CN204302186U - Electrochemical in-situ-Surface enhanced raman spectroscopy detection system - Google Patents
Electrochemical in-situ-Surface enhanced raman spectroscopy detection system Download PDFInfo
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- CN204302186U CN204302186U CN201420535977.9U CN201420535977U CN204302186U CN 204302186 U CN204302186 U CN 204302186U CN 201420535977 U CN201420535977 U CN 201420535977U CN 204302186 U CN204302186 U CN 204302186U
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Abstract
Electrochemical in-situ disclosed in the utility model-Surface enhanced raman spectroscopy detection system, this device comprises and is integrated with three electrode electrochemical in-situ-Surface enhanced raman spectroscopy chip, sample cell, electric signal breakout box and fixed station, sample cell is arranged at one end of the perform region at three welding tip places on electrochemical in-situ-Surface enhanced raman spectroscopy chip, the other end on chip is conducting end, conducting end is connected with electrochemical detector by electric signal breakout box, and chip is fixedly connected on fixed station.The utility model entirely eliminated easy-to-leak liquid problem in conventional detection devices, and structure is simple.The fixed station of chip enables detection chip keep horizontal checkout, improves the collection efficiency of scattered light as far as possible.The utility model integrated level is high, simplicity of design, and miniaturization is convenient to make, and can realize the quick detection of electrochemical in-situ-Surface enhanced raman spectroscopy.
Description
Technical field
The utility model relates to galvanochemistry and Raman spectrum combination analysis research field, particularly relates to a kind of electrochemical in-situ-Surface enhanced raman spectroscopy detection system.
Background technology
Original position EC-SERS is the combination analysis method of testing set up in conjunction with laser Raman spectrometer and electrochemical test system.Electrochemical workstation can provide the redox information of molecule under electric field action, and Raman spectrum can provide the group vibration information of molecule, therefore both combinations can be realized multiple application and research, as obtained the redox information of molecule on electrochemical solution interface, thus probe into electrochemical reaction mechanism; The preenrichment under electric field action can be carried out charge species, thus realize the detection etc. of trace molecules.At present, the electrochemical detector of existing miniaturization Raman spectrometer and standalone feature, corresponding EC-SERS coupling instrument is also just towards miniaturization.Develop the original position EC-SERS detection system that adapts with it and have very large application prospect in quick in situ analysis at the scene.
Traditional EC-SERS detection system generally adopts shaft-like plane electrode, roughening process is carried out by the surface of cyclic voltammetry to shaft-like plane gold or silver electrode, namely by carrying out continuous oxidation-reduction to gold, silver atom, make it form nano particle on surface, thus realize the SERS effect of molecule at electrode surface.Therefore, structure and the shape of corresponding in situ detection system generally design according to shaft-like plane electrode, because whole detection system is three-electrode system, also need to consider contrast electrode and the position to electrode.Consider from the angle of FT-Raman and confocal Raman instrument, laser is from up to down irradiated to working electrode surface, and Raman light is collected by eyepiece by scattering again.When therefore designing, working electrode need vertical place and electrode surface upward, conducting end faces up.Therefore working electrode certainly will need downward penetration-detection pond, and detection cell is liquid environment, therefore need to bottom detection cell and electrode stem intersection do Seal Design.If do not change commercially available general roofbolt shape electrode structure shape, smooth electrode stem surface just has with detecting device contact position the problem not easily sealed, namely easily there is the phenomenon of leakage, and Raman signal collection is generally repeatedly integration overlay model needs the regular hour, once leakage just can affect measurement result, cause result undesirable.In order to overcome this problem, the outward appearance of electrode is improved by existing company, namely at electrode periphery design screw thread and O-ring seal, agrees with, this kind of special special working electrode of method needs with screw socket bottom making its and detection cell.For traditional contrast electrode, owing to itself having certain weight, therefore place it in electrolytic cell side, the balance of whole detection cell will certainly be affected, cause liquid level to keep level, thus affect the collection efficiency of scattered light.So contrast electrode also needs particular design usually with to the size dimension of electrode and placement location.In addition, because detection system assembly is too many, when changing different solution to be measured, needing ceaselessly to dismantle electrode and O-ring seal to complete cleaning, operating comparatively loaded down with trivial details.
