CN101131351A - Inside and outside reflection-switchable surface infrared spectrum pool device - Google Patents
Inside and outside reflection-switchable surface infrared spectrum pool device Download PDFInfo
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- CN101131351A CN101131351A CN 200710044251 CN200710044251A CN101131351A CN 101131351 A CN101131351 A CN 101131351A CN 200710044251 CN200710044251 CN 200710044251 CN 200710044251 A CN200710044251 A CN 200710044251A CN 101131351 A CN101131351 A CN 101131351A
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Abstract
The invention belongs to infrared spectroscopy technical field; specifically a surface infrared spectroscopy device that internal and outer reflection can be switched. The spectroscopy device was composed of internal reflected mode coupling electrode or outer reflected mode working electrode, the reference electrode, outer reflected mode-coupling electrode, electrolytic bath, internal reflected mode silicon semi-cylindrical infrared window or outer reflected mode calcium fluoride semi-cylindrical infrared window. The internal reflected mode coupling electrode or outer reflected mode working electrode, the reference electrode, outer reflected mode-coupling electrode comprises the three-electrode system placed in the electrolytic bath, internal reflected mode silicon infrared window or outer reflected mode calcium fluoride infrared window was placed under the electrolytic bath. The surface infrared spectroscopy device presented by this invention can be used to in internal reflected mode and outer reflected mode, convenient to switch. This device can be used to detect electrochemical real-time infrared spectroscopy signals, simple in structure, stable, convenient and easy to operate.
Description
Technical field
The invention belongs to the infrared spectrum technology field, be specifically related to a kind of surface infrared spectrum pool device, can be applicable to the electrochemical surface infrared spectroscopic study, also can be used for the assessment of the outer absorption effect of surface red.
Background technology
The electrochemical surface science is the forward position crossing domain of current galvanochemistry and surface chemistry research.The Application of Technology such as various high sensitivity and specific on-the-spot spectrum, scanning microprobe and crystal microbalance and development have promoted the application and the development of electrochemical surface science.In the on-the-spot spectral investigation method of electrode surface, surface infrared spectrum
[1]Be to remove Surface enhanced raman spectroscopy
[2]Outer another kind provides the important tools of analysis of electrode interface molecular structure information.Surface infrared spectrum has two kinds of patterns usually: internal reflected mode (ATR-FTIR) and external reflection pattern (IR-RAS).
The ATR-FTIR pattern need cover the conductive metal nanometer thin film of one deck as working electrode on infrared window, ATR-FTIR has that solution resistance is little, potential response is fast; The solution resistance to mass tranfer is little; Distribution of current is even; Can detect advantages such as ADSORPTION STATE species.The IR-RAS pattern has type of electrodes and can be metal all kinds of body electrodes such as (containing monocrystalline and polycrystalline), also can electroplate another layer nanometer metallic film on this basis; IR-RAS can detect solution mutually and ADSORPTION STATE species and can realize following the tracks of advantages such as the reaction mechanism mechanism of reaction, detection reaction intermediate.If the coupling of inside and outside reflection infrared spectrum technology can be provided the information of more relevant reaction mechanisms etc.Present two kinds of patterns can only be used separately, promptly need different light path systems and electrolytic cell device separately, thereby are difficult for realizing easy conversion between internal reflected mode and the external reflection pattern.Be pointed out that simultaneously, because the employing of nano structure membrane, so-called surface in surface infrared spectrum, can occur and strengthen the infrared absorption effect, to its reasonable assessment often need to adopt same light path by on the contrast nano thin-film with base metal on absorption infrared signal size, also shown the necessity of the switchable surface infrared spectrum accessory system of design inside and outside reflection especially.
The present invention proposes a kind of novel surface infrared spectrum cell system, and this system is simple, and promptly internal reflection technique is utilized identical light path system and spectrum tool device with the external reflection technology, can realize easy conversion between internal reflected mode and the external reflection pattern.
1.M.Osawa，In?Handbook?of?Vibrational?Spectroscopy；Chalmers?J.M.，Griffiths，P.R.，Eds.；John?Wiley&Sons：Chichester，UK，2002；Vol.1，p.785.
2.Z.-Q.Tian，B.Ren，D.-Y.Wu，J.Phys.Chem.B2002，106.9467(feature?article)
3.S.-G.Sun，In?Catalysis?and?Electrocatalysis?at?Nanoparticle?Surfaces；Wieckowski，A.，Savinova，E.R.，Vayenas，C.G.，Eds.；Marcel?Dekker：New?York，2003；Chapter?21.
Summary of the invention
The objective of the invention is to propose a kind of surface infrared spectrum pool device of novel inside and outside reflection unification, require this device simple, can easy realization internal reflected mode and the external reflection pattern between change.
