CN103308726A - Scanning electrochemical microscope experimental device for tests in various environments - Google Patents
Scanning electrochemical microscope experimental device for tests in various environments Download PDFInfo
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- CN103308726A CN103308726A CN2013102567464A CN201310256746A CN103308726A CN 103308726 A CN103308726 A CN 103308726A CN 2013102567464 A CN2013102567464 A CN 2013102567464A CN 201310256746 A CN201310256746 A CN 201310256746A CN 103308726 A CN103308726 A CN 103308726A
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Abstract
The invention provides an SECM (scanning electrochemical microscope) experimental device for tests in various environments. The SECM experimental device comprises a square glass shield, a gas inlet tube, an exhaust tube, a carrying plate with an electrolytic tank, a glass shield cover plate, a probe, a reference electrode, a counter electrode, a plastic cone, a probe support and rubber sealing rings. The integral square glass shield is formed by means of pouring and comprises a front side plate, a rear side plate, a left side plate and a right side plate which are identical, the carrying plate with the electrolytic tank is mounted at the bottom of the square glass shield, and the glass shield cover plate is placed on the upper portion of the glass shield. The plastic cone with the probe support is fixed into a circular hole of the rear side plate of the square glass shield, the top of the plastic cone can move in front-rear, left-right and up-down directions, and the probe support on the plastic cone can drive the probe to perform scanning and testing in different regions of a working electrode; gas can be injected onto the device via the gas inlet tube, and scanning electrochemical tests can be performed in environments with gas, mixed gas, gas and liquid interfaces and the like. The SECM experimental device is suitable for scanning electrochemical test research on metal materials in the various environments.
Description
Technical field:
The present invention relates to the scan-type electrochemical microscope experimental provision for test under the multiple environment (as liquid environment, gas-liquid coexisted environment etc.).
Background technology
Scan-type electrochemical microscope (SECM) is a kind of scanning probe microscopy technology that is proposed and grown up by A.J.Bard group the end of the eighties.It is based on electrochemical principle work, can measure material oxidation or the given electrochemical source of current that reduces in the microcell, can provide the topography and geomorphology of sample surfaces, can provide abundant chemical information again.
At present, chemistry or biologically active that scan-type electrochemical microscope (SECM) is used for the study sample surface distribute, the homogeneity of inferior unimolecular layer absorption, measure the speed of quick out-phase charge transfer, one-level or secondary are with the speed of afterreaction, the dynamics of enzyme-intermediate catalytic reaction, the diffusion of film intermediate ion, the dynamic process of solution/membrane interface and liquid/liquid interface, monomolecular detection, the imaging of enzyme and DNA (deoxyribonucleic acid), photosynthetic research, corrosion research, the measurement of chemically modified electrode thickness, the nanoscale etching, during electrochemical issues such as deposition and processing, what all adopt is the experimental provision that the scan-type electrochemical microscope workstation carries.But, along with deepening continuously and refinement of research, in experimentation, there is following shortcoming in this cover experimental provision that uses scan-type electrochemical microscope to carry: (1) can not carry out the scan-type electrochemical test experiments under gas or mixed-gas environment, especially simulate metal material in ground environment or specific environment for use, when having various mixed gases to exist, some material is to the electrochemical reaction process experimental study of metal material; (2) can't carry out scan-type electrochemical testing research, dynamics research etc. under the gas/liquid interface.Therefore, a kind of SECM experimental provision of testing down for multiple environment (as liquid environment, gas-liquid coexisted environment etc.) of research is very necessary.At present, at the problems referred to above and though improved SECM experimental provision can be realized the electro-chemical test research under the gaseous environment, but the probe of this experimental provision can not all around, movement up and down, therefore can not test out the electrochemical properties of working electrode zones of different, can not react working electrode each regional real topography in electrochemical reaction process, thereby limit the major function of improving preceding SECM experimental provision.For this reason, the present invention proposes a kind of SECM experimental provision for test under the multiple environment (as liquid environment, gas-liquid coexisted environment etc.), can address the above problem well.
Summary of the invention
The purpose of this invention is to provide a kind of SECM experimental provision for test under the multiple environment (as liquid environment, gas-liquid coexisted environment etc.), this device is simple, convenient, very easily satisfies the scan-type electrochemical experiment under the multiple different condition.
