CN112461744B - Electrochemical testing device and method for metal failure under liquid film - Google Patents

Electrochemical testing device and method for metal failure under liquid film Download PDF

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CN112461744B
CN112461744B CN202011129433.9A CN202011129433A CN112461744B CN 112461744 B CN112461744 B CN 112461744B CN 202011129433 A CN202011129433 A CN 202011129433A CN 112461744 B CN112461744 B CN 112461744B
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liquid film
working
thickness
electrode
liquid
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CN112461744A (en
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李谦
范洪强
李谋成
刘异峰
鲁鹏
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University of Shanghai for Science and Technology
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    • G01N17/02—Electrochemical measuring systems for weathering, corrosion or corrosion-protection measurement
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract

The invention discloses an electrochemical testing device and a testing method for metal failure under a liquid film. The method can simulate the corrosion failure process of the metal material in the atmospheric environment under the condition of different liquid film thicknesses, and has the advantage of simultaneously carrying out atmospheric corrosion evaluation analysis on a plurality of samples or the samples in the environment with a plurality of liquid film thicknesses at high flux and high efficiency. The testing method of the invention comprises the steps of assembling the sample table, and setting a spraying program and an environment; simulation testing; controlling the thickness of the liquid film; and (6) performing electrochemical test and recording experimental data. The invention can simulate liquid films with different thicknesses and gradient changes; the test efficiency can be greatly improved; can realize high-flux electrochemical characterization, and has the characteristics of simple equipment, easy control and high accuracy. The invention has wide application prospect in the research field of atmospheric corrosion of metal materials.

Description

Electrochemical testing device and method for metal failure under liquid film
Technical Field
The invention belongs to the field of metal material atmospheric corrosion research, particularly relates to an experimental device for generating a liquid film with controllable thickness or a liquid film with gradient thickness, and particularly relates to an electrochemical test method for high-flux and high-efficiency metal material corrosion failure evaluation in the environment of the liquid film with controllable thickness or the liquid film with gradient thickness.
Background
Atmospheric corrosion of a metal material refers to a chemical or electrochemical corrosion process under liquid film coverage. In the atmospheric environment, solid particles are deposited on the surface of a metal material, and when the relative humidity of the environment reaches above a certain critical humidity, condensed water vapor promotes the generation of a liquid film with the thickness of several microns or even hundreds of microns. The oxygen dissolved in the liquid film can directly cause chemical corrosion of the metal material; meanwhile, a liquid film dissolved with anions and cations forms a micro battery on the surface of a metal material, electrochemical corrosion is caused, and the harmfulness of the electrochemical corrosion and the chemical corrosion is stronger than that of the pure chemical corrosion. In addition, the liquid film on the surface of the metal material is not a stable liquid film at first but dynamically changed, for example, wang Jia finds that the thickness of the liquid film is dynamically changed along with the change of environmental influence factors such as temperature, relative humidity, precipitation and the like according to experiments in the book of 'the effect of the liquid film form in atmospheric corrosion', the dissolved oxygen amount, the solution resistance and the like of the liquid film with different thicknesses are different, so that the corrosion characteristics and the corrosion resistance mechanism of the metal material under the condition of different liquid film thicknesses are researched, the atmospheric corrosion rule of the metal material is facilitated to be known, and a certain guiding effect is provided for failure analysis and practical application of the metal material.
The traditional method for constructing a liquid film, for example, chinese patent with patent publication No. CN208313226U, discloses a high-precision thin liquid film thickness control forming device capable of overcoming capillary phenomenon, wherein a working electrode is placed in a solution, the liquid film thickness of a working surface is controlled by controlling the lifting of a platform, a probe connected with an ohmmeter is suspended above the working surface, and the probe is slowly moved to the working surface. The difference between the ohmic expression number of the probe just contacted with the upper surface of the liquid film and the ohmic expression number of the probe contacted with the working surface is large, so that the distance traveled by the probe is used for determining the thickness of the liquid film. The technology has a problem that the evaporation of the solution causes that the thickness of the liquid film cannot be maintained for a long time, and in order to solve the problem, a spraying device is required to maintain the humidity.
The above problems can be solved by adding a spraying device to construct a liquid film, for example, chinese patent No. CN209372660U discloses a device for generating a thin liquid film on a metal surface, wherein a working electrode is placed in a container capable of controlling liquid inlet amount and liquid outlet amount so as to control mist humidity, and when mist slowly forms a liquid film on a working surface and reaches a gas-liquid equilibrium, a stable liquid film with a certain thickness is formed. The technical problem of the technology is that although the mist is supplemented, the gas-liquid equilibrium point is difficult to determine, so that the formed liquid film cannot be accurately determined. To solve the above technical problems, there is a need for a detecting device capable of accurately determining a liquid film thickness required and a control device for maintaining the liquid film thickness.
The traditional electrochemical corrosion characterization method is used for example in Dong Chaofang in the document 'evaluation of corrosion behavior of 316L stainless steel in west sand ocean atmosphere environment', a three-electrode system is constructed in a solution to perform electrochemical tests such as polarization curve, electrochemical impedance spectrum and the like, the electrochemical test method is mature, but the existing problems are obvious, only macroscopic electrochemical information can be provided for the corrosion process of a working electrode, and the specific details of the local part cannot be known. To solve this problem, the working electrode can be modified to be an array electrode to test the local electrochemical information of the sample.
The application principle of the array electrode technology, for example, fan Lin, is summarized through literature research and study in the document "application progress of the array electrode technology in the corrosion field", and the array electrode is formed by miniaturizing the size of a plurality of working electrodes and arranging the working electrodes in an array manner, wherein each working electrode is used as an independent channel to perform electrochemical test, so that local corrosion information of the working electrodes can be obtained. However, the application of the traditional array electrode is only simple single array electrode test, has certain defects, and does not give full play to the advantages of high flux and high working efficiency.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to overcome the defects in the prior art and improve the application of the prior art, and provides an electrochemical testing device for metal failure under a liquid film, a testing method thereof, an experimental device for generating a liquid film with controllable thickness and a liquid film with gradient thickness, and a set of electrochemical testing system capable of performing high-flux and high-efficiency metal material atmospheric corrosion failure evaluation under the environment of generating the liquid film with controllable thickness and liquid film with gradient thickness.
In order to achieve the purpose, the invention adopts the following technical scheme:
an electrochemical testing device for metal failure under a liquid film comprises a spraying box, a spraying control device, a sample table, a liquid film thickness control device, an electrochemical workstation, a working electrode probe and a computer;
the spray box is used as a mist flow providing device for forming a liquid film and comprises a liquid box and a working box, wherein the liquid box is used for storing liquid of required spray types; the top of the working box comprises a sealing cover with a sealing ring, the sealing cover is transparent and can show the internal condition, the middle part of the working box is provided with a sample table supporting plate, the supporting plate is used for placing a sample table, and a space is reserved at the bottom of the working box and can be used for collecting liquid condensed by spraying and discharging the liquid through a liquid discharge pipeline; a small hole is reserved in the wall of the working box, a rubber plug is used for sealing the small hole, and the small hole is used as a mounting hole reserved for a lead connected with a working electrode and an electrochemical workstation; the working is communicated with the liquid tank through a mist outlet of the wall of the working tank through a pipeline; a pump is arranged in the liquid tank, an air compressor is arranged outside the liquid tank, and the liquid in the liquid tank is sucked into the atomizer by using the pump and the air compressor to form a mist flow which passes through the mist outlet from the pipeline so as to enable the mist to enter the working tank;
a humidity sensor is arranged in the working box, the control spraying device is arranged at the position close to the working box or the position close to the liquid box, and the control spraying device is connected with a pump, an air compressor and a control part of the humidity sensor through a circuit to carry out negative feedback regulation on the humidity and the spraying quantity in the working box;
the sample table is arranged in the working box and used for placing a working electrode probe, and the sample table is fixedly connected with a supporting plate of the working box through a base; the sample stage is connected with a liquid film thickness control device through a working platform to adjust the thickness of a liquid film on the surface of the working electrode;
the liquid film thickness control device is used for automatically adjusting the thickness of a liquid film on the surface of a working electrode on the sample platform and is connected with the sample platform;
the electrochemical workstation is connected with the working electrode probe and is used for acquiring corrosion kinetic data of the working electrode in a corrosion failure process;
and the computer is in signal connection with the electrochemical workstation and is used for recording corrosion kinetic data of the working electrode in the corrosion failure process.
