CN106124583B - A kind of reference electrode protection structure of rotary erosion abrasion dynamic electrochemical test system - Google Patents
A kind of reference electrode protection structure of rotary erosion abrasion dynamic electrochemical test system Download PDFInfo
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- CN106124583B CN106124583B CN201610684729.4A CN201610684729A CN106124583B CN 106124583 B CN106124583 B CN 106124583B CN 201610684729 A CN201610684729 A CN 201610684729A CN 106124583 B CN106124583 B CN 106124583B
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- reference electrode
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- contact conductor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/301—Reference electrodes
Abstract
The reference electrode that dynamic electrochemical test system is worn the present invention provides a kind of rotary erosion protects structure, and it includes reference electrode, contact conductor sleeve, preceding protective shell and rear protective shell that the reference electrode, which protects structure mainly,；The reference electrode includes calomel electrode and salt bridge, and salt bridge is made of the saturation potassium chloride and agar mixture filled in Luggin capillary, and calomel electrode and salt bridge form reference electrode.The reference electrode is among preceding protective shell and rear protective shell, and by being connected to potentiostat after the extraction of contact conductor sleeve, the upper end of contact conductor sleeve is fixed on slurry tank cover board the conducting wire of reference electrode.Working electrode, auxiliary electrode and the reference electrode of the present invention is arranged in slurry liquid, can be reflected the electrochemical characteristic during erosive wear in real time, be ensured the authenticity of measurement result；Reduce the attachment device that reference electrode is arranged outside slurry tank simultaneously, simple in structure, operation facility, testing efficiency height.
Description
Technical field：
The invention belongs to electro-chemical test component fields, are surveyed more particularly to a kind of rotary erosion abrasion dynamic electrochemistry
The reference electrode of test system protects structure.
Background technology：
With the continuous development of Electrochemical Measurement Technology, Electrochemical Measurement Technology has become research material corrosion field
A kind of important characterization method, common corrosion electrochemistry research method have polarization curve analytic approach, polarisation resistance method, electrochemistry resistance
Anti- spectrometry and electrochemistry noise etc..Electrochemical test method needs three-electrode system i.e. working electrode, auxiliary electrode and reference
Electrode, three electrodes are put into the electrolytic cell for filling tested media（Generally glass material）In, it is wired to potentiostat.
Tested material is working electrode, opposite with working electrode for auxiliary electrode, working electrode and the polarization electricity of auxiliary electrode group
Road；Common reference electrode has saturated calomel electrode, silver-silver chloride electrode and standard hydrogen electrode etc., reference electrode and work electricity
Pole forms measuring loop, and electric current flows to auxiliary electrode from working electrode, and independent reference electrode only provides reference and no current is logical
It crosses.It is usually glass tube outside auxiliary electrode and reference electrode, is usually used in electrochemistry when tested sample and medium are static
Corrosion test, it is difficult to directly apply to the electrochemical corrosion test under tested sample and/or medium dynamic.
Liquid fixed double phase flow erosive wear phenomenon is prevalent in the industries such as metallurgy, chemical industry, mining, water conservancy and hydropower, is to lead
Cause the major reason of the flow passage components Rapid Damage such as various pipelines, transh pump, valve.During liquid fixed double phase flow erosive wear,
The erosive wear effect of the existing fluid of damage of workpiece, also has the corrosiveness of medium, while also having the reciprocation of the two, has
When reciprocation caused by material bleed rate it is also bigger than pure corrosion and the sum of pure erosive wear, the extent of injury is than pure corrosion
Or pure erosive wear bigger, reciprocation include that erosive wear makees the promotion of erosive wear the facilitation of corrosion and corrosion
With (dynamic during erosive wear）The etching extent of material than it is static when it is much greater.Therefore, how by Electrochemical Measurement Technology
Applied to rotary erosion abrasion test device, into Mobile state on-line testing, accurate characterization punching during erosion resistance tests
The etching extent in wear process is lost, for research material Erosion Wear Mechanisms, controls erosive wear process material bleed rate, if
Suitable wear-resisting erosion resistance material is counted, extending flow passage components service life has important theory and practical directive significance.
