CN112147021B - Electrochemical testing device for dynamic process of metal passive film growth and degradation - Google Patents

Electrochemical testing device for dynamic process of metal passive film growth and degradation Download PDF

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CN112147021B
CN112147021B CN202010795971.5A CN202010795971A CN112147021B CN 112147021 B CN112147021 B CN 112147021B CN 202010795971 A CN202010795971 A CN 202010795971A CN 112147021 B CN112147021 B CN 112147021B
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disc
rod
sand
reducing
test
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CN112147021A (en
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范林
丁康康
侯健
孙明先
马力
张海兵
张彭辉
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725th Research Institute of CSIC
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/56Investigating resistance to wear or abrasion
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N17/00Investigating resistance of materials to the weather, to corrosion, or to light
    • G01N17/006Investigating resistance of materials to the weather, to corrosion, or to light of metals
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N17/00Investigating resistance of materials to the weather, to corrosion, or to light
    • G01N17/02Electrochemical measuring systems for weathering, corrosion or corrosion-protection measurement
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/02Details
    • G01N3/06Special adaptations of indicating or recording means
    • G01N3/066Special adaptations of indicating or recording means with electrical indicating or recording means
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02Details not specific for a particular testing method
    • G01N2203/022Environment of the test
    • G01N2203/023Pressure
    • G01N2203/0232High pressure
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02Details not specific for a particular testing method
    • G01N2203/022Environment of the test
    • G01N2203/0236Other environments
    • G01N2203/024Corrosive
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02Details not specific for a particular testing method
    • G01N2203/026Specifications of the specimen
    • G01N2203/0262Shape of the specimen
    • G01N2203/0278Thin specimens
    • G01N2203/0282Two dimensional, e.g. tapes, webs, sheets, strips, disks or membranes
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02Details not specific for a particular testing method
    • G01N2203/06Indicating or recording means; Sensing means
    • G01N2203/0617Electrical or magnetic indicating, recording or sensing means

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Abstract

The invention provides an electrochemical testing device for a dynamic process of metal passive film growth and degradation, and belongs to the field of material performance detection. The invention realizes the clamping of the sample and the abrasion of the passive film on the surface of the sample through the diameter changing and the rotation of the sand slice groups which are mutually overlapped, so that the test is not limited by the original size of the sample and the size change in the abrasion process in a certain range. Through the design of a supporting plate with a ball bearing structure, locking and integrated rotation actions of relative positions among the sand sheets are realized simultaneously. And single or multiple abrasion tests are realized by controlling the frequency and the duration of the rotary abrasion. And the in-situ and real-time electrochemical test of the passive film growth dynamic process is realized through a built-in electrochemical three-electrode system. The method has the advantages of simple principle and simple and convenient operation, increases the effective test area of the sample compared with the prior scratching electrode technology, and more accurately reflects the dynamic electrochemical behaviors of the abrasion and self-healing of the metal passive film in high-pressure and caustic corrosion environments or under the working condition of frequent abrasion.

Description

Electrochemical testing device for dynamic process of metal passive film growth and degradation
Technical Field
The invention belongs to the technical field of material performance detection, and particularly relates to a device for testing the corrosion electrochemistry of a material, in particular to a dynamic process of the growth and the growth of a metal passive film.
Background
The excellent corrosion resistance of metal materials such as stainless steel and titanium alloy is derived from a passive film on the surface thereof. This thin passivation film, in its intact state, provides sufficient protection of the material from corrosive agents. However, when the passivation film is damaged, the local passive state of the material is damaged, a galvanic couple is formed between the small-area active state and the large-area passive state, the electrochemical thermodynamic equilibrium is broken, and the local corrosion is aggravated. In high pressure, low oxygen deep sea environments, or other caustic corrosive media, or under frequent abrasive conditions, the self-healing behavior of the passivation film is greatly limited, which may in turn lead to more serious material failure problems. Therefore, the understanding of the dynamic process of the passive film growth and the growth on the surface of the metal material has important significance for guiding the research and the application of the material.
