CN102706935B - Electrolytic cell for stereo microscope in-situ corrosion analysis - Google Patents
Electrolytic cell for stereo microscope in-situ corrosion analysis Download PDFInfo
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- CN102706935B CN102706935B CN201210067093.0A CN201210067093A CN102706935B CN 102706935 B CN102706935 B CN 102706935B CN 201210067093 A CN201210067093 A CN 201210067093A CN 102706935 B CN102706935 B CN 102706935B
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Abstract
An electrolytic cell for stereo microscope in-situ corrosion analysis is characterized in that the electrolytic cell is cylindrical or rectangular. The electrolytic cell comprises a cylinder body, a cylinder cover, a cylinder bottom and bolts. The cylinder cover and the cylinder bottom are connected with each other through the bolts. A liquid feeding cylinder, an exhaust hole, a reference electrode inserting hole, an observation window, a counter electrode wiring terminal, a working electrode connector are sequentially disposed on the cylinder body from left to right. A stirring magneton is disposed in the middle of the cylinder bottom. The liquid feeding cylinder is inserted into the middle lower portion of the cylinder body vertically. A sealing rubber plug provided with an air inlet pipe and an air outlet is disposed at the upper end of the liquid feeding cylinder. The air inlet pipe is inserted into the lower portion of the liquid feeding cylinder vertically. The air outlet is located at the upper end of the liquid feeding cylinder. An aerator is disposed at the lower end of the air inlet pipe. A rubber plug is disposed on the exhaust hole on the cylinder cover. A reference electrode is inserted into the reference electrode inserting hole. An annular platinum sheet counter electrode is disposed on the cylinder cover on circumference of the bottom face of the observation window. The working electrode connector is inserted into the upper portion of the cylinder body vertically. A testing sample which is placed horizontally is fixed to the lower end of the working electrode connector through a bolt or a clamping ring.
Description
Technical field
The present invention relates to a kind of Experiment in Erosive Electrochemistry device, relate in particular to a kind of electrolytic cell that stereomicroscope in-situ corrosion is analyzed that is applicable to.
Background technology
Utilize stereomicroscope in-situ observation material surface erosion profile evolution process to there is unique advantage, if not affected by corrosive medium, simple to operate, image is undistorted etc., particularly, along with the raising of stereomicroscope enlargement factor, this technology must be more widely used.Can be used as one of the probe patterns in-situ corrosion research microscopes such as atomic force microscope strong supplementing, for the relevance research between Macrocosm and microcosm corrosion phenomenon, also can be used for the timely monitoring of long-term corrosion research.Yet, in laboratory, lack at present the electrolytic cell device of stereomicroscope in-situ corrosion morphology analysis special use.Some laboratories are reequiped voluntarily simple electrolytic cell or are replaced carrying out microexamination research with beaker, mainly have the following disadvantages:
1. easily pollute mirror body: for the ease of observing, adopting open-top receptacle to carry out in-situ corrosion is the most conventional way, but the volatilization of corrosive medium, splash very large to the infringement of microscope ocular; Be difficult to carry out the corrosion research work that has uniform temperature to require.
2. cannot realize with electro-chemical test and synchronizeing: open-top receptacle makes galvanochemistry three-electrode system be difficult to fix, and can not carry out electro-chemical test, can not be fine corresponding with electrochemical signals thereby erosion profile is changed, greatly hinder the announcement of corrosion mechanism.
3. pair liquid level smoothness requires high: stereomicroscope is that the liquid level of corrosive medium provides a light reflection surface undoubtedly by visible ray catoptric imaging, if liquid fluctuating or affected by bubble etc., judder and therefore distortion, is difficult to carry out CO
2, H
2experimental study under the ventilation test experiments of the corrosive gass such as S and corrosive medium agitation state.
Summary of the invention
In view of above-mentioned, utilize stereomicroscope to carry out electrolysis special pond in in-situ corrosion research experiment to have many deficiencies or shortcoming, the object of the invention is to provide a kind of electrolytic cell that stereomicroscope in-situ corrosion is analyzed that is exclusively used in.