In order to solve simple glass matter reference electrode can not directly be placed in slurry tank carry out rotary erosion wore
Reference electrode is placed in the beaker of slurry external container by the problem of journey electro-chemical test, some researchers, by communicating pipe with
Slurry liquid unicom, this system operatio is more complex, and glass beaker need to be fixed carefully, is frangible.Although some researchers are by three electrodes
System is both mounted in slurry liquid, but sample is in rotation status mostly, complicated.China Patent No. CN
201010603782.X（It is entitled《A kind of rotary experimental device of simulation inner wall of the pipe erosion corrosion》Disclose three electrode systems
System is both mounted in slurry liquid, auxiliary electrode（To electrode）And calomel electrode（Reference electrode）It is disposed adjacent to the interior of slurry tank
At wall, rotation axis is placed in slurry tank central part, is designed with adapter in the middle part of rotation axis, adapter both ends are connected with specimen holder
Tool, lower part have agitator arm, rotation axis to drive specimen holder（Tray sample）, ring specimen and agitator arm revolve in slurry tank
Transhipment is dynamic, carries out slurry erosion resistance tests, and ring specimen carries out telecommunications by copper ball, spring, stainless steel bar, copper ring-carbon brush
Number output, be connected to together with auxiliary electrode and calomel electrode in electro-chemical test equipment carry out electrochemistry monitor in real time；This side
Method has been concentrated the advantages of existing rotary and fluid-guiding type erosion-corrosion experiment device, but specimen holder（Tray sample）, annular examination
Sample and agitator arm one act as high-speed motion, complicated, easily break down.As China Patent No. CN200820153330.4,
It is entitled《Electrochemical behavior test device in dynamic fluid medium》It is tested not to solve the Electrochemistry Information in dynamic fluid
Accurate problem, by that will work, and assist, reference these three electrode positions will fix, flow velocity probe are arranged, and allow them with electrode one
Play rotation, working electrode, auxiliary electrode, three electrode of reference electrode and measurement of rate of flow probe and electric machine rotational axis in the device
Synchronized rotation, the protection of the reliability and electrode of rotating mechanism are relatively difficult together.For another example China Patent No.
It is CN201410035397.8, entitled《A kind of dynamic electrochemical testing device and attaching method thereof》Disclose three electrode systems
System is mounted on using integration mode in sample holder disk, and wherein auxiliary electrode is cyclic annular platinum filament, is positioned over apart from working electrode about
In the annular groove of 10mm, working electrode connect reference electrode placement with auxiliary electrode by line slot with the conducting wire in transmission shaft
In in the strip groove of clamping disk, end is connected apart from working electrode about 1-2mm, the other end by the conducting wire in hollow drive shaft
It is connected to Dynamic link library pond.Three-electrode system is connect by Dynamic link library pond with three electrode connection plates, and last electrochemical signals transmit
To potentiostat；The device is mounted in sample holder disk using integration mode by three electrodes, Dynamic link library pool capacity device is arranged
With the structures such as three electrode cables are drawn in hollow drive shaft, since container is rotated together with transmission shaft during experiment, acusector begin
It keeps good with extraction ring eventually to contact, realizes the reliable and stable transmission of electrochemical signals of sample to be tested during experiment, really
Reflect the electrochemical corrosion situation and Abrasion properties of sample to be tested during testing.But whole system complexity, each part requirement
Height, solution does not seal in Dynamic link library pond, and solution is susceptible in high-speed rotation and is splashed and leakage phenomenon.In addition, literary
It offers《The development of liquid/solid double-phase scouring corrosion experiment apparatus and dynamic electro-chemical test》（Corrosion science and guard technology,
1993,5（4）：286-290）And document《The liquid fixed double phase flow erosive-corrosive wear of stainless steel and carbon steel is studied》（Material engineering,
2004,11:37-40）Working electrode is driven using hollow drive shaft（Tray sample）Rotation, reference electrode and auxiliary electrode are static
Method carries out dynamic electro-chemical test and Erosive Properties analysis, but does not introduce protection and the fixation of electrode.