Therefore, a set of device for material passivation process research is designed by periiridescent and the like, a thin film deposited on glass is broken through falling of a knocking rod, and electrochemical information of a fresh section is measured. The patent CN 108593536 a designs a dynamic electrochemical corrosion and wear test device, which realizes the implementation and monitoring of electrochemical parameters and tribological performance under different working conditions (load, rotation speed, medium), but cannot realize the test under high-pressure environment. The patent CN 102288504B discloses a high-temperature high-pressure in-situ scratching and corrosive wear testing device, which realizes electrochemical research on in-situ single scratching and repeated corrosive wear of the surface of a sample under a high-temperature high-pressure environment, but the problem of dynamic sealing needs to be considered, the structure of the device is complex, and the scratching head is adopted to scratch, so that the damaged surface area of the sample is small, and the measurement precision is influenced. Fourteen et al proposed a method of evaluating the self-passivation ability of a material by an electric dipole method, which enables measurement on a relatively large area of a sample, but first of all, a cathodic potentiostatic activation treatment of the sample was performed, which is only feasible for a passivation film containing an oxide as a main component, and deposition of precipitates due to cathodic polarization on the surface of the material had a large influence on the test results.
Disclosure of Invention
The technical task of the invention is to solve the defects of the prior art, provide an electrochemical testing device for the dynamic process of metal passive film growth and growth, solve the problem of in-situ abrasion test of the material passive film in a high-pressure solution environment, overcome the problems of small scratch area and low signal-to-noise ratio of the existing scratch electrode technology, and realize the electrochemical test of the dynamic process of single or multiple abrasion of the passive film.
The technical scheme adopted by the invention for solving the technical problem is as follows:
an electrochemical testing device for a dynamic process of metal passive film growth and growth, comprising: the kettle cover, the kettle body, internal components and equipment;
the kettle cover is provided with a working electrode, a reference electrode and an auxiliary electrode to form an electrochemical three-electrode system, and the electrochemical test of a dynamic test process is realized by connecting the electrochemical three-electrode system with external electrochemical test equipment, wherein the working electrode is prepared by processing a sample;
the kettle body is internally divided into two cabin sections: the test cabin section is separated from the equipment cabin section through a guide disc;
the liquid inlet pipe and the liquid outlet pipe are connected with an external solution tank through a pump valve, so that the circulation of a test solution and the control of the pressure condition in the test cabin section are realized;
The center of the test cabin section is provided with a plurality of sand sheets which are overlapped with each other to form a cylindrical sand sheet group, the sand sheets are clamped by sand sheet supports, the upper parts of the sand sheet supports are movable joints which can enable the sand sheets to rotate freely, and when the sand sheet group rotates inwards and is reduced to the diameter of a sample, the sand sheets are tightly pressed on the surface of the sample to clamp and fix the sample;
wherein equipment cabin section upper portion sets up the rotary wear subassembly, realizes the wearing and tearing to sample surface passive film, and the rotary wear subassembly includes: reducing disk, supporting disk, bracing piece, main rotating electrical machines, vice rotating electrical machines, transfer line.
