CN109470753A - A kind of electrochemical working electrode preparation facilities for evaluating metal coating corrosion inhibition - Google Patents

A kind of electrochemical working electrode preparation facilities for evaluating metal coating corrosion inhibition Download PDF

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Publication number
CN109470753A
CN109470753A CN201811263268.9A CN201811263268A CN109470753A CN 109470753 A CN109470753 A CN 109470753A CN 201811263268 A CN201811263268 A CN 201811263268A CN 109470753 A CN109470753 A CN 109470753A
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metal coating
glass tube
shoulder
coating sample
electrode
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CN109470753B (en
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邓宽海
林元华
王晓红
曾德智
张晓燕
刘冰
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Southwest Petroleum University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28Electrolytic cell components
    • G01N27/30Electrodes, e.g. test electrodes; Half-cells
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28Electrolytic cell components

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
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Abstract

The present invention provides a kind of electrochemical working electrode preparation facilities for evaluating metal coating corrosion inhibition, it is characterised in that: device specifically includes that transparent PVC plastic plate, metal coating sample, rubber seal, annulus shoulder, transparent PVC electrolytic cell, slender glass tube, positioning disc, shoulder port, support disk;Metal coating sample includes blank face and coat side two parts, and for blank face for connecting electrochemical workstation, coat side is divided into multiple same areas, is respectively used to material characterizations and the evaluation such as activation polarization test and impedance spectrum test;Transparent PVC plastic plate is for fixing metal coating sample;Support disk on transparent PVC electrolytic cell has aperture of the annulus shoulder fixed and positioned for slender glass tube with export to electrode;Slender glass tube is fixed on slender glass tube center by positioning disc and annulus shoulder, it is ensured that reference electrode keeps best and same distance with metal coating sample always.The present invention is suitable for electrochemical measurement and material characterization technical field.

