CN103175876B - Spectroelectrochemical in-situ pool and application thereof - Google Patents
Spectroelectrochemical in-situ pool and application thereof Download PDFInfo
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- CN103175876B CN103175876B CN201110436461.XA CN201110436461A CN103175876B CN 103175876 B CN103175876 B CN 103175876B CN 201110436461 A CN201110436461 A CN 201110436461A CN 103175876 B CN103175876 B CN 103175876B
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Abstract
The invention belongs to the technical field of combination of an electrochemical spectrum instrument, and relates to a spectroelectrochemical in-situ pool. The spectroelectrochemical in-situ pool comprises an upper pole plate, a lower pole plate, a membrane electrode assembly, a first polyester frame, a second polyester frame, a window, an upper pole plate sealing line, a lower pole plate sealing line and a window sealing O ring (8). The spectroelectrochemical in-situ pool can achieve combination of a plurality of spectrographs of external reflecting light paths, is close to an actual work environment of a fuel cell, can achieve heating and pressurizing, and achieves the targets of in-situ detection of fuel cell reaction products, intermediate products and adsorbed species under different work conditions. The spectroelectrochemical in-situ pool is strong in versatility, wide in application range, simple in structure, convenient to process and low in cost, and can achieve detection of a spectral signal on a lower membrane electrode under a plurality of situations.
Description
Technical field
The invention belongs to spectroelectrochemistry technology field, be specifically related to a kind of spectroelectrochemistry original position pond, can under fuel cell operating mode, realize the in situ detection of membrane electrode adsorption species with change in reaction conditions.
Background technology
Spectral technique comprises UV and visible spectra, infrared and Raman vibration-rotation spectrum, electronics and ion power spectrum, X ray spectrum etc.Spectral technique and electrochemical system coupling can be provided to the information of the electrochemical system that pure electrochemistry experiment cannot obtain, can carry out the detection of electrode surface adsorbing species with and the variation that changes with chemistry, electrochemical environment.Can infer based on this electrochemical reaction approach, obtain electrochemical reaction dynamics, at molecular layer understanding electrochemical reaction mechanism, and then instruct eelctro-catalyst synthetic, optimize important in inhibiting.
At present, the characterizing method of spectrum-galvanochemistry coupling is for the catalytic oxidation research at metal single crystal, polycrystalline or thin layer catalyst surface organic molecule, and means are comparatively ripe.But it is very challenging to carry out spectrum observation on membrane-membrane electrode for fuel cell surface, still unresolved so far.Film electrode structure and model electrode structure, fuel cell operating mode and three-electrode system have very large difference, and the direct information that original position is obtained electrochemical reaction in real time on fuel cell list pond has even more important theory value and directive significance for the performance and the stability that improve fuel cell.
The exploitation in the spectroelectrochemistry original position pond characterizing for membrane electrode belongs to the elementary step, the galvanochemistry infrared spectrum original position pond in document, and galvanochemistry X ray near side (ns) diffraction in-situ pond has some examples.But also have following problem: 1) original position pond current density is lower, duty differs greatly with true battery; 2) can not alternating temperature transformation, carry out the investigation 3 of differential responses condition) complex structure, often, for single light path system, universality is poor.
Summary of the invention
For above problem, the object of the invention is to provide a kind of spectroelectrochemistry original position pond, this device can be realized spectroelectrochemistry coupling under fuel cell operating mode, home position observation spectral signal changes with galvanochemistry excitation and reaction environment the variation producing, can spread spectrum electrochemical in-situ technology range of application, for the dynamic Real-Time Monitoring of fuel cell provides characterization method.
For achieving the above object, the technical solution used in the present invention is:
A kind of spectroelectrochemistry original position pond, comprises top crown, bottom crown, membrane electrode assembly, the first polyester frame and the second polyester frame, window, top crown potted line, bottom crown potted line and window sealing O circle;
On top crown, have the spectrum viewport of a penetrating plate face; Be carved with top crown flow field in spectrum viewport one side wall surface, top crown around; On top crown, be provided with the top crown material inlet and the top crown material outlet that are connected with top crown flow field;
One side wall surface of bottom crown is carved with bottom crown flow field; On bottom crown, be provided with the bottom crown material inlet and the bottom crown material outlet that are connected with bottom crown flow field, on the sidewall wall of bottom crown, be provided with heater block socket and thermocouple socket;
One end in the flow field of top crown side, spectrum viewport is provided with a groove, and spectrum viewport is coaxial with groove; Window is placed in inside grooves by the window sealing O circle that snaps in groove, is connected as a single entity with top crown;
The top crown, the first polyester frame, membrane electrode assembly, the second polyester frame, the lower step that are mounted with window overlap together successively, and are assembled into cell to be tested by trip bolt is affixed;
The axis projection in top crown flow field and bottom crown flow field coincides.
