CN109001271A - A kind of thin liquid layer electrochemical reaction cell suitable for In-situ Infrared detection - Google Patents
A kind of thin liquid layer electrochemical reaction cell suitable for In-situ Infrared detection Download PDFInfo
- Publication number
- CN109001271A CN109001271A CN201810584286.0A CN201810584286A CN109001271A CN 109001271 A CN109001271 A CN 109001271A CN 201810584286 A CN201810584286 A CN 201810584286A CN 109001271 A CN109001271 A CN 109001271A
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- window
- situ
- solution
- infrared
- liquid layer
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- 239000007788 liquid Substances 0.000 title claims abstract description 29
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 24
- 238000001514 detection method Methods 0.000 title claims abstract description 22
- 238000003487 electrochemical reaction Methods 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 20
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910001632 barium fluoride Inorganic materials 0.000 claims abstract description 14
- 238000013461 design Methods 0.000 claims abstract description 10
- 238000005259 measurement Methods 0.000 claims abstract description 7
- 238000003860 storage Methods 0.000 claims abstract description 7
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 8
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 16
- 238000004566 IR spectroscopy Methods 0.000 abstract description 13
- 238000012625 in-situ measurement Methods 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 19
- 238000001228 spectrum Methods 0.000 description 4
- 229910021607 Silver chloride Inorganic materials 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000000840 electrochemical analysis Methods 0.000 description 2
- 230000005518 electrochemistry Effects 0.000 description 2
- 241000826860 Trapezium Species 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
- G01N2021/0325—Cells for testing reactions, e.g. containing reagents
Abstract
The invention discloses a kind of thin liquid layer electrochemical reaction cells suitable for In-situ Infrared detection, including pedestal, round storage liquid groove, circular flat BaF2Window and circular upper cover, the assembling mode directly fitted using window and pedestal working electrode, and the thin liquid layer reaction in-situ pond that design forms solution self-adding is connected to liquid groove is stored by solution cavity.The thickness that can reduce liquid layer in solution cavity is directly fitted by working electrode and window, substantially reduces the extraneoas loss of measurement process infrared signal.Meanwhile the design being connected to using liquid groove is stored with solution cavity, the loss of reaction solution in solution cavity can be fed in real time during infrared in situ measurement.The present invention can study for solid-liquid system electrode surface and interface chemical reaction process and provide true and reliable in situ measurement environment, and can be substantially reduced the loss of measurement process mid-infrared light signal, can obtain high s/n ratio, reliable electrode surface infrared spectroscopy information.
Description
Technical field
The present invention relates to infrared spectroscopy test and analyze technical field, more particularly, to it is a kind of suitable for In-situ Infrared detection
Thin liquid layer electrochemical reaction cell.
Background technique
In energy and material surface and interface conversion process of energy, the detection of surface texture and key intermediate species is to material property
Optimization is promoted and catalytic process mechanism study is most important.Infrared spectroscopy is the fields such as chemistry, material, the energy, biology, environment
The important fingerprint technique of one kind of physical property characterization, plays important work in terms of surface and interface structure detection and surface functional group identification
With.However, since aqueous solution has stronger absorption to infrared light, (water is to the absorption length of infrared spectroscopy usually in some tens of pm amount
Grade), heavy losses of the infrared spectroscopy in detection process are caused, infrared spectroscopy is directly restrict and is detected in solid-liquid architecture
In extensive use.Such case is especially prominent in the infrared spectroscopic study in electro-catalysis field.In electrochemistry spectral investigation,
Electrochemical cell is the core of infrared spectroscopy experiment, directly affects the signal-to-noise ratio and correlation detection of acquired infrared spectroscopy
As a result reliability.The infrared reaction tank of electrochemical in-situ possesses work electricity in addition to having the function of Conventional electrochemical reaction tank
Outside pole, auxiliary electrode and reference electrode, it is also necessary to optical window and ultra-thin reaction solution thickness degree with " transparent ", with
Effectively reduce loss of the infrared signal in detection process, it is ensured that obtain the infrared experimental spectrum of high s/n ratio.
In order to realize to effective collection of infrared signal in situ in electrochemical reaction process, need to the infrared original position of electrochemistry
Structure, solution layer thickness, the window material in pond etc. are redesigned.Prior art discloses a variety of electrochemical in-situ infrared lights
Spectrum detection reaction tank, the window used are generally ZnSe window, and electrolytic solution is usually non-compensation model and thickness is uncontrollable,
To meet the total reflection measurement pattern requirement that decays, (i.e. infrared light and ZnSe window are incident at 45 degree of angles, by the multiple anti-of ZnSe
Exiting infrared light spectrum signal is obtained after penetrating) window mostly uses trapezium structure to design, and entire examination of infrared spectrum process is complicated for operation
And there is strict demand to optical path, and acquired infrared signal is readily incorporated the interference of other process signals.
