CN105353173A - Electrolytic tank based on local electrochemical scanning probe research, and application of electrolytic tank - Google Patents
Electrolytic tank based on local electrochemical scanning probe research, and application of electrolytic tank Download PDFInfo
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- CN105353173A CN105353173A CN201510916724.5A CN201510916724A CN105353173A CN 105353173 A CN105353173 A CN 105353173A CN 201510916724 A CN201510916724 A CN 201510916724A CN 105353173 A CN105353173 A CN 105353173A
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Abstract
The invention discloses an electrolytic tank based on local electrochemical scanning probe research, and the electrolytic tank comprises an electrolytic tank cavity and a side wall forming the electrolytic tank cavity through enclosing. The front part of the side wall is provided with an observation window, and the left and right parts of the side wall are respectively provided with a first circular hole and a second circular hole in a vertical and embedded manner, wherein the first and second circular holes are respectively communicated with the electrolytic tank cavity. The bottom of the electrolytic tank cavity is provided with a fixing device which is used for fixing a to-be-detected sample. The bottom of the electrolytic tank is provided with the fixing device, thereby achieving the fixing of the to-be-detected sample. Meanwhile, the to-be-detected sample is observed through the observation window, and the auxiliary adjustment of the distance between a probe and the surface of the to-be-detected sample is monitored through a CCD. The electrolytic tank gives consideration to the structure and function of the electrolytic tank and the type of a related sample. The electrolytic tank can be used for the local electrochemical scanning probe research.
Description
Technical field
The present invention relates to a kind of electrolytic cell based on the research of Local electrochemical scan-probe and application thereof, belong to the technical field of electrochemical cell.
Background technology
At present, be generally used for the electrolytic cell that Local electrochemical is measured, the material workplace that is applicable to conduct a research is the situation of column (as metal bar) xsect or plate surface.But taking into account in electrolyser construction, function and relevant specimen types thereof, these electrolytic cells still have some limitations.
Chinese patent CN102928625A discloses a kind of scan-type electrochemical microscope electrolytic cell for the corrosion research of tabular load sample, this electrolytic cell comprises the superstructure and substructure that surround electrolysis vallecular cavity: the central authorities of substructure are provided with groove, described superstructure comprises rectangular frame, front side wall in rectangular frame is transparent material, the left side wall in rectangular frame with right side wall is respectively arranged with the groove be communicated with in extraneous and electrolytic tank.This invention makes plate tensile sample be horizontally through the structure of electrolytic tank, is especially suitable for the corrosion experiment research of the metal material sample being in stress load or there is unrelieved stress.But this patent of invention is unsuitable for research club-shaped material bottom surface (i.e. workplace).
Chinese patent CN102183678A discloses a kind of Multifunctional electrolysis pond for scan-type electrochemical microscope, the screw thread II that the upper cover that this electrolytic cell comprises in spill, inner side is provided with screw thread I and lower cover and two end band and described screw thread I match and the double-layered cylinder of in-built electrolyte solution.This invention is by the different structure of lower cover, and can complete the experiment of three-electrode system, four electrode systems and complex system, it is easy to operate, improves Efficiency.But the weak point of this patent of invention is: the electrolytic cell involved by (1) attaches the double-layered cylinder that holds electrolyte solution, complicated structure; (2) electrolytic cell is columnar structured, effectively cannot be focused on carry out auxiliary monitoring to probe and base electrode spacing by side-looking window.
Summary of the invention
For existing technical deficiency, the invention provides a kind of electrolytic cell based on the research of Local electrochemical scan-probe.
The present invention also provides a kind of application process of above-mentioned electrolytic cell.
The present invention a kind ofly takes into account electrolyser construction, function and relevant specimen types thereof, can be used for the electrolytic cell of Local electrochemical scan-probe research.The present invention also provides a kind of and utilizes above-mentioned electrolytic cell to carry out the experimental technique of corrosion electrochemistry research to column test button.
Technical scheme of the present invention is as follows:
A kind of electrolytic cell based on the research of Local electrochemical scan-probe, comprise electrolytic cell vallecular cavity and the sidewall surrounding described electrolytic cell vallecular cavity, the front portion of described sidewall is provided with view window, and left part and the right part of described sidewall are vertically embedded with the first circular hole and the second circular hole that are connected with described electrolytic cell vallecular cavity respectively; The bottom of described electrolytic cell vallecular cavity is provided with the stationary installation for fixing sample to be tested.
