CN109507100A - Corrosion electrochemistry test method and device under plate-shape metal sample high stress - Google Patents

Corrosion electrochemistry test method and device under plate-shape metal sample high stress Download PDF

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Publication number
CN109507100A
CN109507100A CN201811407170.6A CN201811407170A CN109507100A CN 109507100 A CN109507100 A CN 109507100A CN 201811407170 A CN201811407170 A CN 201811407170A CN 109507100 A CN109507100 A CN 109507100A
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China
Prior art keywords
sample
electrolytic cell
corrosion
high stress
plate
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CN201811407170.6A
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Chinese (zh)
Inventor
于美
范世洋
刘建华
李松梅
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Beihang University
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Beihang University
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Priority to CN201811407170.6A priority Critical patent/CN109507100A/en
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    • 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
    • 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
    • G01N3/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/08Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
    • 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
    • G01N2203/0014Type of force applied
    • G01N2203/0016Tensile or compressive
    • 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

Abstract

The invention discloses electrochemical test method and devices under a kind of plate-shape metal sample high stress, are related to field of electrochemical test.The electrochemical test method is using the wide centre in both ends is narrow and both ends are provided with the plate-shape metal tensile sample of connecting hole, it is connected between tensile sample and fixture using pin type, pin is using high-intensitive silicon carbide ceramics stick, ensure that pin is able to bear high stress and the insulation between sample, plate tensile sample between insulation clamping screw and electrolytic cell etch pit by being adjacent to, and by rubber seal rings for seal waterproof, 1000MPa high stress level can be loaded onto and carry out accurate electrochemical measurement in situ.The experimental provision is made of corrosion electrolytic cell, loads fixture, plate tensile sample three parts, and the corrosion electrolytic cell includes stationary barrier and closed cylinder etchant solution pond, and etchant solution pond has multiple apertures, and temperature control, ventilation, solution circulation may be implemented.Present apparatus method is simple and easy, convenient disassembly, and electrochemical parameter measurement is accurate, can be carried out electro-chemical test under high stress level, and be able to achieve the simulation test of a variety of environmental conditions.

