CN108519324A - three-electrode system and application thereof - Google Patents

three-electrode system and application thereof Download PDF

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CN108519324A
CN108519324A CN201810204839.5A CN201810204839A CN108519324A CN 108519324 A CN108519324 A CN 108519324A CN 201810204839 A CN201810204839 A CN 201810204839A CN 108519324 A CN108519324 A CN 108519324A
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electrode
working electrode
clamping plate
auxiliary
working
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CN108519324B (en
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徐连勇
路永新
韩永典
赵雷
荆洪阳
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Tianjin University
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    • 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
    • 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

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Abstract

The invention discloses a three-electrode system and application thereof, comprising a reference electrode, a working electrode column, an auxiliary electrode column, a working electrode stabilizing device and an electrode clamp, wherein the working electrode auxiliary stabilizing device comprises a first clamping plate, a second clamping plate, a third clamping plate and a telescopic device, the electrode clamp comprises a stabilizing disc, a lead and a metal sheet, a working electrode groove is arranged in the stabilizing disc, a working electrode sample is arranged in the working electrode groove, the stabilizing disc is connected with the metal sheet through the lead, the reference electrode is fixed between the first clamping plate and the second clamping plate, the stabilizing disc of the electrode clamp is fixed between the second clamping plate and the third clamping plate, the metal sheet is connected with the working electrode through a metal groove inserted below the working electrode column, and a platinum sheet electrode is arranged in the metal groove below the auxiliary electrode column. The device is applied to an electrochemical testing device and is used for researching dynamic high-temperature high-pressure corrosion behaviors and mechanisms.

Description

Three-electrode system and its application
The present patent application is the division of parent application " high temperature and pressure dynamic electro-chemical test experimental provision and test method " Application, parent application application No. is 2016103221363, the applying date is on May 16th, 2016.
Technical field
The present invention relates to electro-chemical test experimental provision, especially high temperature and pressure dynamic electro-chemical test experimental provisions and survey Method for testing.
Background technology
Occur to destroy or go bad caused by chemistry or electrochemical action between metal material and ambient enviroment (medium) to claim For corrosion, metal erosion spreads the every field of industrial and agricultural production and national defense construction, and harm is very serious.And high temperature pressure corrosion It is a kind of to lead to a kind of phenomenon of material failure because electrochemical corrosion acts on.Such as during oil and gas development, in associated gas Often contain H2S and CO2, various pipelines or structure is caused to fail in the form of high temperature pressure corrosion.Carry out high temperature pressure corrosion process Simulated experiment is defeated oil/gas material screening and evaluation, the screening of sustained release agent and evaluation and research material corrosion resistance and etching machine The important means of reason.But due under high-temperature and high-pressure conditions, to working electrode, reference electrode and the isostructural resistance to height of auxiliary electrode Mild high voltage performance has very high requirement, is not easy to realize the output of electrochemical signals.Meanwhile related forming currently on the market The price of product is all higher, affects the extensive research to high temperature pressure corrosion behavior and mechanism.
Invention content
The present invention overcomes the disadvantages of the prior art, provides high temperature and pressure dynamic electro-chemical test experimental provision and surveys Method for testing.The device is suitable for high temperature pressure corrosion medium under the conditions of dynamic operation condition, to metallic material corrosion electrochemical in-situ Signal is detected, and to carry out the behavior of high temperature and pressure Dynamic Corrosion and mechanism study, solving in the past cannot be to simulated solution The problem of electrochemical signals measurement is carried out under high-temperature and high-pressure conditions.