Preferably, the control spraying device comprises a program setting panel used as an input device for setting the parameter setting of the test environment; the switch of the air compressor and the controller of the humidity factor are controlled by the program setting panel, and the switch of the air compressor and the controller of the humidity factor are in signal connection with the spray box equipment in a cable or wireless communication mode so as to perform positive feedback adjustment on the fog flow and the humidity signal.
Preferably, the sample platform comprises a base and a working platform, two supporting lug plates which are arranged in parallel are fixedly arranged on the base, the supporting lug plates are vertically connected with the base, threaded holes are formed in the supporting lug plates, external threads of the screw are matched with internal threads of the supporting lug plates, a nut is fixedly connected to one end of the screw, the working platform is arranged between the two supporting lug plates, the middle of the working platform is fixedly connected to the rod body of the screw, the screw is rotated by a required angle through a knob nut, and the inclined state of the surface of the working platform is regulated and controlled to enable the working platform to reach a horizontal state; the two sides of the working platform crossing the screw rod are provided with 3 through holes, wherein a first through hole and a second through hole are arranged on one side of the working platform, a working electrode and a reference electrode are respectively arranged in the first through hole and the second through hole, the working electrode and the reference electrode are isolated from the surfaces of the through holes through insulating materials, the upper surface of the working electrode is flush with the upper surface of the working platform, a platinum wire is used as an auxiliary electrode, the platinum wire surrounds the side surfaces of the working electrode and the reference electrode in a non-contact arrangement mode, and a three-electrode probe is formed by the platinum wire, the working electrode and the reference electrode; three electrodes are connected with the single-channel electrochemical workstation from small holes reserved in the wall of the working box through three leads, and the single-channel electrochemical workstation is connected to a computer through an optical cable;
the method comprises the following steps of cutting sheets with various thicknesses into a perforated shape which does not shield a working surface of the three electrodes, embedding and fixing the sheets on a working platform, enabling the inner edges of the holes of the sheets to be arranged at the outer sides of the range of the working surface of the three electrodes, enabling the cut holes of the sheets to form a cofferdam with the working surface of the three electrodes, forming a small 'water pool' capable of containing a liquid film in an inner area of the cofferdam, enabling the working surface of the three electrodes to be located at the bottom of the liquid film, and enabling the thicknesses of the various sheets to be different liquid film thicknesses corresponding to the surfaces of the working electrodes when the surfaces of the liquid film are level with the upper edge of the cofferdam, namely the depths of the water pool; the working platform and the sheet are made of insulating materials, so that galvanic corrosion between the working platform and the electrode is avoided;
the device for controlling the thickness of the liquid film comprises a motor with a rotor, wherein the motor is arranged in a third through hole of the working platform, the rotor of the motor is fixedly connected with one end of a connecting rod, the other end of the connecting rod is connected with a brush, the brush can be driven to swing when the rotor of the motor rotates, bristles of the brush sweep the upper edge of a cofferdam formed by the slices, and the excessive liquid film on the sides of the 'water pool' can be brushed away, so that the liquid film on the working electrode can be automatically adjusted and is stabilized at the thickness of the liquid film corresponding to the thickness of the corresponding slice; the brush is made of an insulating material.
Preferably, the periphery of the threaded hole of the supporting lug plate is provided with angle marking scales of 360 degrees in total, and the inclination angle of the working platform is controlled to be adjusted according to the angle marking scales so as to realize the liquid film state with gradient thickness.
Preferably, the working electrode is an array working electrode, the metal to be measured is cut into N × N small square column wires with the side length of a square cross section not higher than 1mm, wherein N is a natural number not less than 2, the small square column wires are arranged in order according to the N × N array to form a square bundle metal array, one end face of the metal array is flush to form an array plane and used as a working face of the array working electrode, the end part of each small square column on one end face of the metal array is connected with a lead, and the side face of the square bundle metal array is wrapped by an insulator material and then embedded in a first through hole of the working platform to form the cylindrical working electrode.
Preferably, two platinum sheets are respectively attached to the sides of the 'water pool', a disconnected conductive terminal is formed on the bank side of the 'water pool', the motor, the power supply, the brush and the two conductive patches are connected by a metal wire to form a circuit, when the thickness of a set liquid film, namely the 'water pool' is full, a current loop access state is formed, a rotor of the motor starts to drive the brush to work, the liquid film which is excessive on the sides of the 'water pool' is brushed away, after the liquid film between the two conductive patches is brushed away when the liquid film is brushed away, the electric connection between the two conductive patches is disconnected, so that the liquid film on the surface of the working electrode is automatically adjusted and stabilized at the thickness of the liquid film corresponding to the thickness of the sheet, and the requirement of generating the liquid film with controllable thickness is achieved through the combined use of the sheet and the brush.
Preferably, a rotor of a motor of the device for controlling the thickness of the liquid film is connected with the L-shaped or inverted T-shaped brush through a connecting rod, and a dry battery with a positive electrode and a negative electrode or other power supplies are used as power supplies.
Preferably, the sheet for controlling the thickness of the liquid film is made of hydrophobic substances with contact angles not less than 90 degrees, and errors caused by condensation and adhesion of mist flow on the working platform and thickness control of the liquid film can be avoided.
Preferably, the side surface of the conductive patch is sealed by insulating waterproof glue, so that the conductive patch and the sheet are kept in a non-contact arrangement structural form, and the liquid film on the sheet is prevented from being conducted by itself;
preferably, the exposed end of the rotor of the motor is a cross-shaped duct; one end of the connecting rod is provided with a pore channel, and one end of the connecting rod is inserted into the cross pore channel of the rotor and then fixedly connected by a bolt and a nut; the other end of the connecting rod is a cross-shaped pore channel; the brush handle end of the brush is a single hole, the brush handle end is inserted into a cross hole of the connecting rod and fixedly connected by a bolt and a nut to form a movement mechanism of the device for controlling the thickness of the liquid film.
Preferably, a levelness adjusting device is arranged, the levelness adjusting device consists of a series of horizontal adjusting nuts, the horizontal adjusting nuts are arranged at the positions, close to the edges, of the working platform, the inclination angle of the working platform is adjusted by screwing the nuts and the horizontal adjusting nuts, and the working platform is adjusted to be in a horizontal state.
The electrochemical test method for metal failure under a liquid film adopts the electrochemical test device for metal failure under a liquid film to carry out test analysis, and comprises the following steps:
a. electrochemical test device setup:
assembling a sample table, manufacturing a working electrode, installing the prepared reference electrode and the working electrode on the sample table together, connecting the three electrodes with an electrochemical workstation through a lead, connecting the electrochemical workstation to a computer through a lead, installing data collection and processing software in a computer system, opening a cover of a salt spray box, arranging the sample table on a working box supporting plate of the spray box, fixing a working platform according to experimental requirements, and closing the cover;
b. the control spraying device starts program setting according to the environmental factors of the required humidity, and the control spraying box starts spraying according to the instruction of the control spraying device;
c. the fog flow contacts the surface of the working electrode and is gradually condensed into liquid state, when the target thickness is reached, the conduction of a loop with a rotor and a brush is observed through the transparent sealing cover, the work is started, and the liquid film starts to be stabilized at the set thickness value; according to the purpose of the experiment, the electrochemical workstation and the computer are determined to be started, and the corrosion kinetic data are recorded.
Preferably, the high-throughput electrochemical test is carried out, the number of sample platforms of the electrochemical testing device for metal failure under the liquid film is not less than 2, each sample platform is set with a liquid film condition with constant thickness according to the experimental requirements for the test, and then working electrodes made of sample materials arranged on each sample platform are respectively connected with an electrochemical workstation and a computer, so that the aim of carrying out the high-throughput test on a plurality of samples under the thickness of a plurality of liquid films is fulfilled.