For achieving the above object, the present invention takes following technical scheme:
A kind of for the following SECM experimental provision of test of multiple environment (as liquid environment, gas-liquid coexisted environment etc.), mainly comprise: the support board of cubic cloche (supreme, bottom surface), draft tube, escape pipe, band electrolytic cell groove, cloche cover plate, probe, contrast electrode, to electrode, plastic cone body, probe support, rubber seal.Wherein plastic cone body top and probe support are fixed as one with sticking glutinous agent, and probe inserts in the terminal aperture of probe support during experiment; The four directions cloche is the integral body that forms by cast molding, comprises 4 the identical side plates in front, rear, left and right; The middle and upper part of back side panel has a circular hole that is complementary with the plastic cone body bottom dimensionally, the plastic cone body that the bottom is had O-ring seal snaps in this circular hole, again with sticking glutinous agent with itself and back side panel permanent fixation, the characteristic that utilize all around, plastic cone body top, moves up and down can drive probe by probe support and scan in the zones of different of working electrode, tests; The left plate middle and upper part links to each other with draft tube, seals with sticking glutinous agent, can change its length according to gas density; The upper right quarter of right plate links to each other with gas outlet, seal with sticking glutinous agent, in like manner can change its length according to gas density, in addition, the upper left quarter of right plate has small circular hole, probe, contrast electrode, the lead of electrode is linked to each other with the SECM potentiometer by small sircle hole, the remaining space of small sircle hole seals with fluid sealant; Support board four limits of band electrolytic cell groove such as all have at the groove of width, recess width is slightly larger than the thickness of cubic each side plate of cloche, in groove, place all rubber seal, the four directions cloche is installed in the groove that has rubber seal, with the support board permanent fixation of sticking glutinous agent with cubic cloche and band electrolytic cell groove; In like manner cloche cover plate four limits such as also have at the groove of width, recess width is slightly larger than the thickness of cubic each side plate of cloche, in groove, place all rubber seal, the cloche cover plate is stuck on each bar rib of cubic cloche tightly, the cloche cover plate can be dismantled as required, as the hermetic seal of need higher pressure, can around it, be coated with and spread fluid sealant.
Advantage of the present invention: utilize this device can either realize all functions of original SECM experimental provision, can realize the scan-type electrochemical test of (as liquid environment, gas-liquid coexistence, mixed gas and liquid coexisted environment etc.) under the multiple environment again; Under the environment that gas exists, can test out the electrochemical properties of working electrode zones of different, react the real topography of each zone in electrochemical reaction process of working electrode simultaneously.
Description of drawings
Fig. 1 is the synoptic diagram of apparatus of the present invention structure.
Fig. 2 is the synoptic diagram that the cloche back side panel is connected with plastic cone body.
Fig. 3 is the synoptic diagram of the support board of band electrolytic cell groove
Fig. 4 is the synoptic diagram of cloche cover plate
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in detail.
Referring to accompanying drawing, the present invention includes: supreme, the bottom surface of cubic cloche 17(), the support board 6 of draft tube 7, gas outlet 8, band electrolytic cell groove 11, cloche cover plate 5, probe 12, contrast electrode 13, to electrode 14, plastic cone body 18, probe support 19, round rubber O-ring seal 20, square rubber seal 21.Wherein the sticking glutinous agent of plastic cone body 18 tops and probe support 19 usefulness is fixed as one, and probe 12 is placed in the probe aperture 22 of probe support 19; Four directions cloche 17 is the integral body that forms by cast molding, comprises 4 the identical side plates in front, rear, left and right; The middle and upper part of back side panel 1 has a circular hole 9 that is complementary with plastic cone body 18 bottoms dimensionally, the plastic cone body 18 that the bottom is had rubber seal 20 snaps in the circular hole 9 of back side panel 1, again with sticking glutinous agent with itself and back side panel 1 permanent fixation, the characteristic that utilize all around, plastic cone body 18 top, moves up and down can drive probe 12 by probe support 19 and scan in the zones of different of working electrode 15, tests; Left plate 4 middle and upper parts link to each other with draft tube 7, seal with sticking glutinous agent, can change its length according to gas density, can feed the required gas with various of test by draft tube 7; The upper right quarter of right plate 3 links to each other with gas outlet 8, seal with sticking glutinous agent, in like manner can change its length according to gas density, can discharge all unwanted gases by gas outlet 8, in addition, the upper left quarter of right plate 3 has small sircle hole 10, probe 12, contrast electrode 13, the lead of electrode 14 is linked to each other with the SECM potentiometer by small sircle hole 10, and small sircle hole 10 remaining spaces seal with fluid sealant; Support board 6 four limits of band electrolytic cell groove 11 such as all have at the groove 16 of width, groove 16 width are slightly larger than the thickness of cubic cloche 17 each side plate, in groove 16, place all rubber seal 21, four directions cloche 17 is installed in the groove 16 that has rubber seal 21, with support board 6 permanent fixations of sticking glutinous agent with cubic cloche 17 and band electrolytic cell groove 11; In like manner cloche cover plate 5 four limits such as also have at the groove 16 of width, recess width is slightly larger than the thickness of cubic cloche 17 each side plate, in groove 16, place all rubber seal 21, cloche cover plate 5 is stuck on each bar rib of cubic cloche 17 tightly, cloche cover plate 5 can be dismantled as required, as the hermetic seal of need higher pressure, can around glass cover-plate 5, be coated with and spread fluid sealant.