In order to solve the above-mentioned technical problem, the present invention is achieved by the following technical solutions:
High temperature and pressure dynamic electrochemical testing device, including high-temperature high-pressure reaction kettle, three-electrode system, external control cabinet, External air supply system, external electrochemical workstation and computer;
High-temperature high-pressure reaction kettle include autoclave body, high pressure kettle cover, air inlet pipe, escape pipe, rotation axis, pressure sensor, Pressure gauge, temperature sensor, heating device and heat preservation heat insulation layer, autoclave body is cylindrical container, in the outside of autoclave body Heating device is set, thermal insulating warm-keeping layer is set in the outside of heating device, high pressure kettle cover is set in the upper surface of autoclave body, tightly Fixing bolt passes through fixed mounting hole, is connected with autoclave body interconnecting piece, so that kettle cover is tightened to an entirety with autoclave body, and realizes It seals, is diametrically disposed on high pressure kettle cover circular surface:Air inlet pipe hole, temperature sensor hole, working electrode hole, Rotational axis hole, charging aperture, pressure sensor hole and outlet pore, wherein rotational axis hole are located at circle centre position, are arranged in rotational axis hole Rotation axis, rotation axis connection control motor, and rotation axis top half is located on high pressure kettle cover, and rotation axis lower half portion is located at height It presses in autoclave body, the lower end of rotation axis is provided with mixing component, is respectively arranged with above and below working electrode hole is adjacent Auxiliary electrode hole and reference electrode hole, are provided with working electrode column on working electrode hole, and auxiliary is arranged on auxiliary electrode hole Reference electrode is arranged on reference electrode hole, air inlet pipe is arranged in air inlet pipe hole, outlet is arranged in outlet pore for electrode column Pipe, setting charging auxiliary device, pressure sensor and pressure gauge are provided on pressure sensor hole on charging aperture;
In the above-mentioned technical solutions, the lower half portion length in autoclave body that is located at of the rotation axis accounts for autoclave body height , the mixing component is agitating paddle or stirring disk;
In the above-mentioned technical solutions, the air inlet pipe gos deep into the bottom of autoclave body, and escape pipe is located in autoclave body It is more than liquid surface;
In the above-mentioned technical solutions, temperature sensor is connected with temperature controller, and temperature controller is connected with heating device;
In above-mentioned technical proposal, when three electrodes is arranged in three electrode holes, electrode is with the structure at high pressure kettle cover sealing, Setting of casing, upper casing and plug are set gradually from bottom to top;
Three-electrode system includes reference electrode, working electrode column, auxiliary electrode column, working electrode stabilising arrangement and electrode Folder, wherein reference electrode are an integral structure Ag/AgCl electrodes, and working electrode column and auxiliary electrode column have identical structure, i.e., Cylindrical structure is arranged metallic channel directed downwardly in the lower section of cylinder, sheet metal is arranged in metallic channel, along cylindrical center's setting The bottom end of portion's conducting wire, inner lead is in contact with the sheet metal in metallic channel, the side setting fastening spiral shell button in the position that is in contact, Fasten the connection that spiral shell button is used for fixing internal conducting wire and sheet metal;In order to make working electrode and reference in autoclave body under stirring Stabilizing distance is kept, therefore working electrode auxiliary stabilizing device is set, which includes first clamping plate, second clamping plate and third clamping plate And telescopic device, telescopic device connect into an entirety across three pieces of clamping plates, first clamping plate and third clamping plate can be along telescopic devices It carries out, close to the activity with separate second clamping plate, secure component (not marking in figure) being arranged in first clamping plate and third clamping plate, For strap and telescopic device, electrode holder includes stable disk, conducting wire and sheet metal, and working electrode groove is arranged in stable disk, Working electrode sample is set in working electrode groove, and stable disk is connected by conducting wire with sheet metal, and reference electrode is fixed on the first folder Between plate and second clamping plate, the stable disk of electrode holder is fixed between second clamping plate and third clamping plate, keeps working electrode sample flat It is hollow structure between clamping plate facing towards reference electrode, makes to be full of experimental solutions between working electrode sample and reference electrode, gold Belong to piece and be connected with working electrode by being inserted into the metallic channel below working electrode column, is set in the lower-lying metal slot of auxiliary electrode column Set platinum plate electrode;
In the above-mentioned technical solutions, the working electrode is the test button of epoxy encapsulation,
In the above-mentioned technical solutions, the auxiliary electrode is the platinum plate electrode of 13 × 10 × 0.2mm, unilateral exposed surface Product is 10 × 10mm,
In the above-mentioned technical solutions, the working electrode surface is away from reference electrode 2-5mm;
In the above-mentioned technical solutions, the working electrode auxiliary stabilizing device and electrode holder are maximum temperature 260 DEG C, maximum pressure is the polytetrafluoroethylene (PTFE) of 10Mpa;
In the above-mentioned technical solutions, the reference electrode is 310 DEG C of maximum temperature, and maximum pressure is the high temperature of 10Mpa High pressure Ag/AgCl electrodes;
External control cabinet is connected with heating and heat-insulating device and rotation axis, and heating and thermal insulation dress can be adjusted by external control cabinet The rotating speed of the temperature and rotation axis set;
External air supply system is connected with the air inlet pipe of device, for providing corrosive gas;
External electrochemical workstation is connected with the terminals of auxiliary electrode, reference electrode and working electrode, auxiliary for acquiring The electrochemical signals of electrode, reference electrode and working electrode, computer are helped to be connected with external electrochemical workstation, for external The data of electrochemical workstation acquisition are recorded, analyzing processing and output.