Description

A kind of electrochemical working electrode preparation facilities for evaluating metal coating corrosion inhibition
Technical field
The present invention relates to electrochemical corrosion measurement and material characterization technical field, specifically a kind of evaluation metal coating inhibition The electrochemical working electrode preparation facilities of performance.
Background technique
Electrochemical research measurement includes common activation polarization, cyclic voltammetric, AC impedance and the electrification risen at present Learn the methods of noise.Since electrochemical method can accurately measure the transfer of charge in electrochemical reaction process, answer extensively at present Use the different fields such as the evaluation of coating corrosion inhibition, corrosion monitoring and material characterization.Electrochemical corrosion test in the most commonly used is Three-electrode system that is, by forming to electrode (also known as auxiliary electrode), reference electrode and working electrode, and is measured in electrochemical research In, the reaction process that is mainly occurred on research work electrode surface.Metal coating inhibition is being evaluated using electrochemical method When performance, after activation polarization test, the metal coating surface as working electrode will receive a degree of damage, cause The coating of metal surface is imperfect, if directly carrying out ac impedance spectroscopy test, to will lead to result error very big.Therefore, in metal In coating corrosion inhibition evaluation procedure, the preparation facilities and method of working electrode have irreplaceable in electrochemical field Status.
Mainly there are inorganic and high-molecular organic material two major classes in working electrode encapsulating material used in now, wherein having Machine high molecular material is the most frequently used.The high-molecular organic material used in electrochemical working electrode encapsulation mainly has following several Kind: polytetrafluoroethylene (PTFE), poly- trifluoro-ethylene, poly(aryl ether ketone) and epoxy resin etc..
Not only chemical stability and electrical insulating property are preferable for polytetrafluoroethylene (PTFE) and poly- trifluoro-ethylene, but also almost all of strong Acid, highly basic, strong oxidizer and organic solvent all do not work to it.In addition, polytetrafluoroethylene (PTFE) can be in 250 DEG C~260 DEG C high temperature Lower long-time service, poly- trifluoro-ethylene, which has, widely uses temperature -50~130 DEG C, and the caking property of metal is good, transparent.So And both materials are all not easy melt fabrication, processing difficulties, easily lead to the electrode leakage of encapsulation, and electrode is caused to scrap, The polytetrafluoroethylene (PTFE) encapsulating material of hydrophobic easily has bubble attachment at the electrode surface in determination of aqueous solution simultaneously, leads to not Carry out electrochemical measurement;Poly- trifluoro-ethylene organic solvent resistance is poor, is not suitable for the electrochemical gaging of organic phase.
Poly(aryl ether ketone) is a series of special engineering plastics haveing excellent performance, have excellent rub resistance, fire-retardant, resistant to hydrolysis and Radiation resistance, stability is good, easily processed into type, and under the operating conditions such as high temperature, high pressure and high humility, insulating properties is remained to It is effectively retained;But the resinoid carries out needing higher temperature when melt-processed as thermoplastic materials, and resin after melting Viscosity is larger, and easily bubble is wrapped near electrode matrix, and electrode is caused to can not work normally, and raw material are costly;
Ring epoxy resin is due to good machinability and higher cost performance, in the encapsulation of electrochemical working electrode In be frequently used.But because its curing material is crisp, resistance to cracking energy, shock resistance are lower, and poor heat resistance, make its application Receive certain limitation.Importantly, after finishing electro-chemical test, to be observed with scanning electron microscope (SEM) The erosion profile of sample, or with energy spectrum analysis (EDS) study corrosion product ingredient, need by outside electrode epoxy resin layer, Scolding tin and metal flexible circuit conductor etc. remove, and steadily could place and test, and the operation leads to the destructurized of electrode, electrode without Method continues to use, thus the utilization rate of electrode is low.If remaking an electrode and carrying out electrochemical test, system is not only increased Make the workload and cost of electrode, and the variation meeting of the difference of different batches material, the error of manufacturing process and experimental enviroment Cause test and test result relatively large deviation occur, and greatly reduces working efficiency.
Therefore, in order to improve the multiple utilization rate and electro-chemical test working efficiency of working electrode, preparation work electricity is reduced Workload, cost and its caused measurement error of pole, the present invention propose a kind of electrochemistry for evaluating metal coating corrosion inhibition Using any high-molecular organic material (such as epoxy resin, polytetrafluoroethylene (PTFE)), i.e., working electrode preparation facilities, the device are not required to The electrochemical working electrode that can be used for evaluating metal coating corrosion inhibition can quickly and easily be prepared.
Summary of the invention
The object of the present invention is to propose a kind of electrochemical working electrode preparation facilities for evaluating metal coating corrosion inhibition.
To achieve the above object, the present invention takes following technical scheme:
A kind of electrochemical working electrode preparation facilities for evaluating metal coating corrosion inhibition proposed by the present invention, feature exist In, specifically include that sample slot, transparent PVC plastic plate, metal coating sample, transparent PVC electrolytic cell, rubber seal, bolt, Support disk, slender glass tube, reference electrode, to electrode, positioning disc, annulus shoulder, shoulder port, insulated conductor.Wherein, Metal coating sample includes blank face and coat side two parts, and blank face is applied for connecting insulated conductor and electrochemical workstation Level is divided into several same areas (quantity that same area is arranged according to experimental program), can be respectively used to metal coating not Material characterizations and the evaluations such as activation polarization test and impedance spectrum test under the conditions of;Transparent PVC plastic plate includes sample slot With the threaded hole for connection, it is mainly used for fixed metal coating sample;Transparent PVC electrolytic cell mainly includes straightway, circular arc Section, shoulder port, support disk and the threaded hole for connection, shoulder port area is certain, the reality as metal coating sample Border working face, and disk is supported to have aperture of the annulus shoulder fixed and positioned for slender glass tube with export to electrode; Rubber seal positioned at shoulder port is mainly used for sealing metal coating sample;Bolt is mainly used for consolidating on metal coating sample It is scheduled on the shoulder port of transparent PVC electrolytic cell;Slender glass tube includes upper straight section, conical section, lower port and setting circle Disk, lower port is for fixed to electrode, and positioning disc is fixed on slender glass tube center by annulus shoulder, it is ensured that elongated glass Reference electrode in glass pipe keeps best and identical distance with metal coating sample always;Reference electrode is located at slender glass tube Center, and be in close contact with slender glass tube conical section, it is contacted by capillary effect with test solution.
The invention has the advantages that
(1) device is not required to using any organic and inorganic macromolecule material (such as epoxy resin, polytetrafluoroethylene (PTFE)), can be simple The electrochemical working electrode that can be used for evaluating metal coating corrosion inhibition is rapidly prepared, can be carried out simultaneously under different condition Coating morphology and chemical composition analysis etc. after activation polarization test, impedance spectrum test and test;
(2) after finishing electro-chemical test, the erosion profile of scanning electron microscope (SEM) observation sample can be directly used, or is used Corrosion product ingredient is studied in energy spectrum analysis (EDS), epoxy resin layer, scolding tin and the metal flexible circuit conductor being not required to outside removal electrode Deng;
(3) structure of device and electrode preparation method are simple, can be realized the quick preparation of electrode, be also able to achieve reference electrode with The distance between working electrode saves best and identical always, additionally it is possible to guarantee that the working electrode prepared has consistent shape Therefore state not only increases the preparation efficiency and utilization rate of working electrode, and improve metal coating inhibition to greatest extent The accuracy of performance evaluation test result.
Detailed description of the invention
Fig. 1 is schematic structural view of the invention.
Fig. 2 is the overlooking structure diagram of metal coating sample and transparent PVC plastic plate.
Specific embodiment
With reference to the accompanying drawings and embodiments, the present invention will be described in detail.
Referring to Fig. 1 and Fig. 2, a kind of electrochemical working electrode preparation for evaluating metal coating corrosion inhibition proposed by the present invention Device, which is characterized in that specifically include that sample slot 2, transparent PVC plastic plate 3, metal coating sample 4, transparent PVC electrolytic cell 8, Rubber seal 5, bolt 6, support disk 18, slender glass tube 10, reference electrode 9, to electrode 11, positioning disc 15, annulus Shoulder 7, shoulder port 16, insulated conductor 23.Wherein, metal coating sample 4 includes 21 two parts of blank face 20 and coat side, empty Fine flour 21 for connecting insulated conductor 23 and electrochemical workstation, divide for several same areas (according to experiment side by coat side 22 Case setting same area quantity), can be respectively used to metal coating at different conditions activation polarization test and impedance spectrum Material characterizations and the evaluations such as test;Transparent PVC plastic plate 3 includes sample slot 2 and the threaded hole 1 for connection, is mainly used for solid Deposit category coating sample 4;Transparent PVC electrolytic cell 8 mainly includes straightway 12, arc section 14, shoulder port 16, support disk 18 And the threaded hole 1 for connection, 16 area of shoulder port is certain, as the real work face of metal coating sample 4, and props up and holds round Disk 18 has aperture 13 of the annulus shoulder 7 fixed and positioned for slender glass tube 10 with export to electrode 11;Positioned at shoulder The rubber seal 5 of port 16 is mainly used for sealing metal coating sample 4;Bolt 6 is mainly used for metal coating sample 4 is fixed In the shoulder port 16 of transparent PVC electrolytic cell 8;Slender glass tube 10 includes upper straight section 20, conical section 19, lower port 17 With positioning disc 15, for lower port 17 for fixed to electrode 11, positioning disc 15 is fixed on slender glass by annulus shoulder 7 The center of pipe 10, it is ensured that the reference electrode 9 in slender glass tube 10 kept always with metal coating sample 4 it is best and it is identical away from From;Reference electrode 9 is located at 10 center of slender glass tube, and is in close contact with 10 conical section 19 of slender glass tube, passes through capillary Effect is contacted with test solution.