According to the scheme, preferably, a guide groove corresponding to the abrasive sheet support is formed in the guide disc, the abrasive sheet support is clamped into the guide groove, and the guide disc is fixed on the main rotating motor below the axis of the guide disc through a connecting rod;
a reducing disc is arranged below the guide disc and rotates around a connecting rod of a main rotating motor, a convex strip matched with the abrasive sheet support is arranged at the upper part of the reducing disc, a driven gear is fixed at the lower part of the reducing disc along the circumferential direction, a driving gear connected with an auxiliary rotating motor is arranged near the driven gear, the driven gear and the driving gear can be meshed with a transmission gear arranged between the driven gear and the driving gear, the transmission gear is arranged at the top end of a transmission rod, the transmission rod is a hydraulic rod, and when the transmission rod is lifted, the transmission gear is simultaneously contacted with the driving gear and the driven gear to complete the rotating action of the reducing disc; when the sand sheet group descends, the transmission gear is separated from the driving gear and the driven gear, the rotation stops, the sand sheet support slides in a guide groove of the guide disc in a reciprocating manner under the pushing of a convex strip on the upper part of the reducing disc along with the rotation of the reducing disc, and therefore the diameter of the sand sheet group is reduced;
The auxiliary rotating motor can realize forward and reverse reciprocating rotation, when the auxiliary rotating motor drives the reducing disc to rotate forward, the raised lines push the sand slice support to slide forward in the guide groove, so that the diameter of a cylinder surrounded by the sand slice group is reduced until a sample is clamped; when the auxiliary rotating motor drives the reducing disc to rotate reversely, the sand sheet support is pushed by the raised lines to slide reversely in the guide groove, so that the diameter of the cylinder formed by the sand sheet group is increased until the initial position is recovered;
a supporting disk is arranged below the variable diameter disk, the upper part of the supporting disk is of a ball bearing structure, the lower part of the supporting disk is connected with a supporting rod, and the supporting rod is a hydraulic rod, so that small-amplitude lifting actions of the supporting disk and the variable diameter disk above the supporting disk are realized; when the supporting rod is lifted, the supporting disk pushes the reducing disk to move upwards to press the sand sheet support between the reducing disk and the guide disk, so that the relative positions of the sand sheets are locked; when the supporting rod descends, the supporting disk drives the reducing disk to move downwards, and the pressed sand sheet support is loosened, so that the subsequent reducing action can be completed.
Preferably, a sealing ring is arranged between the bonding surface of the kettle cover and the kettle body to realize sealing.
The scheme is preferred, the working electrode outside is insulating sealed shell, and inside is electrically conductive core, and electrically conductive core bottom is screwed joint, adopts the cylinder sample during the test, and its top is provided with the screw hole, realizes being connected with screwing of the inside electrically conductive core of working electrode and deriving of signal of telecommunication.
According to the scheme, the kettle cover is connected with the kettle body through a tension and compression rod, the tension and compression rod is a hydraulic rod, when hydraulic oil is filled, positive pressure is formed in the rod, and the kettle cover is pushed upwards to be opened; when the hydraulic oil is pumped out, negative pressure is formed in the rod, the kettle cover is pulled down to be closed, and the tensioning effect of resisting the pressure in the kettle is realized.
Preferably, a hydraulic system and a control system are arranged at the lower part of the equipment cabin section, the hydraulic system provides power for the tension and compression rod, the transmission rod and the support rod, and the control system controls the test program by controlling the starting and stopping of the main rotating motor and the auxiliary rotating motor and the lifting action of the tension and compression rod, the transmission rod and the support rod; the control panel is arranged outside the kettle body and used for setting test programs, including the startup and shutdown of the device, and the frequency and duration of rotary abrasion.
The scheme is preferred, flexible sealing gaskets are bonded between the guide disc and the reducing disc, and waterproof sealing during small-amplitude relative telecontrol between the guide disc and the reducing disc is achieved.
The scheme is preferred, the guiding disc edge links to each other with the rotatory sealing washer of fixing on the internal wall of cauldron, realizes that the guiding disc is rotatory around the axle under main rotating electrical machines's drive, makes experimental cabin section and equipment cabin section mutual isolation simultaneously.
Preferably, the kettle cover is further provided with a bolt for further locking with the kettle body after the kettle cover is closed.
Compared with the prior art, the electrochemical testing device for the dynamic growth and degradation process of the metal passive film has the following beneficial effects:
the electrochemical test method realizes the in-situ abrasion electrochemical test of the material passivation film in a high-pressure solution environment, and realizes pressure-resistant sealing by adopting a mode of combining a hydraulic tension-compression rod, a bolt and a sealing ring;
the circulation of the test solution and the control of the pressure conditions are realized by means of an external pump valve;
the clamping of the sample and the abrasion of the passive film on the surface of the sample are realized through the diameter changing and the rotation of the sand slice groups which are mutually overlapped, so that the test is not limited by the original size of the sample and the size change in the abrasion process within a certain range;
through the design of a supporting plate with a ball bearing structure, locking and integral rotating actions of relative positions among the sand sheets are realized simultaneously;
the dry-wet separation of different cabin sections is realized by arranging the rotary sealing ring and the flexible sealing gasket. By controlling the frequency and the duration of the rotary abrasion, single or multiple abrasion tests are realized;
and the in-situ and real-time electrochemical test of the passive film growth dynamic process is realized through a built-in electrochemical three-electrode system.