Utility model content
In order to overcome above-mentioned defect of the prior art, the present invention sets about improving from electrode, provides electrochemical in-situ-Surface enhanced raman spectroscopy detection system that a kind of integrated level is high, performance good, simple to operate, cost is low.
The present invention is a kind of electrochemical in-situ-Surface enhanced raman spectroscopy detection system, comprise and be integrated with three electrode electrochemical in-situ-Surface enhanced raman spectroscopy chip, sample cell, electric signal breakout box and fixed station, sample cell is arranged at one end of the perform region at three welding tip places on electrochemical in-situ-Surface enhanced raman spectroscopy chip, the other end on chip is conducting end, conducting end is connected with electrochemical detector by electric signal breakout box, and chip is fixedly connected on fixed station.Electrochemical in-situ-Surface enhanced raman spectroscopy chip comprises substrate, substrate is integrated with working electrode, to electrode and contrast electrode, wherein working electrode surface is porous nano dendritic structure, chip list surface layer be provided with conducting end, working electrode working end, to welding tip and contrast electrode working end, other superficial layer specific regions are insulation course, and the perform region at the conductive region at conducting end place and three welding tip places distinguishes by insulation course.
As preferably, the substrate of electrochemical in-situ-Surface enhanced raman spectroscopy chip is provided with Conductive silver ink printed layers, carbon printing ink printed layers and silver/AgCl ink printed layers, working electrode and be positioned at carbon printing ink printed layers to electrode, contrast electrode is positioned at silver/AgCl ink printed layers.Ag is proved to be the metal that can obtain now the enhancing of maximum Raman, therefore prepares electrochemical in-situ-Surface enhanced raman spectroscopy silver chip and has very large actual application value.
As preferably, sample cell pond body contacts with chip operation region, and sample cell pond body bottom area equals or slightly larger than the area in chip operation region, the testing sample liquid in sample cell contacted completely with three electrodes of perform region.
As preferably, the conducting end access electric transducer of electrochemical in-situ-Surface enhanced raman spectroscopy chip, electric transducer by connecing electrode cable, connect active conductors, connect contrast electrode wire and be connected with electrochemical detector.The conducting end of chip can arrange electrode conversion socket, and electric transducer is provided with the connector coordinated with it, the conducting end of chip is connected with electric transducer, and convenient operation person carries out detecting fast, easily.
As preferably, fixed station is provided with slot, and chip is arranged on fixed station by slot.Chip is fixed on fixed station, can make chip maintenance level in testing process, improve the collection efficiency of scattered light as far as possible.Insertion slot type fixed form simplicity of design and convenient operation.
First the utility model improves from the design of electrode, be integrated with working electrode, three-electrode system to electrode and contrast electrode, be an all-in-one-piece sheet electrodes, and working electrode makes it have certain electrochemical in-situ-Surface enhanced raman spectroscopy effect through special processing, achieve electrochemical in-situ-Surface enhanced raman spectroscopy measuring ability.Integrated by three electrodes, change the placement asymmetry problem that in traditional electrochemical in-situ-Surface enhanced raman spectroscopy detection system, column working electrode and contrast electrode need special customization and may bring.Meanwhile, by adding a cover sample cell at an upper portion thereof, entirely eliminated the easy-to-leak liquid problem in traditional electrochemical in-situ-Surface enhanced raman spectroscopy detection system.In addition, because this three electrode chips cost of manufacture is low, can single use, avoid loaded down with trivial details cleaning process.On the other hand, in order to easy to use and reduce costs, chip conductive end arranges plug receptacle, and wire can be drawn from plug receptacle, can be connected with electrochemical workstation very easily.The fixed station of chip enables detection chip keep horizontal checkout, improves the collection efficiency of scattered light as far as possible.This fixed station is designed to insertion slot type according to chip thickness.The utility model detection system integrated level is high, simplicity of design, and miniaturization is convenient to make, and can realize the quick detection of electrochemical in-situ-Surface enhanced raman spectroscopy.