The surface infrared spectrum pool device that the present invention proposes, its structure as shown in Figure 1, this spectral device is made up of electrode (platinized platinum) 3, electrolytic cell 4, internal reflected mode silicon semicolumn infrared window or external reflection pattern calcium fluoride semicolumn infrared window 5 electrode (platinized platinum) or external reflection pattern working electrode (body electrode) 1, contrast electrode (saturated calomel electrode or reversible hydrogen electrode) 2, external reflection pattern internal reflected mode.Wherein, internal reflected mode is formed three-electrode system to electrode or external reflection pattern working electrode 1, contrast electrode 2 and external reflection pattern to electrode 3, place electrolytic cell 4, internal reflected mode silicon infrared window or external reflection pattern calcium fluoride infrared window are positioned at electrolytic cell 4 bottoms.The diameter of external reflection working electrode is 8mm～12mm, and the diameter of silicon semicolumn or calcium fluoride semicolumn is 15-25mm, and height is 20-26mm.
The novel surface infrared spectrum cell system that the present invention proposes can be used for internal reflected mode, can be used for the external reflection pattern again, the convenient conversion that realizes between the inside and outside reflection.This device can be in order to the detection electrochemical real-time infrared spectroscopy signals, and simple and stable structure is convenient and easy.
Description of drawings
Below in conjunction with accompanying drawing and instantiation this novel surface infrared spectrum cell system is further specified.
Fig. 1 is this novel surface infrared spectrum optical device structural representation.
Fig. 2 is an example light spectrogram of internal reflected mode in this device.
Fig. 3 is another example of internal reflected mode in this device.
Fig. 4 is corresponding diagram 3 electric currents and vCO
L, vOH and vCO
BIntegrated intensity is with electrode potential variation relation figure.
Fig. 5 is an example light spectrogram of this device China and foreign countries reflective-mode.
Fig. 6 is another example of this device China and foreign countries reflective-mode.
Fig. 7 is corresponding diagram 6 electric currents and vCO
LAnd vCO
2Integrated intensity is with electrode potential variation relation figure.
Number in the figure: 1 is that internal reflected mode is to electrode or external reflection pattern working electrode; 2 is contrast electrode; 3 is that the external reflection pattern is to electrode; 4 is electrolytic cell; 5 is internal reflected mode silicon infrared window or external reflection calcium fluoride infrared window.
Embodiment
This device concrete structure is mainly by electrolytic cell, contrast electrode, form electrode, silicon semicolumn (internal reflected mode) and calcium fluoride semicolumn (external reflection pattern).The diameter of silicon semicolumn and calcium fluoride semicolumn is 20mm, and height is 25mm.Concrete preparation process is as follows, (1) internal reflected mode:
1. gold nano film on the silicon chip surface electroless plating at first, then on the electroplating surface of gold nano film the platinum film layer as working electrode.2. the platinum film electrode surface covers and goes up silicon rubber loop, in case electrolyte is excessive, and in the electrolytic cell of packing into.3. be inserted in the electrolytic cell with contrast electrode with to electrode, this has just formed the three-electrode system of galvanochemistry spectrum test.
(2) external reflection pattern:
1. at first on golden body electrode surface is electroplated fine and close platinum film layer as working electrode.2. the calcium fluoride semi-cylinder surface covers and goes up silicon rubber loop, in the electrolytic cell of packing into, and makes working electrode be close to the calcium fluoride plane.3. be inserted in the electrolytic cell with contrast electrode with to electrode, this has just formed the three-electrode system of galvanochemistry spectrum test.
Fig. 2 be in the internal reflected mode Pt electrode at the saturated 0.1M HClO of CO
4Surface infrared spectrum figure in the solution, sample spectra is adopted in-0.2V (vs.SCE), and reference spectrum is adopted in 0.8V.This device has detected the signal (2072cm that is adsorbed on Pt surface C O
-1, vCO
L1854cm
-1, vCO
B), also detected the signal (3663cm of common planar water simultaneously
-1, vOH; 1629cm
-1, δ HOH).
Fig. 3 be in the internal reflected mode Pt electrode at the saturated 0.1MHClO of CO
4Dynamics infrared spectrogram in the solution, reference spectrum is adopted in 0.9V, and the temporal resolution of spectra collection is 0.175s, and electric potential scanning speed is 50mV/s.
Fig. 4 be in the corresponding diagram 3 the Pt electrode at the saturated 0.1MHClO of CO
4(solid line) and 0.1MHClO in the solution
4(dotted line) electric current and vCO in the solution
L, vOH and vCO
BIntegrated intensity is with electrode potential variation relation figure.VCO
L, vOH and vCO
BIntegrated intensity is along with CO little by little dies down in the oxidation on Pt surface.