Preferably, a high-flux electrochemical test is carried out, and the liquid film on the working electrode is in gradient distribution by adjusting the inclination angle of the working platform to form a liquid film state with gradient thickness; the working electrode embedded in the workbench adopts an array electrode, and the array electrode is connected with an electrochemical workstation and a computer, so that the corrosion failure process of the metal material under different liquid film thicknesses can be tested at high flux.
Preferably, high-flux electrochemical test is carried out, and through the electrochemical test of the metal material under the gradient liquid film, the metal material can have gradient gradual change due to the environment such as the thickness of the liquid film, and in the comparative analysis of the corrosion test result under the liquid film state with constant thickness, local corrosion kinetic information can be obtained through the array electrode, and the influence of different liquid film thicknesses on the metal material can be represented, so that the purpose of high-flux high-efficiency failure evaluation on the corrosion of the metal material is achieved.
Preferably, in the process of realizing the liquid film with the gradient thickness by the sample stage, the method for calculating the average liquid film thickness on the surface of the working electrode is as follows:
calculating by using the thickness of the liquid film on the surface of the working electrode de, wherein the inclination angle theta and delta abc of the working platform and the horizontal plane are liquid film parts, ab represents the section of the sheet, ab length is the thickness value of the sheet, de represents the surface of at least 5 working electrodes, the length is the actual length value of the working electrode, bn represents the horizontal plane, and Dd and Ee are the thicknesses of the liquid films at the two ends of the at least 5 working electrodes respectively. Let the average liquid film thickness on the surface of de be H de Bd is L bd Bc is L long bc Ab thickness H ab And Dd is H Dd Ee thickness of H Ee Sample length L de Setting H ab ，θ，H Dd ，H ab ，L bd ，L de Using the formula L bc ＝H ab /(tan. Theta.) calculation of L bc From the principle of similarity of triangles H Dd ＝[H ab ×(L bc -L bd )]/L bc (ii) a For the same reason, use formula H Ee ＝[H ab ×(L bc -L bd -L de )]/L bc Calculate H Ee Thus calculating the surface thickness of de as H de ＝(H Dd +H Ee )/2。
Compared with the prior art, the invention has the following obvious substantive characteristics and remarkable advantages:
1. the device is simple and easy to control, can realize the simulation of the liquid film state on the surface of the metal material under the atmospheric condition, and accurately controls the liquid film to be stably kept at the required thickness on the basis of designing a method for detecting the thickness of the liquid film reaching the required thickness;
2. on the basis of realizing the liquid film with the required thickness, the liquid films with different gradient thicknesses can be realized by controlling the angle of the working surface, and the liquid film states with different thicknesses can be realized by replacing patches with different thicknesses;
3. the dynamic data of corrosion of the metal material under liquid films with different thicknesses can be tested by combining the experimental setting state for generating the liquid film with controllable thickness with a single electrode probe and an electrochemical workstation, which plays an important role in understanding the corrosion rule of the metal material in the atmosphere;
4. the method is used in a coupling way with an array electrode technology in an experimental setting state of generating a liquid film with controllable thickness, and can test local dynamic data of corrosion of the metal material under the liquid films with different thicknesses; the dynamic data of the corrosion of the metal material under the liquid films with different thicknesses can be simultaneously tested in the experimental setting state of using the liquid film with the gradient thickness by coupling the experimental setting state with the array electrode technology.
5. The method has wide application prospect in high-efficiency high-flux evaluation and analysis of the corrosion resistance of the metal material in the atmospheric corrosion environment.
Drawings
FIG. 1 is a schematic diagram of a spray box assembly of a mist provider for forming a liquid film in an apparatus according to an embodiment of the present invention.
Fig. 2 is a schematic structural diagram of a sample stage device for placing a sample in the second device according to the embodiment of the present invention.
FIG. 3 is a schematic structural diagram of an apparatus for detecting a liquid film having a desired thickness and accurately controlling the liquid film to be stably maintained at a target thickness according to a third embodiment of the present invention.
FIG. 4 is a schematic diagram illustrating the principle of an electrochemical testing system for metal failure under a liquid film according to various embodiments of the present invention.
Fig. 5 is a schematic diagram illustrating the thickness of the liquid film on the working surface of the working electrode in the liquid film state with gradient thickness according to an embodiment of the present invention.
Figure 6 is a graph of polarization curve test results for 316L stainless steel in a construction of 80 μm thick 5% sodium chloride electrolyte membrane according to example eight of the present invention.
Detailed Description
The above embodiments are further described with reference to the specific embodiments, but the present invention is not limited to these embodiments, and various changes, modifications, substitutions, combinations or simplifications made according to the spirit and principles of the present invention should be equivalent substitutions as long as the technical principles and inventive concepts of the electrochemical testing system for metal materials under liquid film with controllable or gradient thickness are not departed from the present invention. The preferred embodiments of the present invention are detailed below:
the first case is provided for the purpose of performing macroscopic and microscopic electrochemical corrosion tests of a metal material in a liquid film state with a constant thickness.
Example one
In the embodiment, referring to fig. 1 and 4, an electrochemical testing device for metal failure under a liquid film comprises a spray box, a spray control device, a sample stage, a liquid film thickness control device, an electrochemical workstation, a working electrode probe and a computer; the spray box is used as a mist flow providing device for forming a liquid film and comprises a liquid box 3 and a working box 24, wherein the liquid box 3 is used for storing liquid of a required spray type; the top of the working box 24 comprises a sealing cover 25 with a sealing ring, the sealing cover 25 is transparent, the internal condition can be seen, a sample table supporting plate 6 is arranged in the middle of the working box 24, the supporting plate 6 is used for placing a sample table, and a reserved space is reserved at the bottom of the working box 24 and can be used for collecting liquid condensed by spraying and discharging the liquid through a liquid discharge pipeline; a small hole 5 is reserved on the wall of the working box 24, a rubber plug is used for sealing the small hole 5, and the small hole 5 is used as a mounting hole reserved for a lead connected with a working electrode and an electrochemical workstation; the working is communicated with the liquid tank 3 through the mist outlet 1 of the working tank wall 24 and the pipeline 2; a pump 4 is arranged in the liquid tank 3, an air compressor is arranged outside the liquid tank 3, the liquid in the liquid tank 3 is sucked into the atomizer by using the pump 4 and the air compressor to form mist flow, and the mist flow passes through the mist outlet through a pipeline so as to enter the working tank 24; a humidity sensor is arranged in the working box 24, the control spraying device 7 is arranged at the position close to the working box 24 or the position close to the liquid box 3, and the control spraying device 7 is connected with the pump 4, the air compressor and the control part 8 of the humidity sensor through a circuit to carry out negative feedback adjustment on the humidity and the spraying amount in the working box 24; the sample table is arranged in the working box 24 and used for placing a working electrode probe, and the sample table is fixedly connected with the supporting plate 6 of the working box 24 through the base 14; the sample stage is connected with a liquid film thickness control device through a working platform to adjust the thickness of a liquid film on the surface of the working electrode; the liquid film thickness control device is used for automatically adjusting the thickness of a liquid film on the surface of the working electrode 12 on the sample platform and is connected with the sample platform; the electrochemical workstation is connected with the working electrode probe and is used for acquiring corrosion kinetic data of the working electrode 12 in a corrosion failure process; the computer is in signal communication with the electrochemical workstation for recording corrosion kinetics data of the working electrode 12 during corrosion failure.
The device of the embodiment constructs an environment that the liquid film thickness can also have gradient gradual change, and can perform comparative analysis with a corrosion test result in a liquid film state with constant thickness, so that not only can local corrosion dynamics information be obtained, but also the influence of different liquid film thicknesses on metal materials can be represented. The device of the embodiment is simple and easy to control, can realize the simulation of the liquid film state on the surface of the metal material under the atmospheric condition, and accurately controls the liquid film to be stably maintained at the required thickness on the basis of designing a method for detecting the liquid film thickness reaching the required thickness.