Accompanying drawing explanation
Fig. 1 is the front view of the utility model structural representation;
Fig. 2 is the rear view of the utility model structural representation;
Fig. 3 is the structural representation of fixed station of the present utility model;
Fig. 4 is the structural representation of the utility model situ galvanochemistry-Surface enhanced raman spectroscopy chip.
Wherein: 1, fixed station; 2, sample cell; 3, sample application zone; 4, electrochemical in-situ-Surface enhanced raman spectroscopy detection chip; 5, electric signal breakout box; 6, contrast electrode wire is connect; 7, connect electrode cable; 8, working electrode wire is connect; 9, substrate; 10, insulation course; 11, contrast electrode; 12, to electrode; 13, working electrode; 14, slot.
Embodiment
The present embodiment provides a kind of electrochemical in-situ-Surface enhanced raman spectroscopy detection system, comprise and be integrated with three electrode electrochemical in-situ-Surface enhanced raman spectroscopy chip 4, sample cell 2, electric signal breakout box 5 and fixed station 1, sample cell 2 is arranged at one end of the perform region at three welding tip places on electrochemical in-situ-Surface enhanced raman spectroscopy chip 4, sample cell 2 is provided with sample application zone 3, the other end on chip is conducting end, conducting end is connected with electrochemical detector by electric signal breakout box 5, and chip is fixedly connected on fixed station 1.
Wherein electrochemical in-situ-Surface enhanced raman spectroscopy chip 4, comprises substrate 9, and substrate 9 is polyethylene terephthalate plate.Substrate 9 is provided with Conductive silver ink printed layers, carbon printing ink printed layers and silver/AgCl ink printed layers; Substrate 9 is integrated with working electrode 13, to electrode 12 and contrast electrode 11, working electrode 13 and carbon printing ink printed layers is positioned to electrode 12, contrast electrode 11 is positioned at silver/silver chloride electrically conductive ink printed layers; Wherein working electrode 13 surface is porous nano dendritic structure, and chip list surface layer is provided with conducting end, working electrode working end, to welding tip and contrast electrode working end, other superficial layer specific regions are insulation course.The perform region of the conductive region at conducting end place on chip with three welding tip places separates by insulation course.
Above-mentioned electrochemical in-situ-Surface enhanced raman spectroscopy chip adopts screen printing technique successively to print and forms, and at normal temperatures electrodeposit reaction process is carried out to it, specifically comprise following steps: (1) uses silk-screen printing technique, by the printing of Conductive silver ink layer on substrate, after being completed for printing, put into baking oven baking; Rear printing second layer carbon ink layer to be dried, and put into baking oven and again dry, obtained working electrode and to electrode; After this layer of solidification, printing silver/AgCl ink layer, and put into oven for drying, obtained contrast electrode; Rear printing ultra-violet curing insulating oil layer of ink to be dried, solidify under putting into uviol lamp, set time is 15 minutes.Set time can adjust according to the wavelength of uviol lamp and power.In order to increase the consistance of basic electrode, every one deck printing should be aimed at by cross mark.(2) this chip in step 1 is put into the electrolytic solution mixed by Ag2SO4, H2SO4 and water, carry out electrodeposit reaction, by controlling electric current and sedimentation time, common reduction precious metal ion and hydrogen ion under specific larger cathodic polarization electric current, make working electrode surface generate porous nano dendritic structure; By chip as dry in air or nitrogen; (3) the electrolyte residues matter on cleaning electrode surface.
Sample cell 2 pond body contacts with chip operation region, and sample cell pond body bottom area equals or slightly larger than the area in chip operation region, the testing sample liquid in sample cell 2 contacted completely with three electrodes of perform region.The conducting end of electrochemical in-situ-Surface enhanced raman spectroscopy chip arranges electricity conversion socket, electric signal breakout box is provided with the connector coordinated with it, the conducting end of chip is connected with electric signal breakout box, electric signal breakout box by connecing electrode cable 7, connect active conductors 8, connect contrast electrode wire 6 and be connected with electrochemical detector, convenient operation person carries out detecting fast, easily.
