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.