Described spectroelectrochemistry original position pond, wherein, seals pressing by top crown potted line and bottom crown potted line respectively between top crown and the first polyester frame and between lower step and the second polyester frame.
Described spectroelectrochemistry original position pond, described window materials are the one in zinc selenide, calcium fluoride, silicon, germanium, potassium bromide, sodium chloride, quartz, glass.
Described spectroelectrochemistry original position pond, its spectrum viewport is column type, circular platform type, pyramid type or square build.
Described spectroelectrochemistry original position pond, its top crown flow field and bottom crown flow field are point-like flow field, serpentine flow, rectangle channel or interlocking tooth shape flow field.
Described spectroelectrochemistry original position pond, wherein, the material of window sealing O circle, top crown potted line and bottom crown potted line is nitrile rubber, fluororubber or silicon rubber.
Described spectroelectrochemistry original position pond, the insertable heating component of its heater block socket is heating rod, heating plate, heater strip or heating tape.
Described spectroelectrochemistry original position pond, wherein, membrane electrode assembly comprises dielectric film and is placed in the Catalytic Layer of its both sides, also may comprise diffusion layer.
Described spectroelectrochemistry original position pond can be used as the in situ detection device that detects spectral signal, detect the information that spectral signal changes with galvanochemistry excitation and reaction environment, as the mensuration of direct liquid fuel battery course of work Anodic intermediate product and adsorbing species, the mensuration of Cathodic oxygen reduction intermediate product and adsorbing species.
Described spectral signal is UV and visible spectra, infrared or Raman vibration-rotation spectrum, electronics or ion power spectrum or X ray spectrum etc.
Spectroelectrochemistry original position of the present invention pond, its advantage and feature are as follows:
1. spectroelectrochemistry original position of the present invention pond can be realized and the spectrometer coupling of multiple external reflection light path, reach the object to fuel cell reaction product, intermediate product and adsorbing species in situ detection, thereby infer that electrochemical reaction approach is further to instruct the synthetic of eelctro-catalyst.
In its course of work of spectroelectrochemistry original position of the present invention pond with fuel cell actual working environment, can realize heating and pressurization, thus the in situ detection of reaction product, intermediate product and adsorbing species can realize battery and work under different temperatures and gas with various pressure time.
3. spectroelectrochemistry original position of the present invention pond highly versatile, applied widely, simple in structure, easy to process, with low cost, the detection that can realize membrane electrode polishing wax signal in multiple situation.
Brief description of the drawings
Fig. 1 is spectroelectrochemistry original position pool structure schematic diagram of the present invention.
Wherein, 1 is top crown material inlet; 2 is top crown material outlet; 3 bottom crown material inlets; 4 bottom crown material outlets; 5 is heating rod mouth; 6 is thermocouple mouth; 7 is top crown potted line; 8 is window sealing O circle; 9 is window; 10 is the first polyester frame; 10 ' is the second polyester frame; 11 is membrane electrode assembly; 12 is bottom crown potted line; 13 is top crown; 14 is bottom crown; 15 is spectrum viewport; 16 is top crown flow field; 17 is bottom crown flow field; 18 is groove.
Fig. 2 is the DMFC monocell performance curve that adopts original position pool device.
Fig. 3 is DMFC discharge process situ IR Characterization result.
Embodiment
Below in conjunction with embodiment, the present invention is explained in detail.Certainly the present invention is not limited in following specific embodiment.