Example two
This embodiment is substantially the same as the first embodiment, and is characterized in that:
in this embodiment, referring to fig. 2 and 4, the sample stage includes a base 14 and a working platform, two supporting ear plates 9 arranged in parallel are fixedly disposed on the base 14, the supporting ear plates 9 are perpendicularly connected to the base 14, the supporting ear plates 9 are provided with threaded holes, external threads of the screws 16 are adapted to internal threads of the supporting ear plates 9, one ends of the screws 16 are fixedly connected with nuts 17, the working platform is disposed between the two supporting ear plates 9, the middle portion of the working platform is fixedly connected to a rod body of the screws 16, the screws 16 are rotated by a required angle by turning the nuts 17, and an inclined state of the surface of the working platform is regulated and controlled to enable the working platform to reach a horizontal state; the two sides of the position of the working platform crossing the screw 16 are provided with 3 through holes, wherein a first through hole and a second through hole are arranged on one side of the working platform, a working electrode 12 and a reference electrode 13 are respectively arranged in the first through hole and the second through hole, the working electrode 12 and the reference electrode 13 are isolated from the surfaces of the through holes through insulating materials, the upper surface of the working electrode 12 is flush with the upper surface of the working platform, a platinum wire 10 is used as an auxiliary electrode, the platinum wire 10 surrounds the side surfaces of the working electrode 12 and the reference electrode 13 in a non-contact arrangement mode, and a three-electrode probe is formed by the platinum wire 10, the working electrode 12 and the reference electrode 13; three electrodes are connected with the single-channel electrochemical workstation from small holes 5 reserved in the wall of the working box 24 through three leads, and the single-channel electrochemical workstation is connected to a computer through an optical cable;
the method comprises the following steps of cutting a sheet 11 with various thicknesses into a perforated shape which does not shield a working surface of the three electrodes, embedding and fixing the sheet 11 on a working platform, enabling the inner edge of the hole of the sheet 11 to be arranged outside the range of the working surface of the three electrodes, enabling the cut hole of the sheet 11 to form a cofferdam with the working surface of the three electrodes, forming a small 'pool' capable of containing a liquid film in an inner area of the cofferdam, enabling the working surface of the three electrodes to be located at the bottom of the liquid film, and enabling the thicknesses of the various sheets 11 to be different liquid film thicknesses corresponding to the surfaces of the working electrodes when the surfaces of the liquid films are flush with the upper edge of the cofferdam, namely the depths of the 'pool'; the working platform and the sheet 11 are made of insulating materials, so that galvanic corrosion between the working platform and the electrode is avoided;
the device for controlling the thickness of the liquid film comprises a motor 15 with a rotor, wherein the motor 15 is arranged in a third through hole of the working platform, the rotor of the motor 15 is fixedly connected with one end of a connecting rod, the other end of the connecting rod is connected with a brush 18, the brush 18 can be driven to swing when the rotor of the motor 15 rotates, bristles of the brush sweep the upper edge of a cofferdam formed by the thin slices 11, and excessive liquid films on the sides of a 'water pool' can be brushed away, so that the liquid film on the working electrode 12 can be automatically adjusted and is stabilized at the thickness of the liquid film corresponding to the thickness of the corresponding thin slice 11; the brush 18 is made of an insulating material.
In this embodiment, the working electrode 12 is an array working electrode 19, the metal to be measured is cut into N × N small square column wires with a side length of a square cross section not higher than 1mm, where N is a natural number not less than 2, the small square column wires are regularly arranged according to an N × N array to form a square bundle metal array, one end surface of the metal array is flush with and forms an array plane as a working surface of the array working electrode 19, an end portion of each small square column of one end surface of the metal array is connected with a lead, and a side surface of the square bundle metal array is wrapped with an insulator material and then embedded in a first through hole of a working platform to form the cylindrical working electrode 12.
In the experimental setup state for generating the liquid film with the controllable thickness, the dynamic data of corrosion of the metal material under the liquid films with different thicknesses can be tested by combining with a single electrode probe and an electrochemical workstation, which plays an important role in understanding the corrosion rule of the metal material in the atmosphere; the device can generate the experimental setting state of the liquid film with controllable thickness, is coupled with the array electrode technology for use, and can test the local dynamic data of the corrosion of the metal material under the liquid films with different thicknesses; the dynamic data of the corrosion of the metal material under the liquid films with different thicknesses can be simultaneously tested in the experimental setting state of using the liquid film with the gradient thickness by coupling the experimental setting state with the array electrode technology.
EXAMPLE III
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this embodiment, referring to fig. 3 and 4, two platinum sheets 20 are respectively attached to the sides of the "pool" to form a disconnected conductive terminal on the bank of the "pool", the motor 15, the power supply 22, the brush 18 and the two conductive patches 20 are connected by the metal wire 23 to form a circuit, when the "pool" is full, which is the set liquid film thickness, the current loop path state is formed, the rotor of the motor 15 starts to drive the brush 18 to work, the excess liquid film on the sides of the "pool" is brushed away, and after the liquid film is brushed away, the electrical connection between the two conductive patches 20 is disconnected, so that the liquid film on the surface of the working electrode 12 is automatically adjusted and stabilized at the liquid film thickness corresponding to the thickness of the sheet 11, and the requirement of generating a liquid film with controllable thickness is achieved by the combined use of the sheet 11 and the brush 18.
In this embodiment, the side of the conductive patch 20 is sealed by insulating waterproof glue, so that the conductive patch 20 and the sheet 11 maintain a non-contact structural form, and self-conduction due to a liquid film on the sheet 11 is prevented;
in this embodiment, a small hole is reserved on the working platform to install the motor 15 with a rotor, the rotor is connected with the brush 18 through a connecting rod, two conductive patches 20 are disconnected and attached to the side of the 'pool', the motor 15, the power supply 22, the brush 18 and the two conductive patches 20 are connected through a lead to form a circuit, when the thickness of a set liquid film is reached, namely the 'pool' is full, a circuit access state is formed, the rotor 15 starts to drive the brush 18 to work to brush off excessive liquid film, so that the liquid film on the working electrode 12 is automatically adjusted and stabilized at the thickness value, and the purpose of generating the liquid film with controllable thickness is achieved through the sheet 11 and the brush 18.
Example four
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this embodiment, an electrochemical test method for a metal failure under a liquid film, which uses the electrochemical test device for a metal failure under a liquid film according to the first embodiment, includes the following steps:
a. electrochemical test device setup:
assembling a sample table, manufacturing a working electrode, installing the prepared reference electrode and the working electrode on the sample table together, connecting the three electrodes with an electrochemical workstation through a lead, connecting the electrochemical workstation to a computer through a lead, installing data collection and processing software in a computer system, opening a cover of a salt spray box, arranging the sample table on a working box supporting plate of the spray box, fixing a working platform according to experimental requirements, and closing the cover;
b. the control spraying device starts program setting according to the environmental factors of the required humidity, and the control spraying box starts spraying according to the instruction of the control spraying device;
c. the fog flow contacts the surface of the working electrode and is gradually condensed into liquid state, when the target thickness is reached, the conduction of a loop with a rotor and a brush is observed through the transparent sealing cover, the work is started, and the liquid film starts to be stabilized at the set thickness value; according to the purpose of the experiment, the electrochemical workstation and the computer are determined to be started, and the corrosion kinetic data are recorded.
The method can simulate the corrosion failure process of the metal material under different liquid film thicknesses in the atmospheric environment, the sample stage is assembled, and the spraying program and the environment are set; simulation testing; controlling the thickness of the liquid film; and (6) performing electrochemical test and recording experimental data. The method can simulate liquid films with different thicknesses and gradient changes; the test efficiency can be greatly improved; can realize high-flux electrochemical characterization, and has the characteristics of simple and easily controlled equipment and high accuracy. The method has wide application prospect in the field of atmospheric corrosion research of metal materials.
EXAMPLE five
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this embodiment, referring to fig. 2 and 4, the periphery of the threaded hole of the supporting ear plate 9 is provided with angle marking scales of 360 degrees in total, and the inclination angle of the working platform is controlled to adjust according to the angle marking scales to realize the liquid film state with gradient thickness.
In the present embodiment, referring to fig. 3 and 4, a levelness adjusting means is provided, which is composed of a series of horizontal adjusting nuts 21, the horizontal adjusting nuts 21 are provided at positions near the edges of the working platform, and the working platform is adjusted to be horizontal by adjusting the inclination angle of the working platform by screwing the nuts 17 and the horizontal adjusting nuts 21.