The test method of high temperature and pressure dynamic electrochemical testing device is as follows:
Step 1, corrosive liquid is packed into autoclave body by charging auxiliary device and charging aperture, and covers high pressure kettle cover and gives With fixation;
Step 2, it is passed through inert gas in the corrosive liquid by air inlet pipe into autoclave body, to remove in autoclave body Oxygen;
In step 2, inert gas is nitrogen, helium or argon gas;
In step 2, the time for being passed through inert gas is 12-24 hours, preferably 15-20 hours;
Step 3, it is passed through experimental gas in the corrosive liquid by air inlet pipe into autoclave body, so that experimental gas is filled in Autoclave body inner space;
In step 3, the time for being passed through experimental gas is 22-24 hours, experimental gas CO2Or H2S gases;
Step 4, heating and heat-insulating device is started by external control cabinet, autoclave internal corrosion liquid is heated to setting experiment temperature It spends and keeps the temperature, adjusting control case changes rotation rotating speed, reaches preset rotation speed;
Step 5, external electrochemical workstation is connected with working electrode, auxiliary electrode and reference electrode respectively, and receives letter Number, proceed by experiment test.
In actual use, pressure setting, during excluding oxygen, high pressure are carried out by pressure sensor and pressure gauge When pressure reaches preset value in kettle, it can generally assert that oxygroup originally drains;Similarly, when pressure reaches preset value in autoclave, one As can assert that experimental gas has been filled with space in autoclave.
Compared with prior art, the beneficial effects of the invention are as follows:Using high temperature and pressure Ag/AgCl reference electrodes, reach The requirement of test environment leakproofness and heat-resisting quantity, while also ensuring the accuracy of test result, it is assisted using working electrode Stabilising arrangement makes working electrode keep relative distance to fix with reference electrode, and autoclave body meets the requirement of leakproofness and heat-resisting quantity, The device provides the test environments of high temperature and pressure can be used for dynamic high temperature high pressure corrosion behavior and mechanism study.
Description of the drawings
Fig. 1 is the autoclave superstructure schematic diagram of the present invention.
Fig. 2 is the whole kettle side structure schematic view of A-A sections in Fig. 1.
Fig. 3 is that autoclave covers component connection sealing means schematic diagram.
Fig. 4 is working electrode column/reference electrode rod structure schematic diagram.
Fig. 5 is electrode holder structural schematic diagram.
Fig. 6 is working electrode auxiliary stabilizing device overlooking structure diagram.
Fig. 7 is working electrode auxiliary stabilizing device side structure schematic view.
Fig. 8 is temperature 60 C, CO2Divide 0.03Mpa, under 0m/s and 0.3m/s rotating speeds, the electrochemical corrosion of carbon steel A106B Polarization curve.
Fig. 9 is 90 DEG C of temperature, CO2Divide 0.1Mpa, under 0m/s and 0.3m/s rotating speeds, the electrochemical corrosion of carbon steel A106B Polarization curve.
Figure 10 is 90 DEG C of temperature, CO2Divide 0.2Mpa, under 0m/s and 0.5m/s rotating speeds, the electrochemical corrosion of carbon steel A106B Polarization curve.
Figure 11 is 90 DEG C of temperature, CO2Divide 0.5Mpa, under 0m/s and 1m/s rotating speeds, the electrochemical corrosion pole of carbon steel A106B Change curve.