The method has the advantages of simple principle and simple and convenient operation, increases the effective test area of the sample compared with the prior scratching electrode technology, and more accurately reflects the dynamic electrochemical behaviors of the abrasion and self-healing of the metal passive film in high-pressure and caustic corrosion environments or under the working condition of frequent abrasion.
Drawings
In order to more clearly describe the working principle of the electrochemical testing device for the dynamic process of metal passivation film growth and degradation, the following schematic diagram is attached for further explanation.
FIG. 1 is a schematic external view of the present invention;
FIG. 2 is a schematic cross-sectional structure of the present invention;
FIG. 3 is an exploded view of the rotary wear assembly of the present invention;
FIG. 4 is a schematic view of the rotary diameter-changing mode of the sand sheet set of the present invention.
The reference numerals in the figures denote:
1. a kettle cover, 2, a kettle body, 3, a liquid inlet pipe, 4, a control panel, 5 and a reference electrode,
6. working electrode, 7, auxiliary electrode, 8, bolt, 9, liquid outlet pipe, 10, sealing ring,
11. a tension and compression rod 12, a test cabin section 13, a sand sheet 14, a sand sheet support,
15. a guide disc 16, a rotary sealing ring 17, a reducing disc 18 and an equipment cabin section,
19. a transmission rod 20, an auxiliary rotating motor 21, a support rod 22, a main rotating motor,
23. A hydraulic system, 24, a control system, 25, a guide groove, 26, a convex strip,
27. a driving gear 28, a transmission gear 29, a flexible sealing gasket 30, a driven gear,
31. and (4) supporting the disc.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1 and 2, the electrochemical testing apparatus for a dynamic process of metal passivation film growth and degradation according to the present embodiment includes: kettle cover 1, kettle body 2 and the subassembly and the equipment of inside thereof. The kettle cover 1 is connected with the kettle body 2 through a tension and compression bar 11. The tension and compression rod 11 is a hydraulic rod, when hydraulic oil is filled, positive pressure is formed in the rod, and the kettle cover 1 is pushed upwards to be opened; when the hydraulic oil is pumped out, negative pressure is formed in the rod, the kettle cover 1 is pulled down to be closed, and the tensioning effect of resisting the pressure in the kettle is realized. And the bolt 8 on the kettle cover 1 is used for further locking with the kettle body 2 after the kettle cover 1 is closed. A sealing ring 10 is arranged between the bonding surfaces of the kettle cover 1 and the kettle body 2 to realize sealing.
The kettle cover 1 is provided with a working electrode 6, a reference electrode 5 and an auxiliary electrode 7 to form an electrochemical three-electrode system, and the electrochemical test of the dynamic test process is realized by connecting with external electrochemical test equipment. The working electrode 6 is externally provided with an insulating sealing shell, the inside is provided with a conductive core, and the bottom end of the conductive core is provided with a threaded joint. The test adopts the cylinder sample, and its top is provided with the screw hole, realizes screwing with the conductive core of working electrode 6 and leads out of the signal of telecommunication.
The kettle body 2 is externally provided with a control panel 4 for setting a test program, and the control panel mainly comprises a machine for stopping the device, the frequency and the duration of rotary abrasion and the like.
The interior of the kettle body 2 is divided into two cabin sections, including an upper test cabin section 12 and a lower equipment cabin section 18. The outer side of the kettle body 2 of the test cabin section 12 is provided with a liquid inlet pipe 3 and a liquid outlet pipe 9, the pipeline is connected with an external solution tank through a pump valve, and the circulation of the test solution and the control of the pressure condition in the test cabin section 12 are realized through the matching of the pump valve.