As shown in Figure 1, the present invention carries out scan-type electrochemical when test under gaseous environment, at first open cloche cover plate 5, inserts required electrolytic solution and working electrode 15 in electrolytic cell groove 11, simultaneously probe 12 is adjusted at working electrode 15 near; Secondly cloche cover plate 5 tightly is stuck on each bar rib of cubic cloche 17; At last stand-by gas is passed in this device from draft tube 7, open gas outlet 8 simultaneously, till unwanted gas is drained only and is contained a certain amount of stand-by gas in device, simultaneously with probe 12, contrast electrode 13, electrode 14 is linked to each other with the SECM potentiometer by lead, the test of beginning scan-type electrochemical, come the position of traveling probe 12 in the test process by mobile plastic cone body 18, thereby the zones of different of working electrode 15 is scanned, tests.
Claims (1)
1. one kind is used for the scan-type electrochemical microscope experimental provision tested under the multiple environment, it is characterized in that this device comprises: support board (6), cloche cover plate (5), plastic cone body (18), probe support (19), the square rubber seal (21) of cubic cloche (17), draft tube (7), gas outlet (8), band electrolytic cell groove (11); The integral body that the four directions cloche is made up of front side board (2), back side panel (1), left plate (4), right plate (3); The groove (16) that the support board (6) of band electrolytic cell groove (11) and cloche cover plate 5 have by four limits, square rubber seal (21) and sticking glutinous agent and cubic cloche (17) link together and constitute this device, wherein support board (6) and cubic cloche (17) permanent fixation, cloche cover plate (5) can be dismantled as required; Plastic cone body (18) top and probe support (19) are fixed as one with sticking glutinous agent, and probe (12) is placed in the probe aperture (22) of probe support (19); The plastic cone body (18) of band probe support (19) is fixed in the circular hole (9) of back side panel (1), the characteristic that utilize plastic cone body (18) all around, top, moves up and down, probe support (19) can drive probe (12) and scan, test in the zones of different of working electrode (15); Left plate (4) middle and upper part links to each other with draft tube (7), can inject all gases in the SECM experimental provision by draft tube, can carry out the scan-type electrochemical testing research under the environment such as gas, mixed gas, liquid-gas interface; The upper right quarter of right plate (3) links to each other with gas outlet (8), the upper left quarter of right plate has small sircle hole (10), probe (12), contrast electrode (13), the lead of electrode (14) is linked to each other with the potentiometer of scan-type electrochemical microscope by small sircle hole (10), the interior remaining hole of small sircle hole (10) seals with fluid sealant.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310256746.4A CN103308726B (en) | 2013-06-26 | 2013-06-26 | Scanning electrochemical microscope experimental device for tests in various environments |
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| CN201310256746.4A CN103308726B (en) | 2013-06-26 | 2013-06-26 | Scanning electrochemical microscope experimental device for tests in various environments |
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| CN103308726B CN103308726B (en) | 2015-04-22 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104062324A (en) * | 2014-06-19 | 2014-09-24 | 中国船舶重工集团公司第七二五研究所 | Electrochemical detection device for scanning the appearance of local area |
| CN104391137A (en) * | 2014-11-28 | 2015-03-04 | 福州大学 | Novel electro-chemical imaging and temperature imaging synchronizing system for micro-cell |
| CN104502388A (en) * | 2014-11-19 | 2015-04-08 | 华中科技大学 | Photoelectrochemical kinetics test system and method based on scanning electrochemical microscope |
| CN105134199A (en) * | 2015-09-18 | 2015-12-09 | 西南石油大学 | Experimental device and method for simulating formation pore air-driven dynamic features |