In 1-7:1 is autoclave body, and 2 be heating device, and 3 be heat preservation heat insulation layer, and 4 be nut, and 5 be mixing component, and 6 are Escape pipe, 7 be pressure sensor, and 8 be pressure gauge, and 9 be charge door, and 10 be rotation axis, and 11 be auxiliary electrode column, and 12 be reference electricity Pole, 13 be working electrode column, and 14 be temperature sensor, and 15 be air inlet pipe, and 16 be fastening bolt, and 17 be high pressure kettle cover, and 18 be work Make electrode, 19 be auxiliary electrode, and 20 be autoclave outer wall, and 21 be outlet pore, and 22 be pressure sensor hole, and 23 be charging aperture, 24 be rotational axis hole, and 25 be auxiliary electrode hole, and 26 be working electrode hole, and 27 be temperature sensor hole, and 28 be air inlet pipe hole, 29 It is inner lead for reference electrode hole, 30,31 be plug, and 32 be upper casing, and 33 be setting of casing, and 34 be fastening spiral shell button, and 35 be gold Belong to slot, 36 be stable disk, and 37 be working electrode groove, and 38 be conducting wire, and 39 be sheet metal, and 40 be first clamping plate, and 41 be the second folder Plate, 42 be third clamping plate, and 43 be telescopic device, and 44 be fixed mounting hole, and 45 motors in order to control, 46 be autoclave body interconnecting piece.
In 8-11,1 is static lower test, and 2 indicate the lower test of dynamic.
Specific implementation mode
Present invention is further described in detail with specific embodiment below in conjunction with the accompanying drawings:
High temperature and pressure dynamic electrochemical testing device, including high-temperature high-pressure reaction kettle, three-electrode system, external control cabinet, External air supply system, external electrochemical workstation and computer;
High-temperature high-pressure reaction kettle include autoclave body, high pressure kettle cover, air inlet pipe, escape pipe, rotation axis, pressure sensor, Pressure gauge, temperature sensor, heating device and heat preservation heat insulation layer, autoclave body is cylindrical container, in the outside of autoclave body Heating device is set, thermal insulating warm-keeping layer is set in the outside of heating device, high pressure kettle cover is set in the upper surface of autoclave body, tightly Fixing bolt passes through fixed mounting hole, is connected with autoclave body interconnecting piece, so that kettle cover is tightened to an entirety with autoclave body, and realizes It seals, is diametrically disposed on high pressure kettle cover circular surface:Air inlet pipe hole, temperature sensor hole, working electrode hole, Rotational axis hole, charging aperture, pressure sensor hole and outlet pore, wherein rotational axis hole are located at circle centre position, are arranged in rotational axis hole Rotation axis, rotation axis connection control motor, and rotation axis top half is located on high pressure kettle cover, and rotation axis lower half portion is located at height It presses in autoclave body, the lower end of rotation axis is provided with mixing component, is respectively arranged with above and below working electrode hole is adjacent Auxiliary electrode hole and reference electrode hole, are provided with working electrode column on working electrode hole, and auxiliary is arranged on auxiliary electrode hole Reference electrode is arranged on reference electrode hole, air inlet pipe is arranged in air inlet pipe hole, outlet is arranged in outlet pore for electrode column Pipe, setting charging auxiliary device, pressure sensor and pressure gauge are provided on pressure sensor hole on charging aperture;
In the above-mentioned technical solutions, the lower half portion length in autoclave body that is located at of the rotation axis accounts for autoclave body height , the mixing component is agitating paddle or stirring disk;
In the above-mentioned technical solutions, the air inlet pipe gos deep into the bottom of autoclave body, and escape pipe is located in autoclave body It is more than liquid surface;
In the above-mentioned technical solutions, temperature sensor is connected with temperature controller, and temperature controller is connected with heating device;
In above-mentioned technical proposal, when three electrodes is arranged in three electrode holes, electrode is with the structure at high pressure kettle cover sealing, Setting of casing, upper casing and plug are set gradually from bottom to top;