Invention content：
In conclusion in order to overcome the shortcomings of prior art problem, it is dynamic that the present invention has developed a kind of rotary erosion abrasion
The reference electrode of state electrochemical test system protects structure, it solves reference electrode during rotary erosion wear test
Protection problem devises the protection structure of reference electrode.Working electrode, auxiliary electrode and the reference electrode setting of the present invention exists
In slurry liquid, it can reflect the electrochemical characteristic during erosive wear in real time, ensure the authenticity of measurement result；Reduce simultaneously
The attachment device of reference electrode peripheral hardware, simple in structure, operation facility, testing efficiency are high.
The technical scheme is that be achieved：
A kind of reference electrode protection structure of rotary erosion abrasion dynamic electrochemical test system, wherein the ginseng
Include mainly reference electrode, contact conductor sleeve, preceding protective shell and rear protective shell than electrode protection structure；The reference electrode dress
Among preceding protective shell and rear protective shell, preceding protective shell is connected with rear protective shell by protective shell screw；The conducting wire of reference electrode
It is connected to potentiostat after being drawn by contact conductor sleeve, contact conductor sleeve is fixed on preceding protective shell and rear protective shell；
The upper end of contact conductor sleeve is fixed on slurry tank cover board.
Further, the reference electrode includes calomel electrode and salt bridge, and salt bridge is full by what is filled in Luggin capillary
It is constituted with potassium chloride and agar mixture, calomel electrode and salt bridge form reference electrode.
Further, the contact conductor sleeve is fixed on the upper of preceding protective shell and rear protective shell by sleeve connection screw
Side.
Further, the upper end of the contact conductor sleeve is provided with screw thread, is threadedly secured on slurry tank cover board.
Further, reference electrode protection structure is placed directly within inside fluid to be measured.
Further, the preceding protective shell and rear protective shell of reference electrode protection structure are to use superhigh molecular weight polyethylene
Made of alkene material.
The beneficial effects of the invention are as follows：
1, greater impact in dynamic Electrochemical Test Procedure of the present invention for protecting rotary erosion wear test equipment
Reference electrode under force effect, including be used for machinery, chemical industry etc. each field has corrosive single-phase or liquid-solid two-phase fluid mistake
The electrochemical test system of the metal erosion Journal of Sex Research such as flow device, pipeline；Structure is protected by designing reference electrode, avoids height
Fast fluid directly impacts nature of glass reference electrode, solves the protection problem of electrode；By the reference electrode group with protection structure
Part is placed directly within inside slurry liquid, can reference electrode be placed directly within high-velocity fluid（Slurry liquid）Inside, working electrode（It is tested
Sample）It is also disposed in slurry liquid with auxiliary electrode, reflects the electrochemical characteristic during erosive wear in real time, ensure to measure knot
The authenticity of fruit；Reduce the attachment device of reference electrode peripheral hardware simultaneously；
2, reference electrode protection structure of the present invention is split structure, simple in structure, operation facility；Preceding protective shell
It is connected by protective shell screw with rear protective shell, contact conductor sleeve is fixed on preceding protective shell and rear protective shell by telescope-srew
Top, contact conductor sleeve is threadedly secured on slurry tank cover board, dismounting when use, easy to clean, and testing efficiency is high.
Description of the drawings：
Fig. 1 is the structural schematic diagram of working condition of the present invention；
Fig. 2 is that the reference electrode of the present invention protects the shape and structure schematic diagram of structure；
Fig. 3 is that the reference electrode of the present invention protects the assembling schematic diagram of structure.
Specific implementation mode：
With present invention will be described in further detail below with reference to the accompanying drawings.