Claims (1)

1. a kind of electrochemical working electrode preparation facilities for evaluating metal coating corrosion inhibition, which is characterized in that device mainly wraps It includes: sample slot (2), transparent PVC plastic plate (3), metal coating sample (4), rubber seal (5), bolt (6), annulus shoulder (7), transparent PVC electrolytic cell (8), slender glass tube (10), positioning disc (15), shoulder port (16), support disk (18);Gold Belonging to coating sample (4) includes blank face (20) and coat side (21) two parts, and blank face (20) is for connecting insulated conductor (22) And electrochemical workstation, coat side (21) are divided into several same areas (quantity that same area is arranged according to experimental program), It can be respectively used to material characterizations and the evaluations such as the activation polarization of metal coating at different conditions is tested and impedance spectrum is tested;Thoroughly Bright PVC plastic flitch (3) includes sample slot (2) and the threaded hole (1) for connection, is mainly used for fixed metal coating sample (4); Transparent PVC electrolytic cell (8) mainly includes straightway (12), arc section (14), shoulder port (16), support disk (18) and is used for The threaded hole (1) of connection, shoulder port (16) area is certain, as the real work face of metal coating sample (4), and props up and holds round Disk (18) has the annulus shoulder (7) and export the aperture to electrode (11) for being used for that slender glass tube (10) to fix and position (13);Rubber seal (5) positioned at shoulder port (16) is mainly used for sealing metal coating sample (4);Bolt (6) is mainly used In the shoulder port (16) that metal coating sample (4) is fixed on to transparent PVC electrolytic cell (8);Slender glass tube (10) includes upper Portion's straightway (20), conical section (19), lower port (17) and positioning disc (15), lower port (17) is for fixed to electrode (11), positioning disc (15) is fixed on slender glass tube (10) center by annulus shoulder (7), it is ensured that in slender glass tube (10) Reference electrode (9) keep best and identical distance with metal coating sample (4) always;Reference electrode (9) is located at elongated glass Glass pipe (10) center, and be in close contact with slender glass tube (10) conical section (19), it is connect by capillary effect and test solution Touching.
CN201811263268.9A 2018-10-28 2018-10-28 Electrochemical working electrode preparation device for evaluating corrosion inhibition performance of metal coating Active CN109470753B (en)

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CN110646338A (en) * 2019-09-24 2020-01-03 广西大学 External corrosion electrochemical test device of sample
CN111443124A (en) * 2020-04-24 2020-07-24 常州大学 Experimental device for stray current corrosion simulation and near-surface micro-area pH measurement
CN114609206A (en) * 2022-03-21 2022-06-10 中山大学 Electrochemical test method for abradable seal coating system

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CN111443124A (en) * 2020-04-24 2020-07-24 常州大学 Experimental device for stray current corrosion simulation and near-surface micro-area pH measurement
CN114609206A (en) * 2022-03-21 2022-06-10 中山大学 Electrochemical test method for abradable seal coating system
CN114609206B (en) * 2022-03-21 2023-08-11 中山大学 Electrochemical testing method of abradable seal coating system

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