Three-electrode system includes reference electrode, working electrode column, auxiliary electrode column, working electrode stabilising arrangement and electrode Folder, wherein reference electrode are an integral structure Ag/AgCl electrodes, and working electrode column and auxiliary electrode column have identical structure, i.e., Cylindrical structure is arranged metallic channel directed downwardly in the lower section of cylinder, sheet metal is arranged in metallic channel, along cylindrical center's setting The bottom end of portion's conducting wire, inner lead is in contact with the sheet metal in metallic channel, the side setting fastening spiral shell button in the position that is in contact, Fasten the connection that spiral shell button is used for fixing internal conducting wire and sheet metal;In order to make working electrode and reference in autoclave body under stirring Stabilizing distance is kept, therefore working electrode auxiliary stabilizing device is set, which includes first clamping plate, second clamping plate and third clamping plate And telescopic device, telescopic device connect into an entirety across three pieces of clamping plates, first clamping plate and third clamping plate can be along telescopic devices It carries out, close to the activity with separate second clamping plate, secure component (not marking in figure) being arranged in first clamping plate and third clamping plate, For strap and telescopic device, electrode holder includes stable disk, conducting wire and sheet metal, and working electrode groove is arranged in stable disk, Working electrode sample is set in working electrode groove, and stable disk is connected by conducting wire with sheet metal, and reference electrode is fixed on the first folder Between plate and second clamping plate, the stable disk of electrode holder is fixed between second clamping plate and third clamping plate, keeps working electrode sample flat It is hollow structure between clamping plate facing towards reference electrode, makes to be full of experimental solutions between working electrode sample and reference electrode, gold Belong to piece and be connected with working electrode by being inserted into the metallic channel below working electrode column, is set in the lower-lying metal slot of auxiliary electrode column Set platinum plate electrode;
In the above-mentioned technical solutions, the working electrode is the test button of epoxy encapsulation,
In the above-mentioned technical solutions, the auxiliary electrode is the platinum plate electrode of 13 × 10 × 0.2mm, unilateral exposed surface Product is 10 × 10mm,
In the above-mentioned technical solutions, the working electrode surface is away from reference electrode 2-5mm;
In the above-mentioned technical solutions, the working electrode auxiliary stabilizing device and electrode holder are maximum temperature 260 DEG C, maximum pressure is the polytetrafluoroethylene (PTFE) of 10Mpa;
In the above-mentioned technical solutions, the reference electrode is 310 DEG C of maximum temperature, and maximum pressure is the high temperature of 10Mpa High pressure Ag/AgCl electrodes;
External control cabinet is connected with heating and heat-insulating device and rotation axis, and heating and thermal insulation dress can be adjusted by external control cabinet The rotating speed of the temperature and rotation axis set;
External air supply system is connected with the air inlet pipe of device, for providing corrosive gas;
External electrochemical workstation is connected with the terminals of auxiliary electrode, reference electrode and working electrode, auxiliary for acquiring The electrochemical signals of electrode, reference electrode and working electrode, computer are helped to be connected with external electrochemical workstation, for external The data of electrochemical workstation acquisition are recorded, analyzing processing and output.
The test method of high temperature and pressure dynamic electrochemical testing device is as follows:
Step 1, corrosive liquid is packed into autoclave body by charging auxiliary device and charging aperture, and covers high pressure kettle cover and gives With fixation;
Step 2, it is passed through inert gas in the corrosive liquid by air inlet pipe into autoclave body, to remove in autoclave body Oxygen;
In step 2, inert gas is nitrogen, helium or argon gas;
In step 2, the time for being passed through inert gas is 12-24 hours, preferably 15-20 hours;
Step 3, it is passed through experimental gas in the corrosive liquid by air inlet pipe into autoclave body, so that experimental gas is filled in Autoclave body inner space;
In step 3, the time for being passed through experimental gas is 22-24 hours, experimental gas CO2Or H2S gases;
Step 4, heating and heat-insulating device is started by external control cabinet, autoclave internal corrosion liquid is heated to setting experiment temperature It spends and keeps the temperature, adjusting control case changes rotation rotating speed, reaches preset rotation speed;
Step 5, external electrochemical workstation is connected with working electrode, auxiliary electrode and reference electrode respectively, and receives letter Number, proceed by experiment test.
In actual use, pressure setting, during excluding oxygen, high pressure are carried out by pressure sensor and pressure gauge When pressure reaches preset value in kettle, it can generally assert that oxygroup originally drains;Similarly, when pressure reaches preset value in autoclave, one As can assert that experimental gas has been filled with space in autoclave.