Embodiment 1:
Fig. 1 is a kind of spectroelectrochemistry original position pool structure schematic diagram of the present invention.This original position pond is used for studying small organic molecule catalytic oxidation process, and middle adsorbing species is the variation with current potential, temperature, flow velocity, fuel concentration, gaseous tension at the diffuse reflectance IR of membrane electrode anode-side.This original position pond comprises top crown 13, bottom crown 14, membrane electrode assembly 11, window 9, pole plate potted line 7,12, window sealing O circle 8, the first polyester frames 10 and the second polyester frame 10 '.Wherein to adopt 316L stainless steel be materials processing for top crown 13 and bottom crown 14, is processed as point-like flow field in electrode reaction district, is processed with seal groove outside flow field, and top crown potted line 7 and bottom crown potted line 12 are put in respectively in upper and lower pole plate seal groove.Upper and lower polar plate flow field side is gold-plated to reduce contact resistance, and top crown can be baked carbon black and reduce the reflection of metal pair light near light beam side.Be split into tapering in the center of top crown 13 and be the circular hole of 45 °, as spectrum viewport 15, for the introducing of diffuse light; Spectrum viewport 15 inner sides on top crown 13, leave groove 18 as O ring recess and window groove near flow field one side, and window sealing O circle 8 is placed in top crown O ring recess, and window 9 is placed in top crown window groove.Membrane electrode assembly 11 (membrane electrode assembly 11 comprises superimposed successively anode-side diffusion layer, anode catalyst layer, dielectric film, cathode catalysis layer, cathode-side diffusion layer) need reserve with window in the preparation with big or small hole in anode-side diffusion layer, is convenient to infrared light and injects Catalytic Layer.Between upper and lower pole plate, put into successively polyester frame 10, membrane electrode assembly 11, the second polyester frame 10 ', by bottom crown on screw fastening for screw hole, complete the assembling of original position pond.Heating rod inserts bottom crown from heater block mouth 5, and thermopair inserts bottom crown from thermocouple hole 6.Total system can rise to 90 DEG C from room temperature and also keep stable within a few minutes.
The workflow that apply in direct liquid fuel battery in spectroelectrochemistry original position of the present invention pond is: organic molecule aqueous solution is imported by top crown material inlet 1, through top crown flow field, material is flowed out after membrane electrode assembly 11 anode-side are evenly distributed from top crown material outlet 2; Oxygen or air are imported by bottom crown material inlet 3, through bottom crown flow field, material are flowed out after membrane electrode assembly 11 cathode sides are evenly distributed from bottom crown material outlet 4.With electronics load testing control original position tank discharge, test condition is: 75 DEG C, anode passes into 1M methanol solution, and negative electrode passes into oxygen, and flow velocity is 40sccm.As shown in Figure 2, battery maximum power density reaches 45mW/cm to cell I-V curve test result
2, approach with typical DMFC power density.
With this understanding, electrode surface adsorbing species is measured to situation about more approaching under battery operating mode.50mAcm under constant-current discharge condition
-2, 150mAcm
-2gather respectively electrochemical in-situ infrared spectrum, result as shown in Figure 3, can be seen 2080-2090cm under battery operating mode
-1between the absorption of CO not obvious, and at 1000cm
-1left and right has stronger absorption peak to show that, under battery operating mode, the growing amount of methyl formate is larger.
As can be seen from the above-described embodiment spectroelectrochemistry original position of the present invention pond highly versatile, applied widely, simple in structure, easy to process, with low cost, be a kind of device for spectroelectrochemistry in-situ test, can realize the detection of membrane electrode polishing wax signal in multiple situation.
Claims (10)
1. a spectroelectrochemistry original position pond, is characterized in that: comprise top crown (13), bottom crown (14), membrane electrode assembly (11), the first polyester frame (10) and the second polyester frame (10 '), window (9) and window sealing O circle (8);
On top crown (13), have the spectrum viewport (15) of a penetrating plate face; Be carved with top crown flow field (16) in spectrum viewport (15) side wall surface, top crown (13) around; On top crown (13), be provided with the top crown material inlet (1) and the top crown material outlet (2) that are connected with top crown flow field (16);
One side wall surface of bottom crown (14) is carved with bottom crown flow field (17); On bottom crown (14), be provided with the bottom crown material inlet (3) and the bottom crown material outlet (4) that are connected with bottom crown flow field (17), on the sidewall wall of bottom crown (14), be provided with heater block socket (5) and thermocouple hole (6);
Be provided with an annular recess (18) in the flow field side of top crown (13), one end of spectrum viewport (15), spectrum viewport (15) is coaxial with groove (18); Window (9) is placed in groove (18) inside by the window sealing O circle (8) that snaps in groove (18), is connected as a single entity with top crown (13);
The top crown (13), the first polyester frame (10), membrane electrode assembly (11), the second polyester frame (10 '), the bottom crown (14) that are mounted with window (9) overlap together successively, and are assembled into cell to be tested by trip bolt is affixed;
Top crown flow field (16) coincides with the axis projection in bottom crown flow field (17), and flow field is oppositely arranged.
2. spectroelectrochemistry original position pond as claimed in claim 1, is characterized in that:
Wherein, between top crown (13) and the first polyester frame (10) and between bottom crown (14) and the second polyester frame (10 '), seal pressing by top crown potted line (7) and bottom crown potted line (12) respectively.