As shown in FIG. 1, FIG. 1 is the structural schematic diagrams of working condition of the present invention.Rotary erosion abrasion dynamic electrification in Fig. 1
It includes motor 1, transmission main shaft 2, potentiostat 3, auxiliary electrode 4, reference electrode protection structure 5, work electricity to learn test system
Pole 6 is tested sample（Specimen size is 40 ' 20 ' 20mm, and in addition to a 20 ' 20mm are exposed, remaining five face is embedded in polytetrafluoro
Ethylene is protected in the housing of structure）, slurry tank 7, agitator arm 8, slurry tank cover board 9 and slurry liquid 10 etc.；Fig. 3 is reference electrode
The assembling schematic diagram for protecting structure, as shown in figure 3, contact conductor sleeve 5-1, reference electrode 5-2, Luggin capillary 5-3, preceding guarantor
Protective case 5-4, rear protective shell 5-5, protective shell screw 5-6, sleeve connection screw 5-7.
Referring to Fig. 1-3.The reference electrode that rotary erosion wears dynamic electrochemical test system protects structure, the ginseng
Than electrode protection structure mainly include reference electrode 5-2, contact conductor sleeve 5-1, Luggin capillary 5-3, preceding protective shell 5-4 and
Protective shell 5-5 afterwards；The reference electrode 5-2 is among preceding protective shell 5-4 and rear protective shell 5-5, preceding protective shell 5-4 and rear guarantor
Protective case 5-5 passes through the 5-6 connections of protective shell screw；The conducting wire of reference electrode 5-2 is connected to after being drawn by contact conductor sleeve 5-1
On potentiostat 3, output electric signal carries out electro-chemical test；The contact conductor sleeve 5-1 passes through sleeve connection screw 5-7
It is fixed on the top of preceding protective shell 5-4 and rear protective shell 5-5；The upper end of contact conductor sleeve 5-1 is provided with screw thread, passes through screw thread
It is fixed on slurry tank cover board 9；The reference electrode 5-2 includes calomel electrode and salt bridge, and salt bridge is by Luggin capillary 5-3
What the saturation potassium chloride and agar mixture of interior filling were constituted；The reference electrode protection structure 5 is placed directly within fluid to be measured
It is internal；The preceding protective shell 5-4 and rear protective shell 5-5 of the reference electrode protection structure are to use superhigh molecular weight polyethylene material
It is manufactured.
The course of work of the present invention is as follows：As shown in Figure 1,3.
1, it before on-test, first assembles rotary erosion and wears dynamic electrochemical test system.In Luggin capillary 5-3
Filling saturation potassium chloride, agar mixture constitute salt bridge, and salt bridge is assembled into reference electrode 5-2 with calomel electrode；By reference electrode
5-2 is placed among preceding protective shell 5-4, rear protective shell 5-5, and threaded connection hole is designed on preceding protective shell 5-4, rear protective shell 5-5,
Preceding protective shell 5-4, rear protective shell 5-5 pass through the 5-6 connections of protective shell screw；The conducting wire of reference electrode 5-2 passes through contact conductor set
Cylinder 5-1 is drawn, and is connected on potentiostat 3 and is met RE, electrode outlet line sleeve 5-1 is threadedly attached on slurry tank cover board 9.
Working electrode 6 is tested sample（Size is 40 ' 20 ' 20mm）Surface polishing, alcohol washes, are weighed, then using assay balance
It is installed in the housing of polytetrafluoroethylene (PTFE) protection structure, electrode cable is equipped among protection overcoat, by electrode cable by work
Electrode 6（Tested sample）It is connected on potentiostat 3 and meets WE, tested sample only exposes a test surfaces（20´20mm）With material
Slurries 10 contact；Auxiliary electrode 4 is provided with safeguard measure, is fixed on slurry tank cover board 9, and permanent electricity is connected to by contact conductor
CE is met on the instrument 3 of position；Referring to Fig. 1, auxiliary electrode 4 and working electrode 6 are respectively placed in the both sides of reference electrode protective device 5, Lu Jin
The tip of capillary 5-3 and working electrode 6（Tested sample）The distance of exposed surface is between 0.5 ~ 2mm.