Summary of the invention
Technical problem underlying to be solved by this invention is as follows: solving the problems, such as that reaction in-situ Process liquor compensates；It reduces
Additional infrared spectroscopy loss caused by being absorbed in electrochemical in-situ infrared spectroscopy detection process because of window material and reaction solution.
In view of this, the invention discloses a kind of thin liquid layer electrochemical reaction cell suitable for In-situ Infrared detection, this is anti-
Ying Chi combines ultra-thin reaction solution thickness degree using the high window material of infrared transmittivity, and it is red to greatly reduce electrochemical in-situ
The extraneoas loss of external spectrum detection process mid-infrared light signal；By constructing liquid-accumulating trough, realization pair in electrochemical operation area periphery
The compensation of electrochemical reaction area electrolyte；Window is suitable for single incidence-reflection infrared test mode using planar design,
Reduce the interference of other process signals in detection process.
The technical solution adopted by the present invention to solve the technical problems is: a kind of thin liquid layer suitable for In-situ Infrared detection
Electrochemical reaction cell, including pedestal, round storage liquid groove, circular flat BaF2Window and circular upper cover, circular flat BaF2Window
With the working electrode on pedestal using the assembling mode directly fitted, platinum filament is to electrode, working electrode lead-out wire and reference electrode
It is arranged evenly on circular upper cover, working electrode and circular flat are regulated and controled by the fastening bolt of adjustment base and circular upper cover
BaF2Solution layer thickness between window.
Wherein, circular flat BaF2The BaF that window materials select infrared transmittivity high2And use planar design.
Wherein, design has deep × wide circle having a size of 0.5mm × 1.0mm on the outside of the pedestal circular groove
Liquid groove is stored, liquid groove is stored with circle by solution cavity and is connected to design realization to solution luminal solution in In-situ Infrared measurement process
Automatic makeup function.
The principle of the invention is: using the BaF with the 1mm thickness compared with high infrared transmittance2Crystal as light passing window, with
Reduce the loss that infrared light passes through light passing window；The assembly model abutted directly on using window and working electrode, is compressed as far as possible
Solution layer thickness is to micron dimension in optical path；It is 0.5mm × 1mm by constructing depth × width in electro-chemical test area excircle
Circular groove, realize regulation and compensation to electro-chemical test area sample path length；Light passing window is set using circular flat structure
Meter, suitable for single incidence-Reflection measurement mode of infrared light, to reduce other signal interferences in measurement process.
The advantages and positive effects of the present invention are as follows:
Compared with the electrochemical in-situ infrared spectroscopy having disclosed detects reaction tank, the present invention be may be implemented to electrode surface
The real-time compensation of reaction solution ensures the true and reliable of in situ measurement process, while can be substantially reduced during in situ measurement
The extraneoas loss of infrared spectroscopy signals guarantees that detection end detector can obtain high s/n ratio, reliable infrared spectroscopy signals.
Detailed description of the invention
Fig. 1 is a kind of thin liquid layer electrochemical reaction cell schematic diagram of main components suitable for In-situ Infrared detection.
Fig. 2 is the three dimensional structure diagram of one embodiment of the present of invention.
Fig. 3 is the sectional front view of the present embodiment.
Wherein, 1 is pedestal, and 2 store liquid groove to be round, and 3 be circular flat BaF2Window, 4 be circular upper cover, and 5 be platinum filament
To electrode, 6 working electrode lead-out wires, 7 be Ag/AgCl reference electrode, and 8 be O-ring seal, and 9 be bolt, and 10 be working electrode.
Specific embodiment
With reference to the accompanying drawing and specific embodiment further illustrates the present invention.
As shown in Figure 1, the present invention provides a kind of thin liquid layer electrochemical reaction cells suitable for In-situ Infrared detection, including
Pedestal 1；The base center has circular groove, and the interior working electrode that will place is as electrochemical reaction area；The base center
There is round storage liquid groove 2 on the outside of first circular groove, as reaction solution liquid-accumulating trough；On first circular groove of base center
There is circular flat BaF in side2Window 3, the circular flat BaF23 lower surface of window will be directly bonded with electrode top to be formed it is micro-
The ultra-thin solution cavity of meter level；The circular flat BaF23 upper surface of window is directly contacted with circular upper cover 4, passes through upper cover four
The fastening bolt in week adjusts window and electrode surface laminating degree.
Thin liquid layer electrochemical reaction cell provided by the invention suitable for In-situ Infrared detection, main body include pedestal 1, circle
Shape plane BaF24 three parts of window 3 and circular upper cover, pedestal 1 and circular upper cover 4 are organic glass in one embodiment.