3. spectroelectrochemistry original position pond as claimed in claim 1, is characterized in that: described window (9) material is the one in zinc selenide, calcium fluoride, silicon, germanium, potassium bromide, sodium chloride, quartz, glass.
4. spectroelectrochemistry original position pond as claimed in claim 1, is characterized in that: spectrum viewport is column type, circular platform type, pyramid type or square build.
5. spectroelectrochemistry original position pond as claimed in claim 1, is characterized in that: top crown flow field (16) and bottom crown flow field (17) are point-like flow field, serpentine flow, rectangle channel or interlocking tooth shape flow field.
6. spectroelectrochemistry original position pond as claimed in claim 2, is characterized in that: the material of window sealing O circle (8), top crown potted line (7) and bottom crown potted line (12) is nitrile rubber, fluororubber or silicon rubber.
7. spectroelectrochemistry original position pond as claimed in claim 1, is characterized in that: the insertable heating component of heater block socket (5) is heating rod, heating plate, heater strip or heating tape; Thermocouple hole is inserted with thermopair in (6).
8. spectroelectrochemistry original position pond as claimed in claim 1, is characterized in that: described membrane electrode assembly (11) comprises dielectric film and is placed in the Catalytic Layer of its both sides.
9. the application in spectroelectrochemistry original position pond described in a claim 1, it is characterized in that: described in claim 1, spectroelectrochemistry original position pond can be used as the in situ detection device that detects spectral signal, detect the information that spectral signal changes with galvanochemistry excitation and reaction environment.
10. the application in spectroelectrochemistry original position pond as claimed in claim 9, is characterized in that: described spectral signal is ultraviolet or visible spectrum, infrared or Raman vibration-rotation spectrum, electronics or ion power spectrum or X ray spectrum.
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| CN103175876B true CN103175876B (en) | 2014-09-17 |
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| CN103852502B (en) * | 2014-03-28 | 2015-12-09 | 厦门大学 | A kind of electrolytic cell and detection method being applicable to Tip-Enhanced Raman Spectroscopy technology |
| RU2620022C1 (en) * | 2015-12-18 | 2017-05-22 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Московский государственный университет имени М.В. Ломоносова" (МГУ) | Electrochemical cell for in situ spectroscopy |
| CN105403553B (en) * | 2015-12-31 | 2019-01-22 | 中国科学技术大学 | A kind of laminar flows electrolytic cell suitable for the detection of electrochemical in-situ Raman spectrum |
| RU2654314C1 (en) * | 2016-12-28 | 2018-05-17 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Московский государственный университет имени М.В. Ломоносова" (МГУ) | Electrochemical cell with graphene electrode for in situ research of electrode materials and solid or gel electrolytes |
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| RU2692407C1 (en) * | 2017-12-27 | 2019-06-24 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Московский государственный университет имени М.В. Ломоносова" (МГУ) | Electrochemical cell for the electrode materials studying by the x-ray radiation absorption spectroscopy methods |
| CN111220673B (en) * | 2018-11-25 | 2021-06-11 | 中国科学院大连化学物理研究所 | Electrochemical testing device for in-situ Mossbauer spectra and application |
| CN109632848B (en) * | 2018-12-28 | 2020-05-22 | 厦门大学 | Spectrum pool suitable for electrochemistry normal position XRD characterization |
| CN111896518A (en) * | 2020-06-22 | 2020-11-06 | 西安交通大学 | Electrocatalytic CO2In-situ Raman detection electrochemical cell for reducing and synthesizing hydrocarbon fuel |
| CN111893508B (en) * | 2020-06-22 | 2021-05-28 | 西安交通大学 | Side-incident photoelectrocatalysis CO of electrolyte2Reduction reaction tank |
| CN112485310B (en) * | 2020-10-21 | 2022-04-05 | 中山大学 | Electrolytic cell device suitable for in-situ X-ray diffraction test |
| CN112485199B (en) * | 2020-12-01 | 2023-08-18 | 上海科技大学 | Reflection type temperature-control infrared spectrum in-situ cell suitable for gas-solid phase electrochemical reaction |
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| CN2773674Y (en) * | 2004-11-03 | 2006-04-19 | 中国科学院长春应用化学研究所 | On-the-site electrochemical analytical pool for laser Raman spectroscopy |
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| US20070218329A1 (en) * | 2005-07-05 | 2007-09-20 | Keith Kepler D | Combinatorial method and apparatus for screening electrochemical materials |
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| CN2773674Y (en) * | 2004-11-03 | 2006-04-19 | 中国科学院长春应用化学研究所 | On-the-site electrochemical analytical pool for laser Raman spectroscopy |
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