CN102706935A - Electrolytic cell for stereo microscope in-situ corrosion analysis - Google Patents

Electrolytic cell for stereo microscope in-situ corrosion analysis Download PDF

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Publication number
CN102706935A
CN102706935A CN2012100670930A CN201210067093A CN102706935A CN 102706935 A CN102706935 A CN 102706935A CN 2012100670930 A CN2012100670930 A CN 2012100670930A CN 201210067093 A CN201210067093 A CN 201210067093A CN 102706935 A CN102706935 A CN 102706935A
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China
Prior art keywords
tube
electrolytic cell
cover
cylinder
topping
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CN2012100670930A
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Chinese (zh)
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CN102706935B (en
Inventor
韩霞
张建
王增林
王子明
李清方
王田丽
管善峰
孙广领
黄少伟
张启阳
贾鹤年
王民
马梓涵
刘佳佳
曲虎
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Sinopec Petroleum Engineering Corp
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Shengli Oilfield Shengli Engineering & Consulting Co Ltd
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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

Be used for the electrolytic cell that the stereomicroscope in-situ corrosion is analyzed
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 is applicable to that the stereomicroscope in-situ corrosion is analyzed.
Background technology
Utilize stereomicroscope in-situ observation material surface erosion profile evolution process to have special advantages; As do not receive corrosive medium influence, simple to operate, image is undistorted etc.; Particularly along with the raising of stereomicroscope enlargement factor, this technology must obtain using more widely.Can be used as strong replenishing, be used for the relevance research between macroscopic view and the microcosmic corrosion phenomenon, also can be used for the timely monitoring of long-term corrosion research probe patterns in-situ corrosion research microscopes such as atomic force microscopes.Yet, lack the special-purpose electrolytic cell device of stereomicroscope in-situ corrosion morphology analysis at present in the laboratory.Some laboratories are reequiped simple electrolytic cell voluntarily or are replaced carrying out microexamination research with beaker, mainly have following weak point:
1. pollute the mirror body easily: 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, the adjust the telescope to one's eyes infringement of eyepiece of splashing are very big; Be difficult to carry out the corrosion research work that has uniform temperature to require.
2. can't realize with electro-chemical test synchronous: open-top receptacle makes the galvanochemistry three-electrode system be difficult to fix, and can not carry out electro-chemical test, thus make erosion profile change with electrochemical signals can not be fine corresponding, greatly hinder the announcement of corrosion mechanism.
3. the liquid level smoothness is required high: stereomicroscope is to lean on the visible light catoptric imaging, and the liquid level of corrosive medium provides a light reflection surface undoubtedly, if liquid fluctuating or influenced by bubble etc., judder and therefore distortion, is difficult to carry out CO 2, H 2Experimental study under the ventilation test experiments of corrosive gass such as S and the corrosive medium agitation state.
Summary of the invention
In view of the above-mentioned stereomicroscope that utilizes carries out that the electrolysis special pond exists many deficiencies or shortcoming in the in-situ corrosion research experiment, the object of the invention is to provide a kind of electrolytic cell that the stereomicroscope in-situ corrosion is analyzed that is exclusively used in.
The object of the invention can be realized through following measure:
A kind of electrolytic cell that is used for the analysis of stereomicroscope in-situ corrosion is characterized in that electrolytic cell is made as cylindrical or rectangle, comprises cylindrical shell, cover, the tube end, connects cover and the tube bolt at the end; On cover, be provided with topping up tube, vent port, contrast electrode insertion mouth by preface from left to right, view window is to electrode connection terminal, working electrode joint; The middle part is provided with the stirring magneton at the bottom of tube; The topping up tube vertically inserts the middle and lower part of cylindrical shell, and topping up tube upper end is provided with the sealing plug, and fluid sealant is provided with the draft tube and the gas outlet that is in topping up tube upper end of vertical insertion topping up tube bottom beyond the Great Wall, and the draft tube lower end is provided with aeration head; Exhausr port on the cover is provided with plug, inserts on the mouth at contrast electrode and is inserted with contrast electrode, on the cover in view window bottom surface ring week, is provided with annular platinized platinum to electrode; The working electrode joint vertically inserts the top of cylindrical shell, is fixed with the specimen that level is put in working electrode joint lower end with bolt or snap ring.
