, a reference electrode, an auxiliary electrode, a working electrode, an electrolytic cell, a voltage excitation module, a data acquisition module, a display module and a constant potential circuit module; the electrolytic cell is internally provided with a reference electrode, an auxiliary electrode and a working electrode, wherein the working electrode is used for enabling a solution in the electrolytic cell to perform electrochemical reaction, the reference electrode is used as a reference standard of the working electrode, and the auxiliary electrode is used for transmitting corrosion current to the working electrode;
the constant potential circuit module is connected with the voltage excitation module at the input end and the reference electrode, the auxiliary electrode and the working electrode at the output end, and is used for applying excitation voltage given by the voltage excitation module between the reference electrode and the working electrode and keeping the pressure difference between the working electrode and the reference electrode constant;
the input end of the voltage excitation module is connected with the main controller and is used for generating excitation voltage;
the input end of the data acquisition module is connected with the working electrode, the output end of the data acquisition module is connected with the main controller, and the data acquisition module is used for amplifying and converting a current signal output by the working electrode into a voltage signal and then converting the voltage signal into a digital signal to be input into the main controller;
the main controller is used for controlling the voltage excitation module to generate excitation voltage which changes in a certain rule, monitoring the voltage of the reference electrode in real time, calibrating the pressure difference between the reference electrode and the working electrode, and simultaneously transmitting the data input by the data acquisition module to the display module;
the display module is used for displaying the excitation voltage, the corresponding corrosion current and the time information.
As a preferable technical scheme, the reference electrode is a saturated calomel electrode, the working electrode is cylindrical and made of a material to be measured, the auxiliary electrode is a platinum wire electrode, and the effective area of the end part is 0.5-0.7 cm 2 The effective area of the end part of the working electrode is 0.1-0.2 times of that of the end part of the auxiliary electrode, and the auxiliary electrode and the working electrode are respectively positioned at two ends of the electrolytic cell.
As a preferable technical scheme, the constant potential circuit is characterized in that the non-inverting input end of the operational amplifier U1 is connected with the voltage excitation module, the inverting input end of the operational amplifier U2 is connected with the inverting input end of the operational amplifier U2 through a resistor R1, the inverting input end of the operational amplifier U2 is connected with the inverting input end and the output end of the operational amplifier U3 through a resistor R2, the non-inverting input end of the operational amplifier U2 is grounded, the output end of the operational amplifier U2 is connected with the reference electrode, the non-inverting input end of the operational amplifier U3 is connected with the auxiliary electrode, the inverting input end of the operational amplifier U4 is connected with the working electrode and is connected with the output end through a resistor R3, the non-inverting input end is grounded, and the output end is grounded and connected with the main controller through a capacitor C1.
The invention also provides a detection method of the dynamic polarization electrochemical corrosion detection device, which comprises the following steps:
s1, adding an etching medium solution into an electrolytic cell, so that a reference electrode, an auxiliary electrode and a working electrode are completely immersed into the etching medium solution, and waiting for a period of time until the electrodes and the medium reach a stable state;
s2, starting from an initial potential, gradually increasing excitation voltage in a linear mode, and recording current response of an auxiliary electrode after the system reaches balance at each potential point;
s3, drawing a dynamic potential scanning curve by taking the potential as an abscissa and the current as an ordinate;
s4, analyzing an electrokinetic potential scanning curve, and identifying the initial potential of corrosion, namely the corrosion potential and the critical potential, namely the potential with obvious current increase. Based on the curve shape and the current value, the corrosion rate and the corrosion type were evaluated.
The beneficial effects of the invention are as follows:
the constant potential circuit can provide high-precision corrosion current measurement, and can accurately measure the corrosion current by keeping constant potential difference between the working electrode and the reference electrode, so that an accurate current value can be obtained, and the corrosion rate and the corrosion degree can be evaluated. The constant potential circuit can monitor the change of the corrosion current in real time, and can discover the development trend and abnormal condition of the corrosion problem in time, so that timely measures can be taken to prevent corrosion damage, and the service lives of equipment and structures are prolonged.
The constant potential circuit measuring method adopted by the invention is a nondestructive measuring method, and does not need to be in direct contact with an object or structure to be measured. It measures the potential difference between them by comparing the reference electrode with the working electrode without any physical change or damage to the object being measured. This allows the system under test to monitor the corrosion current during operation without interfering with the normal operation of the system.
The invention has simple structure, small volume and convenient carrying, and can be used for on-line pipeline corrosion monitoring.
Drawings
Fig. 1 is a schematic block diagram of the circuit of the present invention.
Fig. 2 is a schematic diagram of the electronics of the potentiostatic circuit module.
FIG. 3 is a plot of the Tafil corrosion rate monitored by the test system.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, but the present invention is not limited to the following embodiments.