Object of the present invention can realize by following measures:
An electrolytic cell of analyzing for stereomicroscope in-situ corrosion, is characterized in that electrolytic cell is made as cylindrical or rectangle, comprises cylindrical shell, cover, the cylinder end, connects the bolt at cover and the cylinder end; On cover, be provided with topping up cylinder, vent port, contrast electrode insert port from left to right by order, view window, to electrode connection terminal, working electrode joint; At the bottom of cylinder, middle part is provided with stirring magneton; Topping up cylinder vertically inserts the middle and lower part of cylindrical shell, and topping up cylinder upper end is provided with seal rubber plug, and seal rubber plug is provided with the draft tube of vertical insertion topping up cylinder bottom and is in the gas outlet of topping up cylinder upper end, and draft tube lower end is provided with aeration head; Exhausr port on cover is provided with plug, in contrast electrode insert port, is inserted with contrast electrode, in view window bottom surface, encircles on all covers and is provided with annular platinized platinum to electrode; Working electrode joint vertically inserts the top of cylindrical shell, in working electrode joint lower end, with bolt or snap ring, is fixed with the test sample that level is put.
On the surface of contact of cover and cylindrical shell and the cylinder end and cylindrical shell, be provided with separately annular groove, at the bottom of groove, be provided with sealing gasket.
The cylindrical shell of electrolytic cell, cover and the cylinder end, are made as the transparent body, and material is that plexiglas or quartz glass are made.
Electrolytic cell provided by the invention, its advantage is:
1. avoid mirror body pollution: owing to adopting closed structure, corrosive medium can directly or indirectly not contact with mirror body, view window and test piece close together, can meet most stereomicroscope in-situ corrosion analyses uses that free operating distance is greater than 50mm.
2. can realize under ventilation or stirring condition and corrode home position observation: the design of topping up is mainly that the factors such as liquid stirrings that ventilation is caused, bubble are limited within the scope of liquid in pipe, leans on bottom and pond Ti Nei UNICOM to realize the homogeneity of liquid property simultaneously.In experiment, be full of corrosive medium in the body of pond completely, vent port is guaranteed remnants
accompanying drawing explanation
Accompanying drawing is the structural representation for the electrolytic cell of stereomicroscope in-situ corrosion analysis
In figure, at the bottom of 1-cover 2-cylindrical shell 3-bolt 4-cylinder, 5-working electrode joint 6-stirs magneton 16-test sample 17-sealing gasket to electrode connection terminal 7-transparent windows 8-exhausr port rubber plug 9-escape pipe 10-draft tube 11-seal rubber plug 12-topping up cylinder 13-aeration head 14-contrast electrode insert port 15-
Embodiment
For further disclosing technical scheme of the present invention, below in conjunction with Figure of description, by embodiment, elaborate:
An electrolytic cell of analyzing for stereomicroscope in-situ corrosion, is characterized in that electrolytic cell is made as cylindrical or rectangle, comprises cylindrical shell, cover, the cylinder end, connects the bolt at cover and the cylinder end; On cover, be provided with topping up cylinder, vent port, contrast electrode insert port from left to right by order, view window, to electrode connection terminal, working electrode joint; At the bottom of cylinder, middle part is provided with stirring magneton; Topping up cylinder vertically inserts the middle and lower part of cylindrical shell, and topping up cylinder upper end is provided with seal rubber plug, and seal rubber plug is provided with the draft tube of vertical insertion topping up cylinder bottom and is in the gas outlet of topping up cylinder upper end, and draft tube lower end is provided with aeration head; Exhausr port on cover is provided with plug, in contrast electrode insert port, is inserted with contrast electrode, in view window bottom surface, encircles on all covers and is provided with annular platinized platinum to electrode; Working electrode joint vertically inserts the top of cylindrical shell, in working electrode joint lower end, with bolt or snap ring, is fixed with the test sample that level is put.
Specific experiment operation steps: outward winding fixedly cover 1, four bolts 3 at the cylinder end 4, cover 1, by transparent view window wiped clean, the test sample 16 use double nuts of the sheet of punching are in advance fixed on to the Ti Nei lower end, pond of working electrode 5, and use silica gel approved sample; The applicable stirring magneton 15 of size is put into electrolytic cell bottom; Cover 1 is covered, adjust after suitable and screw four set bolts 3, pond body is positioned near convenient operation position stereomicroscope.Take off seal rubber plug 11, open vent port 8, test solution is slowly injected by topping up pipe 12, until be full of electrolytic cell pond body, and with exhausr port rubber plug 8, close vent port 8 afterwards without bubble is residual, continue to inject again immediately a small amount of solution to the scale mark place that fluid tube indicates, seal rubber plug 11 and annex thereof installed, to liquid ventilation in the body of pond (as CO
2or H
2s etc.), gas is successively by after draft tube 10, aeration head 13, escape pipe 9, can with part solution hybrid reaction in the body of pond, start and stir magneton 15, after Aerated stirring certain hour, can guarantee that solution is even; The common contrast electrode of external is inserted to contrast electrode introducing port 14, with first with being connected to electrochemical workstation to the external connection of electrode 6, working electrode 5.By the eyepiece of view window 7 alignment body stereomicroscopes, adjust rear preparation and carry out experiment.Can synchronization gain galvanic corrosion signal and surface corrosion Morphology information by this device.