As shown in Figure 2,3, working electrode 10 is placed horizontally in the first circular groove of pedestal, and 10 upper surface of working electrode is direct
With 1mm thickness circular flat BaF2Window 3 contacts, and circular upper cover 4 is placed in the window upper surface, between pedestal 1 and circular upper cover 4
It is fixedly connected by bolt 9.There are three through-holes, respectively platinum filament to draw to electrode (CE) 5, working electrode for distribution on circular upper cover 4
The position that outlet (WK) 6 and Ag/AgCl reference electrode (RE) 7 are placed.Fig. 3 is Fig. 2 cross-sectional view detailed construction, in the circle of pedestal first
There is deep × wide round storage liquid groove 2 having a size of 0.5mm × 1.0mm on the outside of connected in star, is used for storage reaction solution.It tested
Pedestal 1 and circular upper cover 4 are fastenedly connected, then from the platinum of circular upper cover 4 by Cheng Zhong after electrode is placed by bolt 9
Reaction solution is injected reaction solution chamber to 5 hole of electrode by silk, and solution will store liquid groove 2 along circle and penetrate into through capillary action
Working electrode surface；It can be with Effective Regulation window and working electrode by the tightness of adjustment base 1 and upper bolt of cover setting 9
Between solution thickness.Solution injection terminates, and platinum filament is inserted into electrode 5 and Ag/AgCl reference electrode 7 corresponding on circular upper cover 4
Complete three-electrode electro Chemical can be formed to electrode hole and reference electrode hole react pond body in situ system, start In-situ Infrared light
Compose test experience.
Claims (3)
1. a kind of thin liquid layer electrochemical reaction cell suitable for In-situ Infrared detection, it is characterized in that: including pedestal (1), round storage
Liquid groove (2), circular flat BaF2Window (3) and circular upper cover (4), circular flat BaF2 window (3) and the work on pedestal (1)
Make electrode (10) using the assembling mode directly fitted, platinum filament is to electrode (5), working electrode lead-out wire (6) and reference electrode (7)
It is arranged evenly on circular upper cover (4), working electrode is regulated and controled by the fastening bolt (9) of adjustment base (1) and circular upper cover (4)
(10) and circular flat BaF2Solution layer thickness between window (3).
2. the thin liquid layer electrochemical reaction cell according to claim 1 suitable for In-situ Infrared detection, it is characterized in that: round
Plane BaF2The high BaF of window (3) material selection infrared transmittivity2And use planar design.
3. the thin liquid layer electrochemical reaction cell according to claim 1 or 2 suitable for In-situ Infrared detection, it is characterized in that:
Design has deep × wide round storage liquid groove having a size of 0.5mm × 1.0mm on the outside of the pedestal (1) circular groove
(2), liquid groove (2) are stored with circle by solution cavity and is connected to design realization to solution luminal solution in In-situ Infrared measurement process
Automatic makeup function.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810584286.0A CN109001271B (en) | 2018-06-08 | 2018-06-08 | Thin liquid layer electrochemical reaction pond suitable for infrared detection of normal position |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810584286.0A CN109001271B (en) | 2018-06-08 | 2018-06-08 | Thin liquid layer electrochemical reaction pond suitable for infrared detection of normal position |
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| Publication Number | Publication Date |
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| CN109001271A true CN109001271A (en) | 2018-12-14 |
| CN109001271B CN109001271B (en) | 2024-03-29 |
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| CN201810584286.0A Active CN109001271B (en) | 2018-06-08 | 2018-06-08 | Thin liquid layer electrochemical reaction pond suitable for infrared detection of normal position |
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Cited By (4)
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|---|---|---|---|---|
| CN106290161A (en) * | 2016-09-08 | 2017-01-04 | 刘雳 | A kind of sample cell for Dynamic Absorption spectra collection |
| CN111198178A (en) * | 2020-01-08 | 2020-05-26 | 中国科学院过程工程研究所 | Electrochemical in-situ online detection device and use method thereof |
| CN112485199A (en) * | 2020-12-01 | 2021-03-12 | 上海科技大学 | Reflection type temperature control infrared spectrum in-situ cell suitable for gas-solid phase electrochemical reaction |
| CN115266857A (en) * | 2022-06-21 | 2022-11-01 | 厦门大学 | Electrochemical in-situ infrared spectroscopy ATR electrolytic cell device |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106290161A (en) * | 2016-09-08 | 2017-01-04 | 刘雳 | A kind of sample cell for Dynamic Absorption spectra collection |
| CN111198178A (en) * | 2020-01-08 | 2020-05-26 | 中国科学院过程工程研究所 | Electrochemical in-situ online detection device and use method thereof |
| CN112485199A (en) * | 2020-12-01 | 2021-03-12 | 上海科技大学 | Reflection type temperature control infrared spectrum in-situ cell suitable for gas-solid phase electrochemical reaction |
| 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 |
| 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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| CN109001271B (en) | 2024-03-29 |
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