2, the slurry liquid 10 of different liquid-solid ratioes, different soda acid salinity is prepared according to requirement of experiment.By prepared slurry
Liquid 10 is added in slurry tank 7.Slurry tank is promoted to by control button and contacts and fixes with cover board 9, at this time three-electrode system
It immerses in the slurry medium of slurry tank 7 simultaneously.After impregnating 30min pretreatments, static electro-chemical test is carried out first, passes through setting
Corresponding polarization potential and sweep speed, measure polarization curve when static state.
3, start control panel, motor speed and test period are set, and motor 1 drives transmission main shaft 2 to rotate, by stirring
It mixes impeller 8 to be stirred the slurry liquid 10 in slurry tank 7, starts erosion resistance tests.During experiment, as needed, often
Separated in time carries out primary dynamic electro-chemical test, carries out dynamic potential scanning in different time points, measures polarization curve.Examination
After testing, the electrochemical test data measured under static and current intelligence are analyzed.Tested sample is unloaded, through ultrasonic wave
（Acetone）After cleaning, sample weight after weighing with scale erosion resistance tests is adopted, the weight difference of sample is before experiment and after experiment
For weight loss.The erosion of each sample material can be further analyzed using micro- sem observation sample erosive wear rear surface pattern
Abrasion mechanism.For the reliability of guarantee test result, in triplicate with battery of tests.
Claims (6)
1. a kind of reference electrode of rotary erosion abrasion dynamic electrochemical test system protects structure, it is characterised in that：It is described
Reference electrode protection structure mainly include reference electrode, contact conductor sleeve, preceding protective shell and rear protective shell；The reference electricity
Among preceding protective shell and rear protective shell, preceding protective shell is connected with rear protective shell by protective shell screw for pole；Reference electrode
Conducting wire is connected to potentiostat after being drawn by contact conductor sleeve, and contact conductor sleeve is fixed on preceding protective shell and rear protective shell
On；The upper end of contact conductor sleeve is fixed on slurry tank cover board.
2. a kind of reference electrode protection knot of rotary erosion abrasion dynamic electrochemical test system according to claim 1
Structure, it is characterised in that：The reference electrode includes calomel electrode and salt bridge, and salt bridge is the saturation by being filled in Luggin capillary
What potassium chloride and agar mixture were constituted, calomel electrode and salt bridge form reference electrode.
3. a kind of reference electrode protection knot of rotary erosion abrasion dynamic electrochemical test system according to claim 1
Structure, it is characterised in that：The contact conductor sleeve is fixed on the upper of preceding protective shell and rear protective shell by sleeve connection screw
Side.
4. the reference electrode of rotary erosion abrasion dynamic electrochemical test system according to claim 1 protects structure,
It is characterized in that：The upper end of the contact conductor sleeve is provided with screw thread, is threadedly secured on slurry tank cover board.
5. a kind of reference electrode protection knot of rotary erosion abrasion dynamic electrochemical test system according to claim 1
Structure, it is characterised in that：The reference electrode protection structure is placed directly within inside fluid to be measured.
6. a kind of reference electrode protection knot of rotary erosion abrasion dynamic electrochemical test system according to claim 1
Structure, it is characterised in that：The preceding protective shell and rear protective shell of the reference electrode protective device are to use superhigh molecular weight polyethylene
Made of alkene material.
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| CN106769583B (en) * | 2017-01-19 | 2023-06-23 | 北京科技大学 | Rotary friction electrochemical testing device |
| CN108760614A (en) * | 2018-04-25 | 2018-11-06 | 上海海事大学 | The online electrochemical testing device of erosion corrosion and method |
| CN111678827A (en) * | 2020-07-19 | 2020-09-18 | 西南石油大学 | Erosion and corrosion interaction wear simulation test device |
| CN112683154B (en) * | 2020-12-28 | 2022-05-17 | 福州大学 | Indirect measurement method for abrasion of parts which are not easy to disassemble, such as high-speed switch valve and the like |
| CN114370901B (en) * | 2022-03-22 | 2022-06-10 | 四川省郫县豆瓣股份有限公司 | High-precision liquid flow measuring probe |
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| CN200952990Y (en) * | 2006-09-22 | 2007-09-26 | 重庆工学院 | Corrosion and wear interaction dynamic measuring device |
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