Example 1
In fig. 1, the dynamic polarization electrochemical corrosion detection device of the embodiment comprises a main controller, a reference electrode, an auxiliary electrode, a working electrode, an electrolytic cell, a voltage excitation module, a data acquisition module, a display module and a constant potential circuit module. The electrolytic cell is internally provided with a reference electrode, an auxiliary electrode and a working electrode, the reference electrode is a saturated calomel electrode, the auxiliary electrode is a platinum wire electrode, and the effective area of the end part is 0.5-0.7 cm 2 The effective area of the end part of the embodiment is 0.59cm 2 The effective area of the end part of the working electrode is 0.15 times, 0.1 times or 0.2 times of that of the end part of the auxiliary electrode, the auxiliary electrode and the working electrode are respectively positioned at two ends of the electrolytic cell, the working electrode is made of materials to be tested, the working electrode is a cylindrical carbon steel electrode, the working electrode is used for enabling a solution in the electrolytic cell to undergo electrochemical reaction, the reference electrode is used as a reference standard of the working electrode, and the auxiliary electrode is used for transmitting corrosion current.
The constant potential circuit module has an input end connected with the voltage excitation module, an output end connected with the reference electrode, the auxiliary electrode and the working electrode, and is used for applying excitation voltage given by the voltage excitation module between the reference electrode and the working electrode and keeping the pressure difference between the working electrode and the reference electrode constant, and the auxiliary electrode is communicated with the working electrode due to electrochemical reaction of the solution in the electrolytic cell and transmits generated corrosion current to the working electrode; the input end of the voltage excitation module is connected with the main controller and is used for generating excitation voltage; the input end of the data acquisition module is connected with the working electrode, and the output end of the data acquisition module is connected with the main controller and is used for converting a current signal output by the working electrode into a voltage signal, amplifying the voltage signal and then converting the voltage signal into a digital signal to be input into the main controller; and the main controller is used for controlling the voltage excitation module to generate excitation voltage which changes in a certain rule, monitoring the voltage of the reference electrode in real time and calibrating the pressure difference between the reference electrode and the working electrode, so that the pressure difference between the reference electrode and the working electrode is kept constant, and when errors occur, the PID algorithm is adopted for adjustment and correction. Meanwhile, the main controller converts voltage data input by the data acquisition module into current data and transmits the current data to the display module; the display module is a touch screen and is used for displaying excitation voltage, corresponding corrosion current and time, and then inputting the effective area value of the end part of the working electrode to the display module, and the display module obtains the corrosion current density, namely the corrosion current in unit area according to the formula of corrosion current density = corrosion current/effective area of the end part of the working electrode.
In fig. 2, the constant potential circuit of the present embodiment is configured by connecting an operational amplifier U1 to an operational amplifier U4, a resistor R1, a resistor R2, a resistor R3, and a capacitor C1. The non-inverting input end of the operational amplifier U1 is connected with the voltage excitation module, the inverting input end is connected with the output end and is connected with the inverting input end of the operational amplifier U2 through a resistor R1, the inverting input end of the operational amplifier U2 is connected with the inverting input end and the output end of the operational amplifier U3 through a resistor R2, the non-inverting input end of the operational amplifier U2 is grounded, the output end of the operational amplifier U2 is connected with the reference electrode, the non-inverting input end of the operational amplifier U3 is connected with the auxiliary electrode, the inverting input end of the operational amplifier U4 is connected with the working electrode and is connected with the output end through a resistor R3, the non-inverting input end is grounded, and the output end is grounded and connected with the main controller through a capacitor C1.
The non-inverting input terminal of the operational amplifier U1 receives the excitation voltage, the non-inverting input terminal of the operational amplifier U4 is grounded, the working electrode (working electrode, WE) is in a virtual ground state in the state, the non-inverting terminal voltage is 0, and at the moment, that is, the working electrode is 0 to the ground potential, that is, the potential of the working electrode relative to the reference electrode is kept constant, that is, the excitation voltage is kept. As the electrochemical reaction proceeds, the polarization effects a significant effect on the potential of the working electrode, resulting in a significant shift in the potential that does not always stabilize within the range of the supplied excitation voltage. At this time, the operational amplifier U3 will present a high resistance state, and the reference electrode (reference electrode, RE) is required to not flow current according to the "virtual break" characteristic presented in the operational amplifier, so as to ensure that a closed-loop negative feedback system is formed between the reference electrode and the working electrode, thereby realizing accurate control of the electrode, and achieving the best working effect. The voltage offset phenomenon of the working electrode acts on the inverting terminal of the operational amplifier U1 along with the voltage follower, so that the polarization phenomenon in the solution is improved. The operational amplifier U2 is added in the first-stage circuit of the excitation voltage, so that the driving capability of the whole circuit is improved. The maximum bias current of the operational amplifier for detecting the current in the whole circuit reaches 100pA, and the current to be detected is in mu A level, thereby completely meeting the requirements.