In this embodiment, a high-throughput electrochemical test is performed, the number of sample stages of the electrochemical testing apparatus for metal failure under a liquid film in the first embodiment is not less than 2, each sample stage is set with a liquid film condition with a constant thickness according to experimental requirements to perform an experiment, and then working electrodes made of sample materials set in each sample stage are respectively connected to an electrochemical workstation and a computer, so that a high-throughput test of a plurality of samples under a plurality of liquid film thicknesses is achieved.
In this embodiment, a high-throughput electrochemical test is performed, and the liquid film on the working electrode is distributed in a gradient manner by adjusting the inclination angle of the working platform, so as to form a liquid film state with a gradient thickness; the working electrode embedded in the workbench adopts an array electrode, and the array electrode is connected with an electrochemical workstation and a computer, so that the corrosion failure process of the metal material under different liquid film thicknesses can be tested at high flux.
In the embodiment, for the purpose of achieving higher flux and high working efficiency, an environment that the thickness of the liquid film can also have gradient gradual change is constructed, so that the corrosion test result can be compared and analyzed with the corrosion test result in a liquid film state with constant thickness, not only can local corrosion dynamics information be obtained, but also the influence of different liquid film thicknesses on metal materials can be represented; a single array electrode is miniaturized and high-throughput electrochemical testing of multiple array electrodes is performed simultaneously. The method can simulate the corrosion failure process of the metal material in the atmospheric environment under the condition of different liquid film thicknesses, and has the advantage of simultaneously carrying out atmospheric corrosion evaluation analysis on a plurality of samples or the samples in the environment with a plurality of liquid film thicknesses with high flux and high efficiency.
EXAMPLE six
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this embodiment, a high-throughput electrochemical test is performed, and through the electrochemical test of the metal material under the gradient liquid film, gradual gradient change can be achieved due to the environment such as the thickness of the liquid film, and in the comparative analysis of the corrosion test result in the liquid film state with constant thickness, local corrosion dynamics information can be obtained through the array electrode, and the influence of different liquid film thicknesses on the metal material can be represented, so that the purpose of high-throughput and high-efficiency failure evaluation on the corrosion of the metal material is achieved.
The method simulates liquid films with different thicknesses and gradient changes; the test efficiency can be greatly improved; can realize high-flux electrochemical characterization, and has the characteristics of simple and easily controlled equipment and high accuracy. The embodiment has wide application prospect in the field of atmospheric corrosion research of metal materials.
EXAMPLE seven
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this example, the apparatus for electrochemical testing by constructing a thin liquid film in the first example was used to perform a local, i.e., microscopic electrochemical corrosion test of a metal material in a liquid film state of a gradient thickness. The following operations are different from the above-mentioned local electrochemical corrosion test of metal material in the state of liquid film with constant thickness, in that the working platform is fixed at an angle theta to the horizontal direction by screwing the nut 17 and the horizontal adjusting nut 21, and the platinum sheet 20 should be at the edge of the point shown in fig. 5 a.
In this embodiment, referring to fig. 4 and 5, the schematic diagram of the liquid film thickness of the working surface of the working electrode in the liquid film state with gradient thickness includes the inclination angle θ of the working platform to the horizontal plane, Δ abc is the liquid film portion, ab represents the sheet cross section, ab length is the sheet thickness value, de, fg, hi, jk, lm represent the five working electrode surfaces, length is the actual length value of the working electrode, bn represents the horizontal plane, dd, ee, ff, gg, hh, ii, jj, kk, ll, mm are the liquid film thicknesses at the two ends of the five working electrodes, respectively.
The calculation of the liquid film thickness can be obtained from fig. 4 as follows: calculating by using the thickness of the liquid film on the surface of the working electrode de, wherein the inclination angle theta and delta abc of the working platform and the horizontal plane are liquid film parts, ab represents the section of the sheet, ab length is the thickness value of the sheet, de represents the surface of at least 5 working electrodes, the length is the actual length value of the working electrode, bn represents the horizontal plane, and Dd and Ee are the thicknesses of the liquid films at the two ends of the at least 5 working electrodes respectively. Let the average liquid film thickness on the surface of de be H de Bd is L bd Bc is L long bc Ab thickness H ab And Dd is H Dd Ee thickness of H Ee Sample length L de Setting H ab ，θ，H Dd ，H ab ，L bd ，L de Using the formula L bc ＝H ab /(tan. Theta.) calculation of L bc From the principle of similarity of triangles Dd ＝[H ab ×(L bc -L bd )]/L bc (ii) a Similarly, using the formula H Ee ＝[H ab ×(L bc -L bd -L de )]/L bc Calculate H Ee Thereby calculating the surface thickness of de as H de ＝(H Dd +H Ee )/2. The thickness of the liquid film on the surface of the other four working electrodes can be obtained by the same method. It should be noted that the reference electrode, the auxiliary electrode and the working electrode are not shown at the same time at the right end of the diagram 4, and in real cases, the liquid surface of the liquid film needs to cover the three electrodes at the same time, but the use of the principle of the liquid film thickness calculation method is not affected. The embodiment realizes the purpose of realizing high-flux electrochemical test in the process of testing the corrosion failure of the metal material under the thickness of the gradient liquid film on one working electrode.
After the local electrochemical corrosion kinetic data of the metal material in the liquid film with the gradient thickness are measured through experiments, the local electrochemical corrosion kinetic data can be compared with the kinetic data in the liquid film with the constant thickness for analysis to obtain the influence of liquid films with different thicknesses on the corrosion process of the metal material, so that the purpose of high-flux and high-efficiency failure evaluation on the corrosion of the metal material is achieved.
Example eight
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in the present embodiment, referring to fig. 1, the mist flow provider spray box apparatus for forming a liquid film comprises a liquid box 3 for storing a liquid of a desired spray type and a working box 24; the top of the working box comprises a sealing cover 25 with a sealing ring, the sealing cover is transparent and can see the internal situation, the middle part of the working box is provided with a sample table supporting plate 6 for placing a sample table, and the reserved space at the bottom of the working box is used for collecting liquid condensed by spraying and is discharged through a liquid discharge pipeline; a small hole 5 is reserved on the wall of the working box and is sealed by a rubber plug, and a lead for connecting a working electrode and an electrochemical workstation is reserved at the position; the working box and the liquid box are connected by a pipeline 2 through a fog outlet 1 on the wall of the working box, and liquid in the liquid box is sucked into the atomizer by a pump 4 in the liquid box and a commercial air compressor outside the liquid box to form fog flow which enters the working box through the fog outlet by the pipeline; and a humidity sensor is arranged at the position, adjacent to the wall of the working tank, of the control spraying device 7, the control spraying device is connected to carry out negative feedback humidity adjustment, and a program setting panel for controlling the spraying device is arranged for setting the parameter setting of the test environment.
In this embodiment, referring to fig. 2, the sample stage for placing the sample includes a base 14, two supporting ear plates 9 on the base, an angle mark carved on the supporting ear plates 9 around the nut, and a working platform embedded with a platinum wire 10, a sheet 11 with various thicknesses, and three small holes. In addition, the middle of the working platform is internally provided with a pore channel. One end of a supporting lug plate 9 of the sample table is integrated with the base, and the other end of the supporting lug plate is provided with a small hole which can be fixed with a middle hole channel of the working platform into a horizontal state by screwing a nut 17 through a nut 16 with a proper hole diameter. The three small holes are reserved for installing a working electrode 12, a reference electrode 13 and a motor 15 with a rotor respectively. The platinum wire, the working electrode and the reference electrode form three electrodes, and 19 is a schematic diagram of a 5 multiplied by 5 array working electrode.
In this embodiment, referring to fig. 3, an apparatus for detecting the attainment of a desired liquid film thickness and accurately controlling the liquid film to be stably maintained at the target thickness includes a motor with a rotor, such as 15 in fig. 2, a connecting rod and "L" or "t" shaped brush 18, a dry cell or other power source 22 with positive and negative electrodes, a conductive platinum sheet 20, and a copper wire 23 connecting the components into a circuit.