Description

Corrosion electrochemistry test method and device under plate-shape metal sample high stress
Technical field
The present invention relates to electrochemical test method and its device more particularly to a kind of plates under a kind of metal material stress Corrosion test and electrochemical test method and device under shape metal material high stress.
Background technique
It is compound in stress and corrosive medium to be suitable for research metal material for corrosion testing apparatus under metal material stress Corrosion process rule under effect.And by electrochemical test method, it can effectively analyze the reaction for obtaining corrosion process Journey and thermodynamics, dynamic law.It further, can be with by the regulation to factors such as solution system, pH value, temperature, times Obtain stress and multifactor collective effect to the affecting laws of corrosion process.Currently, the tensile stress for metal material acts on Lower electrochemical test experiment device is mainly placed at organic glass electrolytic cell internal cavities center using by tensile sample, makes Solution in sample and electrolytic cell is sealed with rubber stopper, and will be insulated between sample and fixture by polytetrafluoroethylene (PTFE).But this Presently, there are many limitations for kind test method: sample assembly need to do waterproof sealing processing, be not easy to disassembly, repeatedly measurement;Examination Sample work area is handled using manual sealing mode, and work area is inaccurate, easy crevice corrosion, the depth of parallelism are poor;It is poly- by coating It insulate, insulate under high stress vulnerable between tetrafluoroethene and fixture, be not suitable for measuring under high stress level.
Summary of the invention
In view of the drawbacks of the prior art, it is an object of the invention to realize a variety of rings under plate-shaped metal material high stress level Accurate electrochemical measurement under the factor stimulation control condition of border, the lower test button Corrosion Thermodynamics of analysis high stress level effect, Dynamic law inquires into corrosion process changing rule, show that varying environment factor and stress collective effect influence corrosion process Rule.The present invention provides corrosion electrochemistry test method and devices under a kind of plate-shaped metal material high stress level, not only may be used To realize the electro-chemical test under high stress level, and it is convenient using load, and easy to operate, measurement accuracy is high, can carry out The control of a variety of environmental factors is simulated.
Corrosion electrochemistry test method and device under a kind of plate-shape metal sample high stress, the electro-chemical test side Method is narrow using the wide centre in both ends and both ends are provided with connecting hole for the electrochemical in-situ precise measurement under great horizontal stress effect Plate-shape metal tensile sample.It is connected between tensile sample and fixture using pin type, pin is using high-intensitive silicon carbide ceramics Stick ensures that pin is able to bear high stress and the insulation between sample, is loaded onto high stress level, stress by cupping machine Horizontal reachable 1000MPa.Coating film neoprene on the inside of stretching clamp, it is ensured that sample side and energy when fixture interior side contacts are complete All insulation.The corrosion electrolytic cell is provided with round etch pit, after plate tensile sample applies load, passes through insulation clamping screw and electricity It is adjacent between solution pond etch pit, and passes through rubber seal rings for seal waterproof.The experimental rig by corrosion electrolytic cell, loads fixture, Plate tensile sample three parts composition, the corrosion electrolytic cell includes stationary barrier and closed cylinder etchant solution pond, etchant solution pond Have multiple apertures, temperature control, ventilation, solution circulation may be implemented, realize the simulation of a variety of environmental factors.
The electrochemical test method uses three-electrode system, and testing procedure is as follows
1) by tensile sample by connecting between high-strength carborundum ceramic rod and fixture, operation cupping machine adds sample Stress level needed for being downloaded to test;
2) electrolytic cell for being provided with etch pit is adjacent to tensile sample, rubber seal is lined at etch pit, corrode hole site Registration coupon gauge length section corrosion area screws insulation clamping screw for sample and is adjacent to electrolytic cell etch pit, and etch pit size is Working electrode area;
3) test solution is added in electrolytic cell opening, adjusts experimental condition needed for experimental rig aperture controls;
4) reference electrode is placed in Luggin capillary, is put into platinum electrode, connect the electrode to electrochemistry work using conducting wire It stands, starts electro-chemical test;
5) after the completion of testing, first solution is discharged, then sample unloading is removed.
The corrosion electrolytic cell is organic glass processing and fabricating, is equipped with stationary barrier and etchant solution pond, partition and corrosion It connects and fixes by stainless steel screw rod between solution pool.Stationary barrier center is equipped with screw thread, and is equipped with clamping screw and passes through partition Center screw thread makes sample be close to etch pit, clamping screw used is the nylon material of insulation by screwing clamping screw.
The corrosion electrolytic cell is equipped with Luggin capillary, auxiliary electrode, and is fixed by rubber stopper.Be provided with gas outlet, into Liquid mouth, liquid outlet, air inlet.Liquid outlet and air inlet are connected to rubber tube, and are switched by spring clip.The corrosion electrolysis Pond is additionally provided with thermometer, thermocouple, it can be achieved that temperature real-time monitoring and control.