The detection method of the dynamic polarization electrochemical corrosion detection device of the embodiment comprises the following steps:
s1, adding an etching medium solution into an electrolytic cell, wherein the etching medium solution in the embodiment is distilled water plus 1wt% NaCl solution, so that a reference electrode, an auxiliary electrode and a working electrode are completely immersed into the etching medium solution, and waiting for a period of time until the electrodes and the medium reach a stable state;
s2, starting from an initial potential, gradually increasing the excitation voltage in a linear mode, in the embodiment, increasing the excitation voltage by 10mV per second, and recording the current response of the auxiliary electrode after the system reaches balance at each potential point;
s3, drawing a dynamic potential scanning curve by taking the potential as an abscissa and the current as an ordinate;
s4, analyzing an electrokinetic potential scanning curve, and identifying the initial potential of corrosion, namely the corrosion potential and the critical potential, namely the potential with obvious current increase. Based on the curve shape and the current value, the corrosion rate and the corrosion type were evaluated.
The current densities corresponding to the maximum potential and the minimum potential of the dynamic polarized electrochemical corrosion detection device of the embodiment are 8.58 multiplied by 10 respectively -3 A/cm 2 (E＝1.5V)2.03×10 -3 A/cm 2 (E= -1.5V), dynamic polarization electrochemical corrosion detection device of the embodimentThe device is stable in operation in a conventional static corrosion environment, and has no obvious data offset and directivity system error. The data has less effect on cathode and anode tafel curve fitting results, as shown in fig. 3. Therefore, the dynamic polarization electrochemical corrosion detection device can be used for corrosion monitoring of the pipe wall under the conditions of limited space and insufficient power supply and provides a regular corrosion rate result.
Claims (4)
1. A dynamic polarized electrochemical corrosion detection apparatus, comprising: the device comprises a main controller, a reference electrode, an auxiliary electrode, a working electrode, an electrolytic cell, a voltage excitation module, a data acquisition module, a display module and a constant potential circuit module; the electrolytic cell is internally provided with a reference electrode, an auxiliary electrode and a working electrode, wherein the working electrode is used for enabling a solution in the electrolytic cell to perform electrochemical reaction, the reference electrode is used as a reference standard of the working electrode, and the auxiliary electrode is used for transmitting corrosion current to the working electrode;
the constant potential circuit module is connected with the voltage excitation module at the input end and the reference electrode, the auxiliary electrode and the working electrode at the output end, and is used for applying excitation voltage given by the voltage excitation module between the reference electrode and the working electrode and keeping the pressure difference between the working electrode and the reference electrode constant;
the input end of the voltage excitation module is connected with the main controller and is used for generating excitation voltage;
the input end of the data acquisition module is connected with the working electrode, the output end of the data acquisition module is connected with the main controller, and the data acquisition module is used for amplifying and converting a current signal output by the working electrode into a voltage signal and then converting the voltage signal into a digital signal to be input into the main controller;
the main controller is used for controlling the voltage excitation module to generate excitation voltage which changes in a certain rule, monitoring the voltage of the reference electrode in real time, calibrating the pressure difference between the reference electrode and the working electrode, and simultaneously transmitting the data input by the data acquisition module to the display module;
the display module is used for displaying the excitation voltage, the corresponding corrosion current and the time information.
2. The dynamic polarized electrochemical corrosion detection device according to claim 1, wherein the reference electrode is a saturated calomel electrode, the working electrode is made of a material to be detected in a cylindrical shape, the auxiliary electrode is a platinum wire electrode, and the effective area of the end part is 0.5-0.7 cm 2 The effective area of the end part of the working electrode is 0.1-0.2 times of that of the end part of the auxiliary electrode, and the auxiliary electrode and the working electrode are respectively positioned at two ends of the electrolytic cell.
3. The detection method of the dynamic polarization electrochemical corrosion detection device according to claim 1, wherein the constant potential circuit is characterized in that the non-inverting input end of the operational amplifier U1 is connected with the voltage excitation module, the inverting input end is connected with the output end and is connected with the inverting input end of the operational amplifier U2 through the resistor R1, the inverting input end of the operational amplifier U2 is connected with the inverting input end and the output end of the operational amplifier U3 through the resistor R2, the non-inverting input end of the operational amplifier U2 is connected with the ground, the output end of the operational amplifier U2 is connected with the reference electrode, the non-inverting input end of the operational amplifier U3 is connected with the auxiliary electrode, the inverting input end of the operational amplifier U4 is connected with the output end through the resistor R3, the non-inverting input end is connected with the ground and is connected with the main controller through the capacitor C1.
4. The method for detecting dynamic polarized electrochemical corrosion according to claim 1, comprising the steps of:
s1, adding an etching medium solution into an electrolytic cell, so that a reference electrode, an auxiliary electrode and a working electrode are completely immersed into the etching medium solution, and waiting for a period of time until the electrodes and the medium reach a stable state;
s2, starting from an initial potential, gradually increasing excitation voltage in a linear mode, and recording current response of an auxiliary electrode after the system reaches balance at each potential point;
s3, drawing a dynamic potential scanning curve by taking the potential as an abscissa and the current as an ordinate;
s4, analyzing an electrokinetic potential scanning curve, identifying the initial potential of corrosion, namely the corrosion potential and the critical potential, namely the potential with obvious current increase, and evaluating the corrosion rate and the corrosion type according to the curve shape and the current value.
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