In the case of the apparatus of fig. 1 to 3, and with reference to fig. 4, by means of the present example, a macroscopic electrochemical corrosion test of a metallic material in the form of a liquid film of constant thickness can be carried out. Cutting a metal sample into a small cylinder with the diameter of 4mm multiplied by 5mm by warp, grinding two surfaces of the cylinder from 600# to 2000# by SiC abrasive paper step by step, taking one surface as a working surface, welding a copper wire on the other surface, inlaying the copper wire into the cylinder with the diameter of 5mm multiplied by 10mm by using epoxy resin, polishing the working surface by using diamond polishing paste with the diameter of 0.5 mu m, washing the polished working surface by using distilled water, drying the working surface by cold air, ultrasonically cleaning the working surface by using alcohol, and drying the working surface by the cold air to obtain a working electrode WE with the exposed area of 4mm in diameter; installing WE at a small hole 12 with the aperture diameter of phi 5mm on a working platform of a sample table, inserting a commercial silver chloride reference electrode RE with the aperture diameter of phi 3.8mm multiplied by 5mm into a hole 13, and installing the hole 12 and the hole 13 together in an epoxy resin isolation way at a distance of 1 mm; a platinum wire with a diameter of 0.5mm as an auxiliary electrode CE surrounding WE and RE at a distance of 1mm, the platinum wire being positioned as 10; furthermore, a polyethylene terephthalate sheet with a target thickness was attached to the periphery of 2mm from the CE with a double-sided tape; and then the working platform is fixed to be in a horizontal state, namely, the angle is 0 degree with the horizontal direction by screwing the screw cap 17 and the horizontal adjusting nut 21, a liquid film control circuit in the third drawing is installed, it needs to be noted that the brush 18 cannot be contacted with the platinum sheet 20, the brush can sweep from the upper part of the working electrode, the position of the platinum sheet only needs to be at any position of the side of a water pool, and the sample platform is ready. Then the sample stage is placed on a sample support plate 6 of the spray box, the three electrodes are connected with the single-channel electrochemical workstation from a small hole 5 reserved in the wall of a working box 24 through three copper wires, the single-channel electrochemical workstation is connected to a computer through an optical cable, and a sealing cover 25 of the salt spray box is covered. Electrochemical test conditions of a single-channel electrochemical workstation and a computer are set according to experimental purposes, and the experimental conditions of the spray box are set to be 100% of constant relative humidity at room temperature. The spraying box starts spraying according to an instruction for controlling the spraying device; the mist flow contacts the surface of the working electrode and is gradually condensed into liquid, when the target thickness is reached, the conduction of a loop with the rotor 15 and the brush 18 is observed through the transparent sealing cover, the work is started, the liquid film starts to be stabilized at a set thickness value, and the computer and the single-channel electrochemical workstation start to record and collect corrosion dynamic data respectively.
In the embodiment, the test result of the polarization curve of 316L stainless steel in a 5% sodium chloride electrolyte membrane with the thickness of 80 μm is shown in fig. 6, the repeatability of the test result of the polarization curve of two times is good, and the potential at the position where the current density rapidly rises, namely the pitting potential, is 259mV, which proves that the precision of controlling the thickness of the liquid membrane is good.
By the device of the embodiment, the local, namely microscopic electrochemical corrosion test of the metal material in the liquid film state with constant thickness can be carried out. The method comprises the following steps of cutting metal samples into 25 small square column wires with the diameter of 0.5mm multiplied by 5mm through warps, arranging the small square column wires in a 5 multiplied by 5 array, taking one surface as a working surface, welding copper wires on the other surface, inlaying the small square column wires together with epoxy resin into a cylindrical working electrode with the diameter of phi 5mm multiplied by 10mm, processing the working electrode, CE, RE and a thin patch as described above, fixing a working platform to be in a horizontal state, namely, 0 degree is formed between the working platform and the horizontal direction through screwing a screw cap 17 and a horizontal adjusting nut 21, installing a liquid film control circuit in the figure 3, and preparing the sample platform. Then the sample stage is placed on a sample support plate 6, the array electrode and the array electrode electrochemical workstation are connected through 25 copper wires from a small hole 5 reserved in the wall of a working box 24, the array electrode electrochemical workstation is connected to a computer through an optical cable, and a sealing cover 25 of the salt spray box is covered. The electrochemical testing conditions of the array electrode electrochemical workstation and the computer are set according to the experimental purpose of the computer, and the experimental conditions of the spray box are set to be 100% of constant relative humidity at room temperature. The spraying box starts spraying according to an instruction for controlling the spraying device; the fog flow contacts the surface of the working electrode and is gradually condensed into liquid state, when the fog flow reaches the target thickness, the conduction of a loop with the rotor 15 and the brush 18 is observed through the transparent sealing cover and starts to work, the liquid film starts to be stable, and the computer and the array electrode electrochemical workstation start to record corrosion kinetic data.
Example nine
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this embodiment, the number of the sample stages of the electrochemical testing apparatus in the first embodiment is set to 10, 10 sheets with different thicknesses are attached to the working platforms of the 10 sample stages, and then each working electrode is respectively connected to the electrochemical workstation and the computer, so as to achieve the purpose of simultaneously testing a plurality of samples.
The purpose that the corrosion failure process of metal material realized high flux electrochemistry test under the different invariable liquid film thickness of simultaneous test was realized to this embodiment, on the basis of realizing the liquid film of required thickness, can realize the liquid film of different gradient thickness through the angle of control working face, through the paster of changing different thickness, can realize the liquid film state of different thickness.
Example ten
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this embodiment, the control spraying device includes a program setting panel as an input device for setting the parameter setting of the test environment; the switch of the air compressor and the controller of the humidity factor are controlled by the program setting panel, and the switch of the air compressor and the controller of the humidity factor are in signal connection with the spray box equipment in a cable or wireless communication mode so as to perform positive feedback adjustment on the fog flow and the humidity signal.
The device of the embodiment simulates liquid films with different thicknesses and gradient changes; the test efficiency can be greatly improved; can realize high-flux electrochemical characterization, and has the characteristics of simple and easily controlled equipment and high accuracy. The device of the embodiment has wide application prospect in the field of atmospheric corrosion research of metal materials.
EXAMPLE eleven
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this embodiment, the rotor of the motor 15 of the device for controlling the thickness of the liquid film is connected to the brush 18 in an "L" or "t" shape through a connecting rod, and a dry battery or other power source with positive and negative electrodes is used as the power source 22. The conductive platinum sheet is a copper conducting wire which connects all the parts into a loop, all the parts can be removed and replaced by a straight nonconductive plastic sheet, although the function of detecting the time for reaching the liquid film thickness set by the experiment can be lost, the aim of controlling the liquid film thickness can be achieved by controlling the upper limit of the liquid film through the nonconductive plastic sheet.