Corrosion electrochemistry test method and device under plate-shaped metal material high stress level provided by the invention, high stress water The flat lower insulating protection effect of effect will not fail, dielectric pin is indeformable, and the accurate electrochemical that may be implemented under high stress level is surveyed Examination.Working electrode area is fixed by the etch pit of etchant solution pond fixed-area, and passes through rubber seal waterproof sealing, work It is accurate to make electrode area, and does not need approved sample, thus it is easy to operate, and measurement accuracy is high.Sample is bonded by clamping screw to be corroded Solution pool is fixed, easy to disassemble, multiple measurement.In addition, by ventilation, the monitoring adjusting of temperature, solution loop control, Ke Yijin The control simulation of a variety of environmental factors of row, obtains varying environment factor and stress collective effect to corrosion process affecting laws.
Detailed description of the invention
Fig. 1 is experimental rig structural schematic diagram of the invention;
Fig. 2 is present invention test electrolytic cell top view;
Fig. 3 is plate-shape metal sample schematic diagram used in the present invention;
In figure:
1- fixture, 2- silicon carbide rod, 3- sample, the gas outlet 4-, 5- inlet, 6- liquid outlet, 7- air inlet, 8- Lu Jinmao The fixed spiral shell of tubule, 9- thermocouple, 10- heating tube, 11- auxiliary electrode, 12- solution pool, 13- sealing ring, 14- clamping screw rod, 15- Bar, 16- stationary barrier, 17- rubber stopper.
Specific embodiment:
Corrosion electrochemistry under plate-shape metal sample high stress of the invention is tested with reference to the accompanying drawings and examples Method and device is described in detail.
Embodiment
Corrosion electrochemistry test method and device under a kind of plate-shape metal sample high stress, may be implemented high stress water It is flat to act on lower plate-shaped metal material electro-chemical test.This experimental rig is mainly by corrosion electrolytic cell, loads fixture, plate tensile sample three Part forms, such as Fig. 1.Plate-shape metal sample used is that the wide centre in both ends is narrow and both ends are provided with the plate of connecting hole and stretch examination Sample 3, sample specific size such as Fig. 3.It is connected between tensile sample 3 and fixture 1 using pin type, pin is using high-intensitive silicon carbide Ceramic rod 2,3 absolutely insulation, fixtures 1 are connected with cupping machine between sample.1 inside coating film neoprene rubber of stretching clamp Glue, it is ensured that sample side and energy when fixture interior side contacts are completely insulated.
Corrosion electrolytic cell is organic glass processing and fabricating, such as Fig. 2, be equipped with stationary barrier 16 and etchant solution pond 12,16 every It connects and fixes by stainless steel screw rod 15 between plate and etchant solution pond 12, intermediate there are a distances for penetrating sample.Gu 16 center of determine dividing plate is equipped with screw thread, and is equipped with clamping screw 14 and passes through partition center screw thread, and clamping screw 14 used is insulation Nylon material.
It is additionally provided with gas outlet 4, inlet 5, liquid outlet 6, air inlet 7 above etchant solution pond 12, and is put by aperture Heating tube 10, thermocouple 9 may be implemented temperature control, ventilation, carry out solution circulation using circulating pump, realize a variety of environmental factors Simulation, obtain varying environment factor and stress collective effect to corrosion process affecting laws.
Electro-chemical test uses three-electrode system, and corrosion electrolytic cell is equipped with Luggin capillary 8, auxiliary electrode 11, and passes through Rubber stopper 17 is fixed, and when test, reference electrode is placed in Luggin capillary 8, and electrode is connected to electrochemical workstation by conducting wire.
Specific experiment process of the invention are as follows:
1) tensile sample 3 is passed through and corrodes electrolytic cell and fixture 1, behind appropriate alignment jig position, by silicon carbide ceramics stick 2 It is inserted into the connecting hole of fixture and sample 3, sample is fixed;
2) electrolytic cell for being provided with etch pit is adjacent to tensile sample, rubber seal 13 is lined at etch pit, corrode hole location Registration coupon gauge length section corrosion area is set, clamping screw 14 is then aligned the intermediate fragment position of tensile sample 3, turn clamping screw 14 make 3 interlude of tensile sample be close to etch pit, apply 1000MPa stress to tensile sample 3 by cupping machine;
3) liquid outlet 6 is closed, test solution is added from inlet 5, air inlet 7 connects gas cylinder and is passed through gas, and adjusts Air inflow.Later, heating tube 10 and thermocouple 9 are connect with temperature controller, adjusts solution temperature;
4) be put into saturated calomel electrode in Luggin capillary 8, by working electrode, that is, tensile sample 3, saturated calomel electrode, Auxiliary electrode 11 is connected by conducting wire with electrochemical workstation, and electro-chemical test is carried out;
5) after electro-chemical test, first conducting wire is unloaded, the discharge test solution of liquid outlet 6 is opened, then unclamps and compress Screw rod 14 unloads it to tensile sample by cupping machine, finally unloads tensile sample 3.
Corrosion electrochemistry test method and device under plate-shape metal sample high stress as described above, may be implemented height Stress level load, easy to operate, load is convenient, and measurement is accurate, and multiple environmental conditions control simulation may be implemented, obtain different rings Border factor and stress collective effect are to corrosion process affecting laws.