The center of the test cabin section 12 is provided with sand sheets 13, and the sand sheets 13 can form a cylindrical sand sheet 13 group. The sand sheet 13 is clamped by a sand sheet support 14, and the upper part of the sand sheet support 14 is a movable joint which can enable the sand sheet 13 to rotate freely. Between the test bay section 12 and the equipment bay section 18 is a guide disc 15. The edge of the guide disc 15 is connected with a rotary sealing ring 16 fixed on the inner wall of the kettle body 2, so that the guide disc 15 rotates around the shaft under the driving of a main rotating motor 22, and meanwhile, the test cabin section 12 and the equipment cabin section 18 are isolated from each other.
The upper part of the equipment cabin section 18 is provided with a rotary wear assembly which comprises a reducing disc 17, a supporting disc 31, a supporting rod 21, a main rotating motor 22, an auxiliary rotating motor 20 and a transmission rod 19, and the lower part of the equipment cabin section 18 is provided with a hydraulic system 23 and a control system 24. The hydraulic system 23 provides power for the tension and compression bar 11, the transmission bar 19 and the support bar 21. The control system controls the test program by controlling the start and stop of the main rotating motor 22 and the auxiliary rotating motor 20 and the lifting action of the tension and compression rod 11, the transmission rod 19 and the support rod 21.
Referring to fig. 3, the cylindrical abrasive sheet 13 group is formed by a plurality of abrasive sheets 13 which are overlapped with each other, and each abrasive sheet 13 is clamped by a corresponding abrasive sheet support 14 and then changed in position. The guide disc 15 is provided with a guide groove 25 corresponding to the abrasive sheet support 14, and the abrasive sheet support 14 is clamped in the guide groove 25. The guide plate 15 is fixed to a main rotating motor 22 below the axis thereof by a connecting rod. The main rotating electrical machine 22 can realize unidirectional high-speed rotation.
A reducing disc 17 is arranged below the guide disc 15, and the reducing disc 17 can rotate around a connecting rod of a main rotating motor 22. The upper part of the reducing disc 17 is provided with a convex strip 26 matched with the sand slice support 14. A driven gear 30 is fixed to the lower portion of the variable diameter disk 17 along the circumferential direction. A drive gear 27 connected to the sub-rotary electric machine 20 is provided near the driven gear 30. The driven gear 30 and the driving gear 27 may be engaged with a transmission gear 28 disposed therebetween, and the transmission gear 28 is installed at the top end of the transmission rod 19. The transmission rod 19 is a hydraulic rod, and when the transmission rod is lifted, the transmission gear 28 is simultaneously contacted with the driving gear 27 and the driven gear 30 to complete the rotation action of the reducing disc 17; when the vehicle descends, the transmission gear 28 is separated from the drive gear 27 and the driven gear 30, and the rotation is stopped. Along with the rotation of the reducing disc 17, the abrasive sheet support 14 slides in the guide groove 25 of the guide disc 15 in a reciprocating manner under the pushing of the convex strip 26 on the upper part of the reducing disc 17, so that the diameter change of the abrasive sheet 13 group is realized.
Referring to fig. 4, the sub-rotating electrical machine 20 can perform reciprocating rotation in forward and reverse directions. When the auxiliary rotating motor 20 drives the reducing disc 17 to rotate in the forward direction, the convex strips 26 push the abrasive sheet supports 14 to slide in the guide grooves 25 in the forward direction, so that the diameter of the cylinder surrounded by the abrasive sheet 13 is reduced until the sample is clamped. When the auxiliary rotating motor 20 drives the reducing disc 17 to rotate reversely, the raised strips 26 push the abrasive sheet support 14 to slide reversely in the guide grooves 25, so that the diameter of the cylinder surrounded by the abrasive sheets 13 is increased until the initial position is recovered.