On the surface of contact of cover and the tube end and cylindrical shell, be provided with annular groove separately, be provided with sealing gasket at the bottom of the groove.
The cylindrical shell of electrolytic cell is made as the transparent body, and cover also can be transparent with the tube end, and material is that plexiglas or quartz glass are made.
Electrolytic cell provided by the invention, its advantage is:
1. avoid the mirror body pollution: owing to adopt closed structure, corrosive medium can directly or indirectly not contact with the mirror body, and view window and test piece close together can satisfy free operating distance and use greater than most stereomicroscope in-situ corrosion analyses of 50mm.
2. can realize corroding home position observation under ventilation or the stirring condition: the design of topping up mainly is that factors such as liquid stirrings that ventilation is caused, bubble are limited in the liquid in pipe scope, leans on the homogeneity of the interior UNICOM's realization liquid property of bottom and pond body simultaneously.In the experiment, be full of corrosive medium in the body of pond fully, vent port is guaranteed residual air or learning gas are got rid of, and the stirring of liquid in the body of pond will can not cause the formation of new reflecting interface like this.
Description of drawings
Accompanying drawing is the structural representation that is used for the electrolytic cell of stereomicroscope in-situ corrosion analysis
Among the figure at the bottom of the 1-cover 2-cylindrical shell 3-bolt 4-tube 5-working electrode joint 6-electrode connection terminal 7-transparent windows 8-exhausr port rubber plug 9-escape pipe 10-draft tube 11-sealing plug 12-topping up tube 13-aeration head 14-contrast electrode is inserted mouthful 15-stirs a magneton 16-specimen 17-sealing gasket
Embodiment
For further disclosing technical scheme of the present invention, elaborate through embodiment below in conjunction with Figure of description:
A kind of electrolytic cell that is used for the analysis of stereomicroscope in-situ corrosion is characterized in that electrolytic cell is made as cylindrical or rectangle, comprises cylindrical shell, cover, the tube end, connects cover and the tube bolt at the end; On cover, be provided with topping up tube, vent port, contrast electrode insertion mouth by preface from left to right, view window is to electrode connection terminal, working electrode joint; The middle part is provided with the stirring magneton at the bottom of tube; The topping up tube vertically inserts the middle and lower part of cylindrical shell, and topping up tube upper end is provided with the sealing plug, and fluid sealant is provided with the draft tube and the gas outlet that is in topping up tube upper end of vertical insertion topping up tube bottom beyond the Great Wall, and the draft tube lower end is provided with aeration head; Exhausr port on the cover is provided with plug, inserts on the mouth at contrast electrode and is inserted with contrast electrode, on the cover in view window bottom surface ring week, is provided with annular platinized platinum to electrode; The working electrode joint vertically inserts the top of cylindrical shell, is fixed with the specimen that level is put in working electrode joint lower end with bolt or snap ring.
Concrete experimental implementation step: outward winding fixedly cover 1, four bolts 3 at the tube end 4, cover 1 with transparent view window wiped clean, is fixed on the specimen 16 usefulness double nuts of the sheet of punching in advance the lower end in the pond body of working electrode 5, and uses the silica gel approved sample; The stirring magneton 15 that size is fit to is put into the electrolytic cell bottom; Cover 1 is covered, adjust four set bolts 3 of screwing after suitable, be convenient to operating position near the pond body is positioned over stereomicroscope.Take off sealing plug 11; Open vent port 8, test solution is slowly injected by topping up pipe 12, until being full of electrolytic cell pond body; And do not have the residual back of bubble and close vent port 8 with exhausr port rubber plug 8; Continue to inject the scale mark place that small volume of solution to fluid tube indicates immediately again, will seal plug 11 and annex thereof and install, to liquid ventilation in the body of pond (like CO 2Or H 2S etc.), gas is successively through after the 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, inflation can guarantee that solution is even after stirring certain hour; The common contrast electrode of external is inserted contrast electrode introducing port 14, with first with being connected to electrochemical workstation to the external connection of electrode 6, working electrode 5.With the eyepiece of view window 7 alignment body stereomicroscopes, adjust the back and prepare to carry out experiment.But develop information by this device synchronization gain galvanic corrosion signal and surface corrosion pattern.