Example twelve
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this embodiment, the device for controlling the thickness of the liquid film comprises a motor with a rotor, a brush connected with a connecting rod in an L shape or an inverted T shape, a dry battery or other power supply with a positive electrode and a negative electrode, a conductive platinum sheet, a copper wire connecting the components into a loop, and sheets with various thicknesses. The device comprises various thin sheets with different thicknesses, wherein the thin sheets are cut into a shape which does not shield a working surface of the three electrodes and then are embedded in a working platform to form a small ' water pool ' for accommodating a liquid film with fixed thickness, the bottom of the water pool ' comprises two reserved small holes for placing a working electrode and a reference electrode respectively and a platinum wire which is used as an auxiliary electrode to be embedded around the two small holes, the various thin sheets are attached to the working platform and do not cover the working electrode through cutting, the liquid film is settled at the cutting part to form the ' water pool ' shape, the working electrode is arranged at the bottom of the ' water pool ', and the thickness of the various thin sheets is just the thickness of the liquid film on the surface of the working electrode, namely the height of the ' water pool '; a small hole is reserved on the working platform and is provided with a motor with a rotor, the rotor is connected with the brush through a connecting rod, two platinum sheets are disconnected and attached to the edge of the water tank, the motor, a power supply, the brush and the two platinum sheets are connected through a copper wire to form a loop, when the set liquid film thickness, namely the water tank, is full, a passage state is formed, the rotor starts to drive the brush to work and brush away excessive liquid films, so that the liquid films on the working electrodes are automatically adjusted and stabilized at the thickness value, and the purpose of generating the liquid films with controllable thickness is achieved through the sheets and the brush; the thin sheet for controlling the thickness of the liquid film is made of hydrophobic substances with a contact angle larger than 90 degrees, such as polytetrafluoroethylene, and the like, so that errors caused by the fact that fog flow condensation is adhered to the working platform and then the thickness of the liquid film is controlled can be avoided to the greatest extent. The brush is made of insulating materials such as polytetrafluoroethylene, the conductive patch is made of materials with good conductivity and inertia such as platinum sheet and gold sheet, and the conductive patch is sealed on the non-contact surface of the sheet by insulating waterproof glue such as silica gel to prevent the self conduction of a liquid film on the sheet; the exposed end of the rotor of the motor is a cross-shaped pore channel; one end of the connecting rod is provided with a pore canal which is inserted into the cross pore canal of the rotor and then fixedly connected by a bolt and a nut; the other end of the connecting rod is a cross pore canal; the upper end of the brush is a single pore channel, is inserted into the cross pore channel of the connecting rod and is fixedly connected with the screw cap by a bolt.
The mist flow provider spray box for forming the liquid film comprises a liquid box, a spray head and a spray head, wherein the liquid box is used for storing liquid of a required spray type; when the type of the liquid is changed into salt spray, the electrochemical test of metal corrosion failure in sodium chloride with different concentrations under a liquid film can be carried out by changing the concentration of the sodium chloride in the salt spray; when the liquid species are changed to other species of ionic concentration, the device has the function similar to that of performing electrochemical tests in different thin liquid film liquid environments. The method can simulate the corrosion failure process of the metal material in the atmospheric environment under the condition of different liquid film thicknesses, and has the advantages of simultaneously carrying out atmospheric corrosion evaluation analysis on a plurality of samples or the samples in the environment with a plurality of liquid film thicknesses with high flux and high efficiency.
The embodiments of the present invention have been described with reference to the accompanying drawings, but the present invention is not limited to the embodiments, and various changes and modifications can be made according to the purpose of the invention, and any changes, modifications, substitutions, combinations or simplifications made according to the spirit and principle of the technical solution of the present invention shall be equivalent substitutions, as long as the purpose of the present invention is met, and the present invention shall fall within the protection scope of the present invention without departing from the technical principle and inventive concept of the present invention.

Claims (13)

1. The utility model provides a metal inefficacy electrochemistry testing arrangement under liquid membrane which characterized in that: comprises a spraying box, a spraying control device, a sample table, a liquid film thickness control device, an electrochemical workstation, a working electrode probe and a computer;
the spray box is used as a mist flow providing device for forming a liquid film and comprises a liquid box (3) and a working box (24), wherein the liquid box (3) is used for storing liquid of a required spray type; the top of the working box (24) comprises a sealing cover (25) with a sealing ring, the sealing cover (25) is transparent and can see the internal condition, a sample table supporting plate (6) is arranged in the middle of the working box (24), the supporting plate (6) is used for placing a sample table, and a reserved space is reserved at the bottom of the working box (24) and can be used for collecting liquid condensed by spraying and discharging the liquid through a liquid discharge pipeline; a small hole (5) is reserved in the wall of the working box (24), a rubber plug is used for sealing the small hole (5), and the small hole (5) is used as a mounting hole reserved for a lead connected with a working electrode and an electrochemical workstation; the working is communicated with the liquid tank (3) through a pipeline (2) through a mist outlet (1) of the working tank (24); a pump (4) is arranged in the liquid tank (3), an air compressor is arranged outside the liquid tank (3), the liquid in the liquid tank (3) is sucked into the atomizer by the pump (4) and the air compressor, a mist flow is formed, the mist flows through a mist outlet from a pipeline, and the mist enters the working tank (24);
a humidity sensor is arranged in the working box (24), the control spraying device (7) is arranged at the position close to the working box (24) or the position close to the liquid box (3), and the control spraying device (7) is connected with a pump (4), an air compressor and a control part (8) of the humidity sensor through a circuit to carry out negative feedback regulation on the humidity and the spraying amount in the working box (24);
the sample table is arranged in the working box (24) and used for placing a working electrode probe, and the sample table is fixedly connected with a supporting plate (6) of the working box (24) through a base (14); the sample stage is connected with a liquid film thickness control device through a working platform to adjust the thickness of a liquid film on the surface of the working electrode;
the liquid film thickness control device is used for automatically adjusting the thickness of a liquid film on the surface of a working electrode (12) on the sample table and is connected with the sample table;
the electrochemical workstation is connected with the working electrode probe and is used for acquiring corrosion kinetic data of the working electrode (12) in a corrosion failure process;
the computer is in signal connection with the electrochemical workstation and is used for recording corrosion kinetic data of the working electrode (12) in the corrosion failure process;
the control spraying device comprises a program setting panel which is used as input equipment and used for setting parameter setting of a test environment; the switch of the air compressor and the controller of the humidity factor are controlled by a program setting panel, and the switch of the air compressor and the controller of the humidity factor are in signal connection with the spray box equipment in a cable or wireless communication mode so as to perform positive feedback adjustment on a mist flow and a humidity signal;
the sample platform comprises a base (14) and a working platform, wherein two supporting lug plates (9) which are arranged in parallel are fixedly arranged on the base (14), the supporting lug plates (9) are vertically connected with the base (14), the supporting lug plates (9) are provided with threaded holes, external threads of a screw rod (16) are matched with internal threads of the supporting lug plates (9), a nut (17) is fixedly connected with one end of the screw rod (16), the working platform is arranged between the two supporting lug plates (9), the middle part of the working platform is fixedly connected onto a rod body of the screw rod (16), the screw rod (16) is rotated by a required angle through turning the nut (17), the inclined state of the surface of the working platform is regulated, and the working platform is made to be in a horizontal state; the two sides of the position of the working platform crossing the screw rod (16) are provided with 3 through holes, wherein a first through hole and a second through hole are arranged on one side of the working platform, a working electrode (12) and a reference electrode (13) are respectively arranged in the first through hole and the second through hole, the working electrode (12) and the reference electrode (13) are isolated from the surfaces of the through holes through insulating materials, the upper surface of the working electrode (12) is flush with the upper surface of the working platform, a platinum wire (10) is used as an auxiliary electrode, the platinum wire (10) surrounds the side surfaces of the working electrode (12) and the reference electrode (13) in a non-contact arrangement mode, and a three-electrode probe is formed by the platinum wire (10), the working electrode (12) and the reference electrode (13); three electrodes are connected with the single-channel electrochemical workstation from a small reserved hole (5) on the wall of the working box (24) through three leads, and the single-channel electrochemical workstation is connected to a computer through an optical cable;
the method comprises the following steps of cutting a sheet (11) with various thicknesses into a shape with holes which does not shield a three-electrode working surface, embedding and fixing the sheet (11) on a working platform, enabling the inner edge of the hole of the sheet (11) to be arranged on the outer side of the range of the three-electrode working surface, enabling the cut-off hole part of the sheet (11) to form a cofferdam with the three-electrode working surface, forming a small 'water pool' capable of containing a liquid film in the inner area of the cofferdam, enabling the three-electrode working surface to be positioned at the bottom of the liquid film, and enabling the thicknesses of various sheets (11) to be different liquid film thicknesses corresponding to the surfaces of working electrodes when the surfaces of the liquid film are flush with the upper edge of the cofferdam, namely the depths of the water pools; the working platform and the sheet (11) are made of insulating materials, so that galvanic corrosion between the working platform and the electrode is avoided;
the device for controlling the thickness of the liquid film comprises a motor (15) with a rotor, wherein the motor (15) is arranged in a third through hole of the working platform, the rotor of the motor (15) is fixedly connected with one end of a connecting rod, the other end of the connecting rod is connected with a brush (18), the brush (18) can be driven to swing when the rotor of the motor (15) rotates, bristles of the brush sweep the upper edge of a cofferdam formed by the thin sheet (11) and can brush the excessive liquid film on the edge of a 'water pool', so that the liquid film on the working electrode (12) can be automatically adjusted and is stabilized at the thickness of the liquid film corresponding to the thickness of the corresponding thin sheet (11); the brush (18) is made of insulating material;
two conductive platinum sheets (20) are respectively attached to the sides of a 'water pool', a disconnected conductive terminal is formed on the bank side of the 'water pool', a metal lead (23) is used for connecting a motor (15), a power supply (22), a brush (18) and the two conductive platinum sheets (20) to form a circuit, when the 'water pool' is full with a set liquid film thickness, a current loop access state is formed, a rotor of the motor (15) starts to drive the brush (18) to work, excessive liquid films on the sides of the 'water pool' are brushed away, when the liquid films are brushed away, the liquid films between the two conductive platinum sheets (20) are brushed away, the electric connection between the two conductive platinum sheets (20) is disconnected, and therefore the liquid films on the surface of a working electrode (12) are adjusted and stabilized at the thickness corresponding to the thickness of the sheet (11), and the liquid films (18) are combined for use, and the requirement of generating controllable thickness is achieved.