Claims (4)

1. corrosion electrochemistry test method and device under a kind of plate-shape metal sample high stress, the electrochemical test method For the electrochemical in-situ precise measurement under great horizontal stress effect, using three-electrode system, it is characterised in that: wide using both ends Intermediate narrow and both ends are provided with the plate-shape metal tensile sample 3 of connecting hole, are connected between tensile sample 3 and fixture 1 using pin type, Pin ensures that pin is able to bear high stress and the insulation between sample, by stretching using high-intensitive silicon carbide ceramics stick 2 Testing machine is loaded onto high stress level, and stress level is rotten by sample and electrolytic cell by insulation clamping screw 14 up to 1000MPa It is adjacent between borrosion hole, it is ensured that the accuracy of insulation and working electrode area, and waterproof is sealed by rubber seal 13, it is added real After testing solution, environmental condition control simulation is carried out by adjusting experimental rig aperture;The experimental rig by corrosion electrolytic cell, plus Fixture, plate tensile sample three parts composition are carried, the corrosion electrolytic cell includes stationary barrier 16 and closed cylinder etchant solution pond, corruption Erosion solution pool has multiple apertures, and temperature control, ventilation, solution circulation may be implemented, realize the simulation of a variety of environmental factors.
2. corrosion electrochemistry test method and device under plate-shape metal sample high stress described in accordance with the claim 1, Be characterized in that: steps are as follows for the electro-chemical test
1) by tensile sample 3 by connecting between high-strength carborundum ceramic rod 2 and fixture 1, operation cupping machine adds sample Stress level needed for being downloaded to test;
2) electrolytic cell for being provided with etch pit is adjacent to tensile sample, rubber seal, etch pit position alignment is lined at etch pit Sample marking distance section corrosion area screws insulation clamping screw 14 for sample and is adjacent to electrolytic cell etch pit, and etch pit size is work Make electrode area;
3) test solution is added in electrolytic cell opening, adjusts experimental condition needed for experimental rig aperture controls;
4) reference electrode is placed in Luggin capillary 8, is put into platinum electrode, connect the electrode to electrochemical operation using conducting wire It stands, starts electro-chemical test;
5) after the completion of testing, first solution is discharged, then sample unloading is removed.
3. corrosion electrochemistry test method and device under plate-shape metal sample high stress described in accordance with the claim 1, It is characterized in that, the corrosion electrolytic cell is equipped with stationary barrier 16, is consolidated partition and etchant solution pond 12 using stainless steel screw rod 15 It is fixed, partition center screw thread is passed through using nylon material clamping screw 14, by screwing clamping screw, sample is made to be close to etch pit.
4. corrosion electrochemistry test method and device under plate-shape metal sample high stress described in accordance with the claim 1, Be characterized in that: the corrosion electrolytic cell is equipped with Luggin capillary 8, auxiliary electrode 11, and fixed by rubber stopper 17;It is provided with outlet Mouth 4, inlet 5, liquid outlet 6, air inlet 7, liquid outlet and air inlet are connected to rubber tube, and are switched by spring clip;Institute State corrosion electrolytic cell be additionally provided with heating tube 10, thermocouple 9, it can be achieved that temperature real-time monitoring and control.
CN201811407170.6A 2018-11-23 2018-11-23 Corrosion electrochemistry test method and device under plate-shape metal sample high stress Pending CN109507100A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110261294A (en) * 2019-06-04 2019-09-20 中国船舶重工集团公司第七二五研究所 Metal erosion electrochemical test experiment device in cracked zone under a kind of simulated deep-sea environment
CN111504801A (en) * 2020-05-20 2020-08-07 西安稀有金属材料研究院有限公司 Device and method for performing stress corrosion experiment in high-temperature liquid phase corrosion environment
CN111855556A (en) * 2020-06-30 2020-10-30 国网天津市电力公司电力科学研究院 Metallographic detection device and detection method for corrosion-resistant iron matrix welded joint
CN113588417A (en) * 2021-06-24 2021-11-02 中国特种设备检测研究院 Metal coating stress corrosion test method and device in corrosion environment
CN113866083A (en) * 2021-08-16 2021-12-31 中山大学 Corrosion device for simulating combined action of dynamic microorganisms and stress
CN115112555A (en) * 2022-07-20 2022-09-27 黄山学院 Stress electrochemical corrosion device
CN115855653A (en) * 2022-12-15 2023-03-28 太原理工大学 Corrosion electrochemistry testing arrangement of controllable temperature
CN116539512A (en) * 2023-05-12 2023-08-04 北京科技大学 Stress corrosion simulation experiment equipment