Claims (1)
1. an electrolytic cell of analyzing for stereomicroscope in-situ corrosion, is characterized in that electrolytic cell is made as cylindrical or rectangle, comprises cylindrical shell, cover, the cylinder end, connects the bolt at cover and the cylinder end; On cover, be provided with topping up cylinder, vent port, contrast electrode insert port from left to right by order, view window, to electrode connection terminal, working electrode joint; At the bottom of cylinder, middle part is provided with stirring magneton; Topping up cylinder vertically inserts the middle and lower part of cylindrical shell, and topping up cylinder upper end is provided with seal rubber plug, and seal rubber plug is provided with the draft tube of vertical insertion topping up cylinder bottom and is in the gas outlet of topping up cylinder upper end, and draft tube lower end is provided with aeration head; Exhausr port on cover is provided with plug, in contrast electrode insert port, is inserted with contrast electrode, in view window bottom surface, encircles on all covers and is provided with annular platinized platinum to electrode; Working electrode joint vertically inserts the top of cylindrical shell, in working electrode joint lower end, with bolt or snap ring, is fixed with the test sample that level is put; On the surface of contact of cover and cylindrical shell and on the surface of contact of the cylinder end and cylindrical shell, be provided with separately annular groove, at the bottom of groove, be provided with sealing gasket; The cylindrical shell of electrolytic cell, cover and the cylinder end, are made as the transparent body, of plexiglas, make.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210067093.0A CN102706935B (en) | 2012-03-05 | 2012-03-05 | Electrolytic cell for stereo microscope in-situ corrosion analysis |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210067093.0A CN102706935B (en) | 2012-03-05 | 2012-03-05 | Electrolytic cell for stereo microscope in-situ corrosion analysis |
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| CN102706935A CN102706935A (en) | 2012-10-03 |
| CN102706935B true CN102706935B (en) | 2014-07-16 |
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| CN105699285B (en) * | 2014-11-28 | 2019-08-02 | 中国石油天然气股份有限公司 | A kind of electrochemical appliance for the test of elementary sulfur underdeposit corrosion |
| CN104764780B (en) * | 2015-04-23 | 2018-02-06 | 合肥工业大学 | Battery for in-situ spectral analysis and use method and application thereof |
| CN108982344B (en) * | 2018-08-07 | 2021-02-26 | 中国石油大学(华东) | In-situ microscopic image scanning and collecting platform and method in electrochemical corrosion development process |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202676658U (en) * | 2012-04-30 | 2013-01-16 | 胜利油田胜利勘察设计研究院有限公司 | Electrolytic tank device for stereoscopic microscope and electrochemical testing in combination mode |
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| JPS58135947A (en) * | 1982-02-09 | 1983-08-12 | Mitsubishi Heavy Ind Ltd | Measurement of crystal particle size for steel pipe |
| JPH08211008A (en) * | 1995-02-03 | 1996-08-20 | Mitsubishi Heavy Ind Ltd | Method and device for measuring corrosion resistance |
| US5963040A (en) * | 1997-09-24 | 1999-10-05 | Taiwan Semiconductor Manufacturing Co. Ltd. | Method and apparatus for detecting pin-holes in a passivation layer |
| CN2758756Y (en) * | 2004-09-30 | 2006-02-15 | 中国海洋大学 | Observing bearing device of electrode for electrochemical corrosion experiment |
| CN2748906Y (en) * | 2004-09-30 | 2005-12-28 | 中国海洋大学 | Electrode for electrochemical corrosion experiment |
| CN201017692Y (en) * | 2007-03-06 | 2008-02-06 | 南开大学 | Real time monitoring system for manufacturing nano detecting probe with electrochemical corrosion |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN202676658U (en) * | 2012-04-30 | 2013-01-16 | 胜利油田胜利勘察设计研究院有限公司 | Electrolytic tank device for stereoscopic microscope and electrochemical testing in combination mode |
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Effective date of registration: 20190521 Address after: 257026 No. 49 Jinan Road, Dongying District, Dongying City, Shandong Province Patentee after: SINOPEC PETROLEUM ENGINEERING DESIGN CO., LTD. Address before: 257026 No. 49 Jinan Road, Dongying District, Dongying City, Shandong Province Patentee before: Shengli Oilfield Shengli Engineering & Consulting Co., Ltd. |