A flexible sealing gasket 29 is bonded between the guide disc 15 and the reducing disc 17, and waterproof sealing is achieved between the guide disc 15 and the reducing disc 17 during small-amplitude relative telecontrol.
A support disc 31 is arranged below the reducing disc 17. The upper part of the supporting disc 31 is of a ball bearing structure, and the lower part of the supporting disc 31 is connected with the supporting rod 21. The support rod 21 is a hydraulic rod, and small-amplitude lifting motion of the support plate 31 and the reducing plate 17 above the support plate is achieved. When the supporting rod 21 rises, the supporting disk 31 pushes the reducing disk 17 to move upwards, and the sand sheet support 14 between the reducing disk 17 and the guide disk 15 is pressed tightly, so that the relative position between the sand sheets 13 is locked; when the supporting rod 21 descends, the supporting disk 17 drives the reducing disk 17 to move downwards, and the pressed abrasive sheet support 14 is loosened, so that the subsequent reducing action can be completed.
In use, the present invention is applied by coating the top and bottom surfaces of the sample with an epoxy resin to electrically isolate the two surfaces, and then screwing the sample onto the working electrode 6. The kettle cover 1 is pulled downwards to be closed by starting the pull and press rod 11, and the kettle cover 1 is locked on the kettle body 2 by the bolt 8. At this time, the sample is well dropped into the center of the cylindrical structure surrounded by the sand 13. The working electrode 6, the reference electrode 5 and the auxiliary electrode 7 are connected to an external electrochemical test device.
The test chamber section 12 is filled with a test solution prepared in advance in an external solution tank, and the test solution is circulated between the external solution tank and the test chamber section 12 through an external pump valve, and the inside of the test chamber section 12 is maintained under a desired pressure condition.
And (3) setting test programs such as the frequency, the duration and the like of the rotary wear through the control panel 4, starting the test, simultaneously starting external electrochemical test equipment, and monitoring dynamic electrochemical information in the test process.
After the test is started, the transmission rod 19 drives the transmission gear 28 to move upwards so that the transmission gear is in contact with the driving gear 27 and the driven gear 30. At this time, the sub-rotating electrical machine 20 starts the forward rotation to rotate the variable diameter disk 17 in the forward direction. The convex strip 26 on the upper part of the reducing disc 17 pushes the abrasive sheet support 14 to slide in the guide groove 25 on the guide disc 15 in the positive direction, so that the diameter of the mutually overlapped group of the abrasive sheets 13 is reduced until the diameter is reduced to the size of the diameter of the sample and is tightly pressed on the surface of the sample. The auxiliary rotating motor 20 is stopped, and the supporting rod 21 pushes the supporting disk 31 to move upwards, so that the abrasive disk seat 14 is pressed between the guide disk 15 and the reducing disk 17, and the relative position between the abrasive disks 13 is locked. The drive link 19 drops back, disengaging the drive gear 28 from the drive gear 27 and the driven gear 30. At this time, the main rotating motor 22 is started to make the guide disc 15 and the reducing disc 17 which are pressed against each other rotate together, and drive the abrasive disk 13 group pressed against the surface of the sample to rotate at a high speed around the sample, so that the passive film on the surface of the sample is abraded. When the rotary wear duration reaches a preset value, the main rotating motor 22 is stopped, the support rod 21 drives the support plate 31 to move downwards, and the clamped abrasive sheet support 14 is loosened. The transmission rod 19 moves up to bring the transmission gear 28 into contact with the driving gear 27 and the driven gear 30 again. At this time, the sub-rotary electric machine 20 starts the reverse rotation. The convex strips 26 on the upper part of the reducing disc 17 push the abrasive sheet support 14 to reversely slide in the guide grooves 25 on the guide disc 15, so that the diameter of the abrasive sheet 13 group is increased until the original position is recovered. The sub-rotating electrical machine 20 is stopped and the transmission rod 19 falls back, separating the transmission gear 28 from the driving gear 27 and the driven gear 30. Thereby completing a wear process. When a plurality of abrasion tests are carried out, the control system 24 repeats the steps according to the preset rotating abrasion frequency and time length to complete the corresponding test flow. In the process, external electrochemical test equipment records the electrochemical potential and current change conditions of the passivation film abrasion and self-healing dynamic process in situ through an electrochemical three-electrode system.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (9)

1. An electrochemical testing device for a dynamic process of metal passive film growth and degradation is characterized by comprising: the kettle cover (1), the kettle body (2) and internal components and equipment;