With the present apparatus under different rotating speeds, temperature and air pressure conditions to the electrochemical corrosion polarization curve of carbon steel A106B into Row test, sample impregnates before testing continues 1 hour in the solution, until specimen surface system reaches dynamic stability, test result As shown below.1 indicates static lower test in figure, and 2 indicate the lower test of dynamic.Fig. 8 is temperature 60 C, CO20.03Mpa is divided, Polarization curve under 0m/s and 0.3m/s rotating speeds.Due to CO2Relatively low and Acclimation temperature is divided, the anode of polarization curve is propped up with activity Based on dissolving.Meanwhile rotating speed reduces polarization curve cathode in such a way that diffusion polarization controls.Fig. 9 is 90 DEG C of temperature, CO2Point Press 0.1Mpa, the polarization curve under 0m/s and 0.3m/s rotating speeds.Due to CO2The raising of partial pressure, the anode branch and Fig. 8 of polarization curve It compares, slight deactivation phenomenon occurs, this is because raising and the CO of temperature2The raising of partial pressure accelerates specimen surface corrosive film Formation, it can be seen that the passivation phenomenon of the lower specimen surface of static state becomes apparent from.The raising and dynamic test of temperature are so that polarization is bent Line cathode is no longer carried out with polarization curve cathode.Figure 10 is 90 DEG C of temperature, and CO2 divides 0.2Mpa, under 0m/s and 0.5m/s rotating speeds Polarization curve.Test result and Fig. 9 are close under this condition, are that anode surface slight deactivation occurs, cathode turns to electrochemistry Polarizing control.Figure 11 is 90 DEG C of temperature, CO2Divide 0.5Mpa, the polarization curve under 0m/s and 1m/s rotating speeds.Due to CO2Partial pressure carries Height, anode branch passivation phenomenon is apparent, and cathode is carried out with activation polarization control mode.
It describes the invention in detail, but content is only the preferred embodiment of the present invention, cannot be recognized above For the practical range for limiting the present invention.Any changes and modifications in accordance with the scope of the present application should all still return Belong within the patent covering scope of the present invention.

Claims (6)

1. three-electrode system, which is characterized in that stablize dress including reference electrode, working electrode column, auxiliary electrode column, working electrode It sets and electrode holder, wherein reference electrode is an integral structure Ag/AgCl electrodes, working electrode column and auxiliary electrode column have identical Structure, i.e. cylindrical structure are arranged metallic channel directed downwardly in the lower section of cylinder, sheet metal are arranged in metallic channel, along cylinder Inner lead is arranged in the heart, and the bottom end of inner lead is in contact with the sheet metal in metallic channel, is arranged in the side for the position that is in contact Spiral shell button is fastened, the connection of fixing internal conducting wire and sheet metal is used for;Working electrode auxiliary stabilizing device, for make working electrode with Reference keeps stabilizing distance under stirring;The device includes first clamping plate, second clamping plate and third clamping plate and telescopic device, Telescopic device connects into an entirety across three pieces of clamping plates, first clamping plate and third clamping plate can be carried out along telescopic device it is close with it is remote Secure component is arranged in first clamping plate and third clamping plate in activity from second clamping plate, is used for strap and telescopic device;Electricity Pole folder includes stable disk, conducting wire and sheet metal, and working electrode groove is arranged in stable disk, and setting working electrode tries in working electrode groove Sample, stable disk are connected by conducting wire with sheet metal, and reference electrode is fixed between first clamping plate and second clamping plate, electrode holder it is steady Price fixing is fixed between second clamping plate and third clamping plate, makes working electrode sample plane towards reference electrode, in being between clamping plate Hollow structure makes to be full of experimental solutions between working electrode sample and reference electrode, and sheet metal is by being inserted into below working electrode column Metallic channel be connected with working electrode, platinum plate electrode is set in the lower-lying metal slot of auxiliary electrode column.
2. three-electrode system according to claim 1, which is characterized in that the auxiliary electrode is 13 × 10 × 0.2mm Platinum plate electrode, unilateral bare area be 10 × 10mm.