Claims (3)

1. one kind is used for the electrolytic cell that the stereomicroscope in-situ corrosion is analyzed, and it is characterized in that electrolytic cell is made as cylindrical or rectangle, comprises cylindrical shell, cover, the tube end, connects cover and the tube bolt at the end; On cover, be provided with topping up tube, vent port, contrast electrode insertion mouth by preface from left to right, view window is to electrode connection terminal, working electrode joint; The middle part is provided with the stirring magneton at the bottom of tube; The topping up tube vertically inserts the middle and lower part of cylindrical shell, and topping up tube upper end is provided with the sealing plug, and fluid sealant is provided with the draft tube and the gas outlet that is in topping up tube upper end of vertical insertion topping up tube bottom beyond the Great Wall, and the draft tube lower end is provided with aeration head; Exhausr port on the cover is provided with plug, inserts on the mouth at contrast electrode and is inserted with contrast electrode, on the cover in view window bottom surface ring week, is provided with annular platinized platinum to electrode; The working electrode joint vertically inserts the top of cylindrical shell, is fixed with the specimen that level is put in working electrode joint lower end with bolt or snap ring.
2. according to claims 1 described electrolytic cell that is used for the analysis of stereomicroscope in-situ corrosion, it is characterized in that on the surface of contact of cover and the tube end and cylindrical shell, being provided with annular groove separately, be provided with sealing gasket at the bottom of the groove.
3. according to claims 1 described electrolytic cell that is used for the analysis of stereomicroscope in-situ corrosion, it is characterized in that the cylindrical shell of electrolytic cell is made as the transparent body, cover also can be transparent with a tube end, and material is that plexiglas or quartz glass are made.
CN201210067093.0A 2012-03-05 2012-03-05 Electrolytic cell for stereo microscope in-situ corrosion analysis Active CN102706935B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104764780A (en) * 2015-04-23 2015-07-08 合肥工业大学 Battery for in-situ spectral analysis and use method and application thereof
CN105699285A (en) * 2014-11-28 2016-06-22 中国石油天然气股份有限公司 An electrochemical device used for testing corrosion under elemental sulfur deposits
CN108982344A (en) * 2018-08-07 2018-12-11 中国石油大学(华东) Electrochemical corrosion development process original position micro-image scanning collection platform and method

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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
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CN2758756Y (en) * 2004-09-30 2006-02-15 中国海洋大学 Observing bearing device of 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
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
CN2748906Y (en) * 2004-09-30 2005-12-28 中国海洋大学 Electrode for electrochemical corrosion experiment
CN2758756Y (en) * 2004-09-30 2006-02-15 中国海洋大学 Observing bearing device of 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
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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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105699285A (en) * 2014-11-28 2016-06-22 中国石油天然气股份有限公司 An electrochemical device used for testing corrosion under elemental sulfur deposits
CN104764780A (en) * 2015-04-23 2015-07-08 合肥工业大学 Battery for in-situ spectral analysis and use method and application thereof
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
CN108982344A (en) * 2018-08-07 2018-12-11 中国石油大学(华东) Electrochemical corrosion development process original position micro-image scanning collection platform and method

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Address after: 257026 No. 49 Jinan Road, Dongying District, Dongying City, Shandong Province

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Address before: 257026 No. 49 Jinan Road, Dongying District, Dongying City, Shandong Province

Patentee before: Shengli Oilfield Shengli Engineering & Consulting Co., Ltd.