The kettle cover (1) is provided with a working electrode (6), a reference electrode (5) and an auxiliary electrode (7) to form an electrochemical three-electrode system, and the electrochemical three-electrode system is connected with external electrochemical test equipment to realize electrochemical test of a dynamic test process, wherein the working electrode (6) is prepared by processing a sample;
the kettle body (2) is internally divided into two cabin sections: the test cabin section (12) is arranged at the upper part, and the equipment cabin section (18) is arranged at the lower part, wherein the test cabin section (12) is separated from the equipment cabin section (18) through a guide disc (15);
wherein the outer side of the kettle body (2) of the test cabin section (12) is provided with a liquid inlet pipe (3) and a liquid outlet pipe (9), the liquid inlet pipe (3) and the liquid outlet pipe (9) are connected with an external solution tank through a pump valve, so that the circulation of a test solution and the control of the pressure condition in the test cabin section (12) are realized;
the test chamber section (12) is provided with a plurality of sand sheets (13) which are mutually overlapped to enclose a cylindrical sand sheet group, the sand sheets (13) are clamped by a sand sheet support (14), the upper part of the sand sheet support (14) is a movable joint which can enable the sand sheets (13) to freely rotate, and when the sand sheet group rotates inwards and is reduced to the diameter of a sample, the sand sheets (13) are tightly pressed on the surface of the sample to clamp and fix the sample;
Wherein equipment cabin section (18) upper portion sets up the rotatory wearing and tearing subassembly, realizes the wearing and tearing to sample surface passive film, and the rotatory wearing and tearing subassembly includes: reducing disc (17), supporting disk (31), bracing piece (21), main rotating electrical machines (22), vice rotating electrical machines (20), transfer line (19).
2. The electrochemical testing device for the metal passive film growth and degradation dynamic process according to claim 1, wherein a guide groove (25) corresponding to the abrasive disc support (14) is formed in the guide disc (15), the abrasive disc support (14) is clamped in the guide groove (25), and the guide disc (15) is fixed on the main rotating motor (22) below the axis of the guide disc (15) through a connecting rod;
a reducing disc (17) is arranged below the guide disc (15), the reducing disc (17) rotates around a connecting rod of a main rotating motor (22), a convex strip (26) matched with the abrasive sheet support (14) is arranged on the upper portion of the reducing disc (17), a driven gear (30) is fixed on the lower portion of the reducing disc (17) along the circumferential direction, a driving gear (27) connected with an auxiliary rotating motor (20) is arranged near the driven gear (30), the driven gear (30) and the driving gear (27) are meshed with a transmission gear (28) arranged between the driven gear and the driving gear, the transmission gear (28) is installed at the top end of a transmission rod (19), the transmission rod (19) is a hydraulic rod, and when the hydraulic rod rises, the transmission gear (28) is simultaneously contacted with the driving gear (27) and the driven gear (30), so that the rotating action of the reducing disc (17) is completed; when the sand sheet group descends, the transmission gear (28), the driving gear (27) and the driven gear (30) are separated, the rotation stops, the sand sheet support (14) slides in a guide groove (25) of the guide disc (15) in a reciprocating mode under the pushing of a convex strip (26) on the upper portion of the reducing disc (17) along with the rotation of the reducing disc (17), and therefore the diameter of the sand sheet group is changed;
The auxiliary rotating motor (20) can realize forward and reverse reciprocating rotation, when the auxiliary rotating motor (20) drives the reducing disc (17) to rotate in the forward direction, the convex strips (26) push the sand slice support (14) to slide in the guide groove (25) in the forward direction, so that the diameter of a cylinder surrounded by the sand slice groups is reduced until a sample is clamped; when the auxiliary rotating motor (20) drives the reducing disc (17) to rotate reversely, the raised lines (26) push the sand slice support (14) to slide reversely in the guide grooves (25), so that the diameter of the cylinder formed by the sand slice groups is increased until the initial position is recovered;
a supporting disk (31) is arranged below the reducing disk (17), the upper part of the supporting disk (31) is of a ball bearing structure, the lower part of the supporting disk (31) is connected with a supporting rod (21), and the supporting rod (21) is a hydraulic rod, so that small-amplitude lifting actions of the supporting disk (31) and the reducing disk (17) above the supporting disk are realized; when the supporting rod (21) rises, the supporting disk (31) pushes the reducing disk (17) to move upwards to press the sand sheet support (14) between the reducing disk (17) and the guide disk (15) so as to realize the locking of the relative position between the sand sheets (13); when the supporting rod (21) descends, the supporting disk (17) drives the reducing disk (17) to move downwards, and the pressed sand sheet support (14) is loosened, so that the subsequent reducing action can be completed.