For specific testing sample, should first analyze its molecular structure, according to Raman choosing rule, determine whether it has Raman active group.Secondly analyze the Static and dynamic demand of determination data needed for it, directly measure or connect Dynamic Reaction Cell mensuration.Again, under investigating the change of the condition such as voltage, electric current, the Raman signal that testing sample produces at chip surface, and by inquiry handbook or theory calculate, analyze the strong peak position change in peak.Finally, as requested, study reaction mechanism or set up concrete detection method.
Claims (6)
1. electrochemical in-situ-Surface enhanced raman spectroscopy detection system, comprise and be integrated with three electrode electrochemical in-situ-Surface enhanced raman spectroscopy chip, sample cell, electric signal breakout box and fixed station, sample cell is arranged at one end of the perform region at three welding tip places on electrochemical in-situ-Surface enhanced raman spectroscopy chip, the other end on chip is conducting end, conducting end is connected with electrochemical detector by electric signal breakout box, and chip is fixedly connected on fixed station.
2. electrochemical in-situ according to claim 1-Surface enhanced raman spectroscopy detection system, it is characterized in that: electrochemical in-situ-Surface enhanced raman spectroscopy chip comprises substrate, substrate is integrated with working electrode, to electrode and contrast electrode, wherein working electrode surface is porous nano dendritic structure, chip list surface layer be provided with conducting end, working electrode working end, to welding tip and contrast electrode working end, other superficial layer specific regions are insulation course, and the perform region at the conductive region at conducting end place and three welding tip places distinguishes by insulation course.
3. electrochemical in-situ according to claim 2-Surface enhanced raman spectroscopy detection system, it is characterized in that: the substrate of electrochemical in-situ-Surface enhanced raman spectroscopy chip is provided with Conductive silver ink printed layers, carbon printing ink printed layers and silver/AgCl ink printed layers, working electrode and be positioned at carbon printing ink printed layers to electrode, contrast electrode is positioned at silver/AgCl ink printed layers.
4. electrochemical in-situ according to claim 1-Surface enhanced raman spectroscopy detection system, it is characterized in that: sample cell pond body contacts with chip operation region, sample cell pond body bottom area equals or slightly larger than the area in chip operation region, the testing sample liquid in sample cell is contacted completely with three electrodes of perform region.
5. electrochemical in-situ according to claim 1-Surface enhanced raman spectroscopy detection system, it is characterized in that: the conducting end of electrochemical in-situ-Surface enhanced raman spectroscopy chip access electric transducer, electric transducer by connecing electrode cable, connect active conductors, connect contrast electrode wire and be connected with electrochemical detector.
6. electrochemical in-situ according to claim 1-Surface enhanced raman spectroscopy detection system, it is characterized in that: fixed station is provided with slot, chip is arranged on fixed station by slot.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420535977.9U CN204302186U (en) | 2014-09-18 | 2014-09-18 | Electrochemical in-situ-Surface enhanced raman spectroscopy detection system |
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| CN201420535977.9U CN204302186U (en) | 2014-09-18 | 2014-09-18 | Electrochemical in-situ-Surface enhanced raman spectroscopy detection system |
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| CN204302186U true CN204302186U (en) | 2015-04-29 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104215624A (en) * | 2014-09-18 | 2014-12-17 | 浙江工业大学 | In-situ electrochemical-surface enhanced raman spectroscopy (EC-SERS) detection system and detection method thereof |
| TWI759776B (en) * | 2020-06-22 | 2022-04-01 | 淡江大學 | Detection substrate, raman spectrum detection system and raman spectrum detection method |
-
2014
- 2014-09-18 CN CN201420535977.9U patent/CN204302186U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104215624A (en) * | 2014-09-18 | 2014-12-17 | 浙江工业大学 | In-situ electrochemical-surface enhanced raman spectroscopy (EC-SERS) detection system and detection method thereof |
| TWI759776B (en) * | 2020-06-22 | 2022-04-01 | 淡江大學 | Detection substrate, raman spectrum detection system and raman spectrum detection method |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150429 Termination date: 20150918 |
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| EXPY | Termination of patent right or utility model |