Preferred according to the present invention, described first circular hole is consistent with the degree of depth of described electrolytic cell vallecular cavity with the height of the second circular hole.
Preferred according to the present invention, described first circular hole is communicated with electrolytic cell vallecular cavity respectively by the rectangular channel arranged in described sidewall with the second circular hole.
Preferred according to the present invention, the external dimensions of described electrolytic cell is as follows, length range: 55-60mm, width range: 55-60mm, altitude range: 55-60mm.
Preferred according to the present invention, the size of described electrolytic cell vallecular cavity is as follows, length range: 35-40mm, width range: 35-40mm, altitude range: 45-50mm.
Preferred according to the present invention, described stationary installation is be arranged on the groove bottom described electrolytic cell vallecular cavity, and preferably, described groove is cylindrical.
Preferred according to the present invention, the size of described columniform groove is as follows, diameter range: 4-5mm.
Preferred according to the present invention, the diameter of described first circular hole and the second circular hole is respectively 5-6mm.
Preferred according to the present invention, the size of the xsect of described rectangular channel is as follows: width range: 4-5mm, altitude range: 10-15mm.
Preferred according to the present invention, described view window is organic glass material, thickness range: 2-3mm.The view window of organic glass material of the present invention utilizes the auxiliary monitoring of CCD enforcement to distance adjustment between scan-type electrochemical probe and matrix working electrode.
One utilizes above-mentioned electrolytic cell to test button bottom surface, i.e. workplace, carries out the method for corrosion experiment, comprises step as follows:
1) prepare and the suitable test button of electrolytic cell vallecular cavity base fixture size;
2) installation of sample and electrode:
Be fixed on bottom described electrolytic cell vallecular cavity by described test button by described stationary installation, only exposed described test button bottom surface flushes with bottom described electrolytic cell vallecular cavity;
In described first circular hole and the second circular hole, contrast electrode and auxiliary electrode are installed respectively;
3) install, regulate probe: stationary probe on X-Y-Z three-dimensional position sensing device, regulated by position transducer and make described probe near described test button bottom surface, the distance between monitoring probe and test button bottom surface;
4) in described electrolytic cell groove, electrolyte solution is added;
5) described probe, test button, contrast electrode are connected with double potentiostat respectively with auxiliary electrode, carry out Experiment in Erosive Electrochemistry measurement.
The invention has the advantages that:
The bottom of a kind of electrolytic cell based on the research of Local electrochemical scan-probe of the present invention arranges stationary installation and realizes being fixed sample to be tested, window observation is carried out to sample to be tested simultaneously, and the auxiliary adjustment of the spacing of probe and specimen surface is monitored by CCD, system of the present invention is a kind of takes into account electrolyser construction, function and relevant specimen types (geometric configuration) thereof, can be used for the electrolytic cell of Local electrochemical scan-probe research.
Accompanying drawing explanation
The vertical view of Fig. 1 electrolytic cell of the present invention;
In FIG, 1, electrolytic cell vallecular cavity; 2, sidewall; 3, view window; 4, the first circular hole; 5, the second circular hole; 6, stationary installation; 7, rectangular channel.
Embodiment
Below in conjunction with embodiment and Figure of description, the present invention is described in detail, but is not limited thereto.
Embodiment 1,
A kind of electrolytic cell based on the research of Local electrochemical scan-probe, comprise electrolytic cell vallecular cavity 1 and the sidewall 2 surrounding described electrolytic cell vallecular cavity 1, the front portion of described sidewall 2 is provided with view window 3, and left part and the right part of described sidewall 2 are vertically embedded with the first circular hole 4 and the second circular hole 5 be connected with described electrolytic cell vallecular cavity respectively; The bottom of described electrolytic cell vallecular cavity 1 is provided with the stationary installation 6 for fixing sample to be tested.
Described view window 3 is organic glass material, thickness range: 2-3mm.
Embodiment 2,
As described in Example 1 based on an electrolytic cell for Local electrochemical scan-probe research, its difference is, described first circular hole 4 is consistent with the degree of depth of described electrolytic cell vallecular cavity 1 with the height of the second circular hole 5.