3. The electrochemical testing device for the dynamic process of the metal passivation film growth and degradation as claimed in claim 1, wherein a sealing ring (10) is arranged between the bonding surfaces of the kettle cover (1) and the kettle body (2) to realize sealing.
4. The electrochemical testing device for the dynamic process of metal passivation film growth and degradation according to claim 1, wherein the working electrode (6) is externally provided with an insulating sealed shell, the inside is provided with a conductive core, the bottom end of the conductive core is provided with a threaded joint, a cylindrical sample is adopted during testing, and the top end of the cylindrical sample is provided with a threaded hole to realize screwing connection with the conductive core inside the working electrode (6) and lead out of an electric signal.
5. The electrochemical testing device for the dynamic process of metal passive film growth and degradation according to claim 1, wherein the kettle cover (1) is connected with the kettle body (2) through a tension and compression rod (11), the tension and compression rod (11) is a hydraulic rod, when hydraulic oil is filled, positive pressure is formed in the rod, and the kettle cover (1) is pushed upwards to be opened; when the hydraulic oil is pumped out, negative pressure is formed in the rod, the kettle cover (1) is pulled down to be closed, and the tensioning effect of resisting the pressure in the kettle is realized.
6. The electrochemical testing device for the dynamic process of metal passivation film growth and degradation according to claim 5, wherein a hydraulic system (23) and a control system (24) are arranged at the lower part of the equipment cabin section (18), the hydraulic system (23) provides power for the tension and compression rod (11), the transmission rod (19) and the support rod (21), and the control system controls the test program by controlling the starting and stopping of the main rotating motor (22) and the auxiliary rotating motor (20) and the lifting and lowering actions of the tension and compression rod (11), the transmission rod (19) and the support rod (21); the kettle body (2) is externally provided with a control panel (4) for setting a test program, including the startup and shutdown of the device, and the frequency and duration of rotary abrasion.
7. The electrochemical testing device for the dynamic process of metal passive film growth and degradation according to claim 1, wherein a flexible sealing gasket (29) is bonded between the guide disc (15) and the reducing disc (17) to realize waterproof sealing between the guide disc (15) and the reducing disc (17) during small-amplitude relative telecontrol.
8. The electrochemical testing device for the dynamic process of metal passivation film growth and degradation according to claim 1, characterized in that the edge of the guide disc (15) is connected with a rotary sealing ring (16) fixed on the inner wall of the kettle body (2) to realize that the guide disc (15) rotates around a shaft under the drive of a main rotating motor (22) and simultaneously isolate the test cabin section (12) and the equipment cabin section (18) from each other.
9. The electrochemical testing device for the dynamic process of metal passivation film growth and degradation according to claim 1, wherein the kettle cover (1) is further provided with a bolt (8) for further locking with the kettle body (2) after the kettle cover (1) is closed.
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