2. The electrochemical testing device for metal failure under liquid film according to claim 1, characterized in that: the periphery of the threaded hole of the supporting lug plate (9) is provided with angle marking scales of 360 degrees in total, and the inclination angle of the working platform is controlled to be adjusted according to the angle marking scales so as to realize the liquid film state with gradient thickness.
3. The electrochemical testing device for metal failure under liquid film according to claim 1, characterized in that: the working electrode (12) is an array working electrode (19), metal to be measured is cut into small square column wires N multiplied by N, the side length of each small square column wire is not larger than 1mm, the small square column wires N is a natural number not smaller than 2, the small square column wires are orderly arranged according to the N multiplied by N array to form a square bundle metal array, one end face of the metal array is flush to form an array plane and used as a working face of the array working electrode (19), the end portion of each small square column wire of one end face of the metal array is connected with a lead wire, the side face of the square bundle metal array is wrapped by an insulator material and then is inlaid in a first through hole of a working platform, and the cylindrical working electrode (12) is formed.
4. The electrochemical testing device for metal failure under liquid film according to claim 1, characterized in that: the rotor of the motor (15) of the device for controlling the thickness of the liquid film is connected with the L-shaped or inverted T-shaped brush (18) through a connecting rod, and a dry battery with a positive electrode and a negative electrode or other power supplies are adopted as a power supply (22).
5. The electrochemical testing device for metal failure under liquid film according to claim 1, characterized in that: the thin sheet (11) for controlling the thickness of the liquid film is made of hydrophobic substances with contact angles not smaller than 90 degrees, and errors caused by the fact that fog flow is condensed and adhered to the working platform and then the thickness of the liquid film is controlled can be avoided.
6. The electrochemical testing device for metal failure under liquid film according to claim 1, characterized in that: the side surface of the conductive platinum sheet (20) is sealed by insulating waterproof glue, so that the conductive platinum sheet (20) and the thin sheet (11) keep a non-contact arrangement structural form, and the liquid film on the thin sheet (11) is prevented from conducting automatically.
7. The electrochemical testing device for metal failure under liquid film according to claim 1, characterized in that: the exposed end of the rotor of the motor (15) is a cross pore canal; one end of the connecting rod is provided with a pore channel, and one end of the connecting rod is inserted into the cross pore channel of the rotor and then fixedly connected by a bolt and a nut; the other end of the connecting rod is a cross-shaped pore channel; the brush handle end of the brush is a single pore channel, the brush handle end is inserted into the cross pore channel of the connecting rod and fixedly connected by a bolt and a nut to form a movement mechanism of the device for controlling the thickness of the liquid film.
8. The electrochemical testing device for metal failure under liquid film according to claim 1, characterized in that: the levelness adjusting device is arranged and consists of a series of horizontal adjusting nuts (21), the horizontal adjusting nuts (21) are arranged at the position, close to the edge, of the working platform, the inclination angle of the working platform is adjusted by screwing the nuts (17) and the horizontal adjusting nuts (21), and the working platform is adjusted to be in a horizontal state.
9. An electrochemical test method for metal failure under liquid film, which is characterized in that the electrochemical test device for metal failure under liquid film of claim 1 is used for test analysis, and comprises the following steps:
a. electrochemical test device setup:
assembling a sample table, manufacturing a working electrode, installing the prepared reference electrode and the working electrode on the sample table together, connecting the three electrodes with an electrochemical workstation through a lead, connecting the electrochemical workstation to a computer through a lead, installing data collection and processing software in a computer system, opening a cover of a salt spray box, arranging the sample table on a working box supporting plate of the spray box, fixing a working platform according to experimental requirements, and closing the cover;
b. the control spraying device starts program setting according to the environmental factors of the required humidity, and the control spraying box starts spraying according to the instruction of the control spraying device;
c. the fog flow contacts the surface of the working electrode and is gradually condensed into liquid state, when the target thickness is reached, the conduction of a loop with a rotor and a brush is observed through the transparent sealing cover, the work is started, and the liquid film starts to be stabilized at the set thickness value; according to the purpose of the experiment, the electrochemical workstation and the computer are determined to be started, and the corrosion kinetic data are recorded.
10. The electrochemical test method for metal failure under liquid film according to claim 9, wherein the high-throughput electrochemical test is performed, the number of sample stations of the electrochemical test device for metal failure under liquid film according to claim 1 is not less than 2, each sample station is used for performing the test under the condition of setting a liquid film with a constant thickness according to the experimental requirements, and then the working electrode made of the sample material arranged on each sample station is respectively connected with the electrochemical workstation and the computer, so that the aim of performing the high-throughput test on a plurality of samples under the thickness of a plurality of liquid films is fulfilled.
11. The electrochemical test method for metal failure under a liquid film according to claim 9, wherein a high-throughput electrochemical test is performed, and the liquid film on the working electrode is distributed in a gradient manner by adjusting the inclination angle of the working platform, so as to form a liquid film state with a gradient thickness; the working electrode embedded in the workbench adopts an array electrode, and the array electrode is connected with an electrochemical workstation and a computer, so that the corrosion failure process of the metal material under different liquid film thicknesses can be tested at high flux.
12. The electrochemical test method for metal failure under liquid film according to claim 11, wherein a high-flux electrochemical test is performed, an environment with a liquid film thickness capable of changing gradually in a gradient manner is constructed through the electrochemical test of the metal material under the gradient liquid film, the comparison analysis is performed with the corrosion test result under the liquid film state with a constant thickness, the local corrosion dynamics information can be obtained through the array electrode, the influence of different liquid film thicknesses on the metal material can be represented, and the purpose of high-flux high-efficiency failure evaluation on the corrosion of the metal material is achieved.
13. The method for electrochemically testing the sub-liquidus metal failure according to claim 11, wherein the average liquid film thickness on the surface of the working electrode is calculated by the following method in the process of realizing the liquid film with gradient thickness by the sample stage:
calculating by using the thickness of the liquid film on the surface of the working electrode de, wherein the inclination angle theta and delta abc of the working platform and the horizontal plane are liquid film parts, ab represents the section of the sheet, ab length is the thickness value of the sheet, length is the actual length value of the working electrode, bn represents the horizontal plane, dd and Ee are respectively the thickness of the liquid film at two ends of the working electrode de, and the average thickness of the liquid film on the surface of the working electrode de is set as H de Bd is L bd Bc is L long bc Ab thickness H ab And Dd is H Dd Ee thickness of H Ee Sample length L de Setting H ab ，θ，H Dd ，H ab ，L bd ，L de Using the formula L bc ＝H ab /(tan. Theta.) calculation of L bc From the principle of similarity of triangles H Dd ＝[H ab ×(L bc -L bd )]/L bc (ii) a For the same reason, use formula H Ee ＝[H ab ×(L bc -L bd -L de )]/L bc Calculate H Ee Thereby calculating the average surface thickness of the working electrode de as H de ＝(H Dd +H Ee )/2。
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