3. three-electrode system according to claim 1, which is characterized in that the reference electrode is 310 DEG C of maximum temperature, Maximum pressure is the high temperature and pressure Ag/AgCl electrodes of 10Mpa.
4. three-electrode system according to claim 1, which is characterized in that the working electrode auxiliary stabilizing device and electricity Pole folder is 260 DEG C of maximum temperature, and maximum pressure is the polytetrafluoroethylene (PTFE) of 10Mpa.
5. three-electrode system according to claim 1, which is characterized in that the working electrode surface is away from reference electrode 2- 5mm。
6. application of the three-electrode system as described in one of claim 1-5 in electrochemical testing device, which is characterized in that In the test of dynamic high temperature high pressure corrosion behavior, working electrode is set to be kept with reference electrode using working electrode auxiliary stabilizing device Relative distance is fixed.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101074487A (en) * 2007-03-29 2007-11-21 上海交通大学 Electrochemical experimental device
CN101865816A (en) * 2010-05-28 2010-10-20 北京科技大学 Experimental apparatus for high-temperature high-pressure loop spray corrosion simulation and electrochemical testing
CN104075987A (en) * 2014-07-22 2014-10-01 华北电力大学(保定) Electrochemistry test probe
CN204536262U (en) * 2015-03-09 2015-08-05 扬州工业职业技术学院 A kind of electrolytic cell three-electrode system position adjustable spiral clamp device
CN105115887A (en) * 2015-09-08 2015-12-02 中国科学院海洋研究所 Metal material corrosion testing device and method under high-pressure densely-compacted bentonite environment
CN205139078U (en) * 2015-11-20 2016-04-06 山西大同大学 Three electrode system fixing device with adjustable

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08102402A (en) * 1994-09-30 1996-04-16 Matsushita Electric Ind Co Ltd Resistor and manufacture method thereof
CN2475033Y (en) * 2001-02-26 2002-01-30 中国科学院海洋研究所 Electrolytic cell
CN1304834C (en) * 2005-03-25 2007-03-14 北京科技大学 Dynamic high-temperature and pressure electro-chemical measurement experimental device
RU2346267C1 (en) * 2007-05-07 2009-02-10 Инновационный технический центр Общество с ограниченной ответственностью "СИТИС" Method of determining electronic work function in vacuum (versions)
CN101349672A (en) * 2008-09-12 2009-01-21 福州大学 Microflow control chip electrochemical detection device capable of accurately controlling electrode distance
CN202471565U (en) * 2012-03-14 2012-10-03 东北石油大学 High temperature and high pressure H2S/CO2 corrosion reaction device capable of realizing dynamic electrochemical test
CN202814909U (en) * 2012-10-29 2013-03-20 黑龙江八一农垦大学 Inter-electrode distance adjustable electrolytic bath
CN102944593A (en) * 2012-11-05 2013-02-27 上海大学 Miniature regulated electrolysis device
CN103411879B (en) * 2013-07-18 2015-04-29 北京科技大学 High temperature and high pressure dynamic electrochemical test and pH in situ monitoring experimental device
CN204086201U (en) * 2014-07-04 2015-01-07 中国检验检疫科学研究院 A kind of clipping three electrode assemblies for micro-example Electrochemical Detection
CN205679515U (en) * 2016-05-16 2016-11-09 天津大学 HTHP dynamic electric test chemical experimental provision

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101074487A (en) * 2007-03-29 2007-11-21 上海交通大学 Electrochemical experimental device
CN101865816A (en) * 2010-05-28 2010-10-20 北京科技大学 Experimental apparatus for high-temperature high-pressure loop spray corrosion simulation and electrochemical testing
CN104075987A (en) * 2014-07-22 2014-10-01 华北电力大学(保定) Electrochemistry test probe
CN204536262U (en) * 2015-03-09 2015-08-05 扬州工业职业技术学院 A kind of electrolytic cell three-electrode system position adjustable spiral clamp device
CN105115887A (en) * 2015-09-08 2015-12-02 中国科学院海洋研究所 Metal material corrosion testing device and method under high-pressure densely-compacted bentonite environment
CN205139078U (en) * 2015-11-20 2016-04-06 山西大同大学 Three electrode system fixing device with adjustable

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