| CN105353173A (en) * | 2015-12-10 | 2016-02-24 | 山东大学 | Electrolytic tank based on local electrochemical scanning probe research, and application of electrolytic tank |
| CN107677713A (en) * | 2017-11-06 | 2018-02-09 | 山东大学 | A kind of electrolytic cell and its application for Local electrochemical research |
| CN108693474A (en) * | 2018-03-02 | 2018-10-23 | 合肥国轩高科动力能源有限公司 | A kind of lithium battery device for detecting performance |
| CN109856115A (en) * | 2019-02-11 | 2019-06-07 | 南杰智汇(深圳)科技有限公司 | The device of in-situ test can be carried out to metal ion battery |
| CN115060776A (en) * | 2022-05-24 | 2022-09-16 | 广州大学 | Temperature-controllable scanning probe closed detection pool for biological cell detection and detection method |
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| US5202004A (en) * | 1989-12-20 | 1993-04-13 | Digital Instruments, Inc. | Scanning electrochemical microscopy |
| CN101403681A (en) * | 2008-11-15 | 2009-04-08 | 西北师范大学 | Current fitting curve sudden change elimination method for liquid/liquid interface scanning electro-chemical microscope |
| US20100306886A1 (en) * | 2009-05-29 | 2010-12-02 | Hitachi, Ltd. | Probe Microscope |
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2013
- 2013-06-26 CN CN201310256746.4A patent/CN103308726B/en not_active Expired - Fee Related
Patent Citations (3)
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| US5202004A (en) * | 1989-12-20 | 1993-04-13 | Digital Instruments, Inc. | Scanning electrochemical microscopy |
| CN101403681A (en) * | 2008-11-15 | 2009-04-08 | 西北师范大学 | Current fitting curve sudden change elimination method for liquid/liquid interface scanning electro-chemical microscope |
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Non-Patent Citations (1)
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| 尹其和: "《扫描电化学显微镜的基本原理与应用》", 《中山大学研究生学刊（自然科学、医学版）》, vol. 32, no. 2, 31 December 2011 (2011-12-31) * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104062324A (en) * | 2014-06-19 | 2014-09-24 | 中国船舶重工集团公司第七二五研究所 | Electrochemical detection device for scanning the appearance of local area |
| CN104062324B (en) * | 2014-06-19 | 2017-05-24 | 中国船舶重工集团公司第七二五研究所 | Electrochemical detection device for scanning the appearance of local area |
| CN104502388B (en) * | 2014-11-19 | 2017-02-22 | 华中科技大学 | Photoelectrochemical kinetics test system and method based on scanning electrochemical microscope |
| CN104502388A (en) * | 2014-11-19 | 2015-04-08 | 华中科技大学 | Photoelectrochemical kinetics test system and method based on scanning electrochemical microscope |
| CN104391137A (en) * | 2014-11-28 | 2015-03-04 | 福州大学 | Novel electro-chemical imaging and temperature imaging synchronizing system for micro-cell |
| CN104391137B (en) * | 2014-11-28 | 2017-01-25 | 福州大学 | Electro-chemical imaging and temperature imaging synchronizing system for micro-cell and method thereof |
| CN105134199A (en) * | 2015-09-18 | 2015-12-09 | 西南石油大学 | Experimental device and method for simulating formation pore air-driven dynamic features |
| CN105353173A (en) * | 2015-12-10 | 2016-02-24 | 山东大学 | Electrolytic tank based on local electrochemical scanning probe research, and application of electrolytic tank |
| CN107677713A (en) * | 2017-11-06 | 2018-02-09 | 山东大学 | A kind of electrolytic cell and its application for Local electrochemical research |
| CN108693474A (en) * | 2018-03-02 | 2018-10-23 | 合肥国轩高科动力能源有限公司 | A kind of lithium battery device for detecting performance |
| CN109856115A (en) * | 2019-02-11 | 2019-06-07 | 南杰智汇(深圳)科技有限公司 | The device of in-situ test can be carried out to metal ion battery |
| CN115060776A (en) * | 2022-05-24 | 2022-09-16 | 广州大学 | Temperature-controllable scanning probe closed detection pool for biological cell detection and detection method |
| CN115060776B (en) * | 2022-05-24 | 2023-06-16 | 广州大学 | Temperature-controllable scanning probe closed detection pool for biological cell detection and detection method |
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| CN103308726B (en) | 2015-04-22 |
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