Embodiment 3,
A kind of electrolytic cell based on the research of Local electrochemical scan-probe as described in embodiment 1,2, its difference is, described first circular hole 4 is communicated with electrolytic cell vallecular cavity 1 respectively by the rectangular channel 7 arranged in described sidewall 2 with the second circular hole 5.The size of the xsect of described rectangular channel 7 is as follows: width range: 4-5mm, altitude range: 10-15mm.
Embodiment 4,
A kind of electrolytic cell based on the research of Local electrochemical scan-probe as described in embodiment 1,2,3, its difference is, the external dimensions of described electrolytic cell is as follows, length range: 55-60mm, width range: 55-60mm, altitude range: 55-60mm.
The size of described electrolytic cell vallecular cavity 1 is as follows, length range: 35-40mm, width range: 35-40mm, altitude range: 45-50mm.
Embodiment 5,
A kind of electrolytic cell based on the research of Local electrochemical scan-probe as described in embodiment 1,2,3,4, its difference is, described stationary installation 6 is for being arranged on the groove bottom described electrolytic cell vallecular cavity 1, and preferably, described groove is cylindrical.
Embodiment 6,
As described in Example 5 based on an electrolytic cell for Local electrochemical scan-probe research, its difference is, the size of described columniform groove is as follows, diameter range: 4-5mm.
Embodiment 7,
A kind of electrolytic cell based on the research of Local electrochemical scan-probe as described in embodiment 1-6, its difference is, the diameter of described first circular hole 4 and the second circular hole 5 is respectively 5-6mm.
Embodiment 8,
A kind of utilization electrolytic cell as described in embodiment 1-7, to test button bottom surface, i.e. workplace, carries out the method for corrosion experiment, comprises step as follows:
1) prepare and the suitable test button of electrolytic cell vallecular cavity base fixture size;
2) installation of sample and electrode:
Be fixed on bottom described electrolytic cell vallecular cavity by described test button by described stationary installation, only exposed described test button bottom surface flushes with bottom described electrolytic cell vallecular cavity;
In described first circular hole and the second circular hole, contrast electrode and auxiliary electrode are installed respectively;
3) install, regulate probe: stationary probe on X-Y-Z three-dimensional position sensing device, regulated by position transducer and make described probe near described test button bottom surface, the distance between monitoring probe and test button bottom surface;
4) in described electrolytic cell groove, electrolyte solution is added;
5) described probe, test button, contrast electrode are connected with double potentiostat respectively with auxiliary electrode, carry out Experiment in Erosive Electrochemistry measurement.
Application examples as embodiment 8:
Described test button is column 304 stainless steel sample, in step 1) need to process column 304 stainless steel sample before: with 800
#with 1000
#abrasive paper for metallograph is polished step by step, polishing sample bottom surface and periphery to bright in mirror surface, rinse surface with high purity water, drying for standby; Described contrast electrode selects saturated calomel electrode (SCE); Described auxiliary electrode is Pt silk; In step 4) in the electrolyte solution that adds be the NaCl solution of volumetric molar concentration 0.1mol/L; In step 5) in, probe, cylindrical metal sample, contrast electrode and auxiliary electrode are connected with the double potentiostat of SECM270 type scan-type electrochemical microscope respectively, utilize the Local electrochemical testing software installed on computers to carry out Experiment in Erosive Electrochemistry measurement.
Claims (10)
1. the electrolytic cell based on the research of Local electrochemical scan-probe, it is characterized in that, this electrolytic cell comprises electrolytic cell vallecular cavity and surrounds the sidewall of described electrolytic cell vallecular cavity, the front portion of described sidewall is provided with view window, and left part and the right part of described sidewall are vertically embedded with the first circular hole and the second circular hole that are connected with described electrolytic cell vallecular cavity respectively; The bottom of described electrolytic cell vallecular cavity is provided with the stationary installation for fixing sample to be tested.
2. a kind of electrolytic cell based on the research of Local electrochemical scan-probe according to claim 1, it is characterized in that, described first circular hole is consistent with the degree of depth of described electrolytic cell vallecular cavity with the height of the second circular hole.