Fig. 5 be in the external reflection pattern Pt electrode at the saturated 0.1MHClO of CO
4Infrared spectrogram in the solution, sample spectra are adopted in-0.2V (vs.SCE), and reference spectrum is adopted in 0.8V.This device has detected the signal (2066cm that is adsorbed on Pt surface C O
-1, vCO
L), also detected CO oxidation product CO simultaneously
2Signal (2344cm
-1, vCO
2).
The Pt electrode is at the saturated 0.1MHClO of CO in Fig. 6 external reflection pattern
4Dynamics infrared spectrogram in the solution, reference spectrum is adopted in 0.9V, and the temporal resolution of spectra collection is 0.301s, and electric potential scanning speed is 5mV/s.
The Pt electrode is at the saturated 0.1MHClO of CO in Fig. 7 external reflection pattern
4(solid line) and 0.1MHClO in the solution
4(dotted line) electric current and vCO in the solution
LAnd vCO
2Integrated intensity is with electrode potential variation relation figure.
Claims (2)
1. switchable surface infrared spectrum pool device of inside and outside reflection is characterized in that this spectral device is made up of electrode (3), electrolytic cell (4), internal reflected mode silicon semicolumn infrared window or external reflection pattern calcium fluoride semicolumn infrared window (5) electrode or external reflection pattern working electrode (1), contrast electrode (2), external reflection pattern internal reflected mode; Wherein, internal reflected mode is formed three-electrode system to electrode or external reflection pattern working electrode (1), contrast electrode (2) and external reflection pattern to electrode (3), place electrolytic cell (4), internal reflected mode silicon infrared window or external reflection pattern calcium fluoride infrared window are positioned at electrolytic cell (4) bottom.
2. according to the switchable surface infrared spectrum pool device of the described inside and outside reflection of claim 1, the diameter that it is characterized in that described external reflection working electrode (3) is 8mm～12mm, and the diameter of silicon semicolumn or calcium fluoride semicolumn is 15-25mm, and height is 20-26mm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200710044251 CN101131351A (en) | 2007-07-26 | 2007-07-26 | Inside and outside reflection-switchable surface infrared spectrum pool device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710044251 CN101131351A (en) | 2007-07-26 | 2007-07-26 | Inside and outside reflection-switchable surface infrared spectrum pool device |
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| CN101131351A true CN101131351A (en) | 2008-02-27 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103033474A (en) * | 2012-12-10 | 2013-04-10 | 中南大学 | Electrochemical-optical combined in-situ study spectral cell |
| CN103389331A (en) * | 2013-08-07 | 2013-11-13 | 苏州扬清芯片科技有限公司 | Sealed electrolytic cell for ultraviolet-visible spectrum |
| CN112730551A (en) * | 2020-12-16 | 2021-04-30 | 南方科技大学 | In-situ electrolytic cell for high-voltage electrochemistry |
| CN113447546A (en) * | 2021-06-28 | 2021-09-28 | 中国科学院长春应用化学研究所 | Vacuum-compatible surface-enhanced infrared spectroscopy electrochemical device and application |
| CN115266857A (en) * | 2022-06-21 | 2022-11-01 | 厦门大学 | Electrochemical in-situ infrared spectroscopy ATR electrolytic cell device |
-
2007
- 2007-07-26 CN CN 200710044251 patent/CN101131351A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103033474A (en) * | 2012-12-10 | 2013-04-10 | 中南大学 | Electrochemical-optical combined in-situ study spectral cell |
| CN103033474B (en) * | 2012-12-10 | 2016-06-08 | 中南大学 | Electrochemistry optics coupling on-spot study spectrum tool |
| CN103389331A (en) * | 2013-08-07 | 2013-11-13 | 苏州扬清芯片科技有限公司 | Sealed electrolytic cell for ultraviolet-visible spectrum |
| CN112730551A (en) * | 2020-12-16 | 2021-04-30 | 南方科技大学 | In-situ electrolytic cell for high-voltage electrochemistry |
| CN113447546A (en) * | 2021-06-28 | 2021-09-28 | 中国科学院长春应用化学研究所 | Vacuum-compatible surface-enhanced infrared spectroscopy electrochemical device and application |
| CN115266857A (en) * | 2022-06-21 | 2022-11-01 | 厦门大学 | Electrochemical in-situ infrared spectroscopy ATR electrolytic cell device |
| CN115266857B (en) * | 2022-06-21 | 2024-05-03 | 厦门大学 | Electrochemical in-situ infrared spectrum ATR electrolytic cell device |
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