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CN103323387A (en) * 2013-06-25 2013-09-25 沈阳建筑大学 Electro-chemical corrosion simulator with in-situ loading
CN204116137U (en) * 2014-10-24 2015-01-21 中国石油天然气集团公司 A kind of electrochemical corrosion test fixture loading tension for petroleum pipeline
CN106769474A (en) * 2017-01-14 2017-05-31 常州大学 Loading biaxial tension stress sample Experiment in Erosive Electrochemistry device and method of testing

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Publication number Priority date Publication date Assignee Title
CN2217798Y (en) * 1994-12-15 1996-01-17 核工业理化工程研究院 Spring constant-load stress corrosion testing device
CN101608995A (en) * 2008-06-20 2009-12-23 宝山钢铁股份有限公司 The measuring method of galvanic corrosion and sample thereof under the high-stress state of welded tube weld seam
CN103323387A (en) * 2013-06-25 2013-09-25 沈阳建筑大学 Electro-chemical corrosion simulator with in-situ loading
CN204116137U (en) * 2014-10-24 2015-01-21 中国石油天然气集团公司 A kind of electrochemical corrosion test fixture loading tension for petroleum pipeline
CN106769474A (en) * 2017-01-14 2017-05-31 常州大学 Loading biaxial tension stress sample Experiment in Erosive Electrochemistry device and method of testing

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110261294A (en) * 2019-06-04 2019-09-20 中国船舶重工集团公司第七二五研究所 Metal erosion electrochemical test experiment device in cracked zone under a kind of simulated deep-sea environment
CN110261294B (en) * 2019-06-04 2022-04-19 中国船舶重工集团公司第七二五研究所 Electrochemical test device for simulating metal corrosion of crack area under deep sea environment
CN111504801A (en) * 2020-05-20 2020-08-07 西安稀有金属材料研究院有限公司 Device and method for performing stress corrosion experiment in high-temperature liquid phase corrosion environment
CN111855556A (en) * 2020-06-30 2020-10-30 国网天津市电力公司电力科学研究院 Metallographic detection device and detection method for corrosion-resistant iron matrix welded joint
CN113588417A (en) * 2021-06-24 2021-11-02 中国特种设备检测研究院 Metal coating stress corrosion test method and device in corrosion environment
CN113866083A (en) * 2021-08-16 2021-12-31 中山大学 Corrosion device for simulating combined action of dynamic microorganisms and stress
CN115112555A (en) * 2022-07-20 2022-09-27 黄山学院 Stress electrochemical corrosion device
CN115112555B (en) * 2022-07-20 2023-09-22 黄山学院 Stress electrochemical corrosion device
CN115855653A (en) * 2022-12-15 2023-03-28 太原理工大学 Corrosion electrochemistry testing arrangement of controllable temperature
CN116539512A (en) * 2023-05-12 2023-08-04 北京科技大学 Stress corrosion simulation experiment equipment
CN116539512B (en) * 2023-05-12 2023-12-22 北京科技大学 Stress corrosion simulation experiment equipment

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Application publication date: 20190322