3. a kind of electrolytic cell based on the research of Local electrochemical scan-probe according to claim 1, it is characterized in that, described first circular hole is communicated with electrolytic cell vallecular cavity respectively by the rectangular channel arranged in described sidewall with the second circular hole.
4. a kind of electrolytic cell based on the research of Local electrochemical scan-probe according to claim 1, it is characterized in that, the external dimensions of described electrolytic cell is as follows, length range: 55-60mm, width range: 55-60mm, altitude range: 55-60mm.
5. a kind of electrolytic cell based on the research of Local electrochemical scan-probe according to claim 1, it is characterized in that, the size of described electrolytic cell vallecular cavity is as follows, length range: 35-40mm, width range: 35-40mm, altitude range: 45-50mm.
6. a kind of electrolytic cell based on the research of Local electrochemical scan-probe according to claim 1, it is characterized in that, described stationary installation is be arranged on the groove bottom described electrolytic cell vallecular cavity, and preferably, described groove is cylindrical.
7. a kind of electrolytic cell based on the research of Local electrochemical scan-probe according to claim 6, it is characterized in that, the size of described columniform groove is as follows, diameter range: 4-5mm.
8. a kind of electrolytic cell based on the research of Local electrochemical scan-probe according to claim 1, it is characterized in that, the diameter of described first circular hole and the second circular hole is respectively 5-6mm; The size of the xsect of described rectangular channel is as follows: width range: 4-5mm, altitude range: 10-15mm.
9. a kind of electrolytic cell based on the research of Local electrochemical scan-probe according to claim 1, it is characterized in that, described view window is organic glass material, thickness range: 2-3mm.
10. utilize electrolytic cell as described in claim 1-9 any one test button bottom surface to be carried out to a method for corrosion experiment, it is characterized in that, it is as follows that the method comprising the steps of:
1) prepare and the suitable test button of electrolytic cell vallecular cavity base fixture size;
2) installation of sample and electrode:
Be fixed on bottom described electrolytic cell vallecular cavity by described test button by described stationary installation, only exposed described test button bottom surface flushes with bottom described electrolytic cell vallecular cavity;
In described first circular hole and the second circular hole, contrast electrode and auxiliary electrode are installed respectively;
3) install, regulate probe: stationary probe on X-Y-Z three-dimensional position sensing device, regulated by position transducer and make described probe near described test button bottom surface, the distance between monitoring probe and test button bottom surface;
4) in described electrolytic cell groove, electrolyte solution is added;
5) described probe, test button, contrast electrode are connected with double potentiostat respectively with auxiliary electrode, carry out Experiment in Erosive Electrochemistry measurement.
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Cited By (3)
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CN106525929A (en) * | 2016-12-02 | 2017-03-22 | 山东大学 | Electrolytic bath suitable for electrochemical test and sample surface analysis, and application thereof |
CN107677713A (en) * | 2017-11-06 | 2018-02-09 | 山东大学 | A kind of electrolytic cell and its application for Local electrochemical research |
CN109270137A (en) * | 2018-11-02 | 2019-01-25 | 西南石油大学 | It is a kind of to test scan-type electrochemical microscope sample stage of more gauge coupons with electrolytic cell |
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CN102183678A (en) * | 2010-12-13 | 2011-09-14 | 西北师范大学 | Multifunctional electrolytic tank for scanning electrochemical microscope |
CN102928625A (en) * | 2012-10-22 | 2013-02-13 | 山东大学 | Scanning electrochemical microscope electrolytic cell for plate-shaped load sample corrosion research and application thereof |
CN103235158A (en) * | 2013-01-10 | 2013-08-07 | 北京航空航天大学 | Electrochemical atomic force microscope probe carriage-electrolytic cell device |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106525929A (en) * | 2016-12-02 | 2017-03-22 | 山东大学 | Electrolytic bath suitable for electrochemical test and sample surface analysis, and application thereof |
CN107677713A (en) * | 2017-11-06 | 2018-02-09 | 山东大学 | A kind of electrolytic cell and its application for Local electrochemical research |
CN109270137A (en) * | 2018-11-02 | 2019-01-25 | 西南石油大学 | It is a kind of to test scan-type electrochemical microscope sample stage of more gauge coupons with electrolytic cell |
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