CN109001271B - Thin liquid layer electrochemical reaction pond suitable for infrared detection of normal position - Google Patents
Thin liquid layer electrochemical reaction pond suitable for infrared detection of normal position Download PDFInfo
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- CN109001271B CN109001271B CN201810584286.0A CN201810584286A CN109001271B CN 109001271 B CN109001271 B CN 109001271B CN 201810584286 A CN201810584286 A CN 201810584286A CN 109001271 B CN109001271 B CN 109001271B
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- 239000007788 liquid Substances 0.000 title claims abstract description 30
- 238000001514 detection method Methods 0.000 title claims abstract description 26
- 238000003487 electrochemical reaction Methods 0.000 title claims abstract description 18
- 238000011065 in-situ storage Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 22
- 230000008569 process Effects 0.000 claims abstract description 20
- 238000003860 storage Methods 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000002329 infrared spectrum Methods 0.000 claims abstract description 17
- 229910016036 BaF 2 Inorganic materials 0.000 claims abstract description 11
- 238000013461 design Methods 0.000 claims abstract description 6
- 238000005259 measurement Methods 0.000 claims abstract description 6
- 238000004891 communication Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 34
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 9
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 5
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 238000002474 experimental method Methods 0.000 claims description 3
- 230000009471 action Effects 0.000 claims description 2
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- 239000013067 intermediate product Substances 0.000 claims description 2
- 239000012466 permeate Substances 0.000 claims description 2
- 229910001632 barium fluoride Inorganic materials 0.000 claims 1
- 238000012625 in-situ measurement Methods 0.000 abstract description 4
- 238000011160 research Methods 0.000 abstract description 4
- 239000012295 chemical reaction liquid Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 7
- 238000004566 IR spectroscopy Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- 238000000840 electrochemical analysis Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229920005372 Plexiglas® Polymers 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000005102 attenuated total reflection Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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
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- 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
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- 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
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Molecular Biology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
- Optical Measuring Cells (AREA)
Abstract
The invention discloses a thin liquid layer electrochemical reaction tank suitable for in-situ infrared detection, which comprises a base, a circular liquid storage groove and a circular plane BaF 2 The window sheet and the round upper cover adopt an assembling mode that the window sheet is directly attached to the base working electrode, and a thin liquid layer in-situ reaction tank for self-supplying solution is formed through the communication design of the solution cavity and the liquid storage groove. The working electrode is directly attached to the window sheet, so that the thickness of a liquid layer in the solution cavity can be reduced, and the extra loss of infrared light signals in the measuring process is greatly reduced. Meanwhile, the liquid storage groove is communicated with the solution cavity, so that the loss of the reaction liquid in the solution cavity can be supplied in real time in the infrared in-situ measurement process. The invention can provide a real and reliable in-situ measurement environment for the research of the solid-liquid electrode surface interface chemical reaction process, can obviously reduce the loss of infrared light signals in the measurement process, and can obtain reliable electrode surface infrared spectrum information with high signal-to-noise ratio.
Description
Technical Field
The invention relates to the technical field of infrared spectrum detection and analysis, in particular to a thin liquid layer electrochemical reaction tank suitable for in-situ infrared detection.
Background
In the process of interfacial energy conversion of an energy material surface, detection of an electrode surface structure and a key intermediate product is important to optimization and improvement of material performance and research of a catalytic process mechanism. Infrared spectroscopy is an important fingerprint technology for physical property characterization in the fields of chemistry, materials, energy sources, biology, environment and the like, and plays an important role in surface interface structure detection and surface functional group identification. However, the aqueous solution has strong absorption to infrared light (the absorption length of water to infrared spectrum is usually in the order of tens of micrometers), so that serious loss of infrared spectrum in the detection process is caused, and the wide application of infrared spectrum in solid-liquid structure detection is directly restricted. This is particularly true in the field of infrared spectroscopy research in the field of electrocatalysis. In electrochemical spectroscopy research, the electrochemical cell is the core part of an infrared spectroscopy experiment, and directly influences the signal-to-noise ratio of the acquired infrared spectrum and the reliability of related detection results. Besides the function of the conventional electrochemical reaction tank, namely the working electrode, the auxiliary electrode and the reference electrode, the electrochemical in-situ infrared reaction tank also needs to have a transparent optical window and an ultrathin reaction solution layer thickness so as to effectively reduce the loss of infrared light signals in the detection process and ensure that an infrared experimental spectrum with high signal to noise ratio is obtained.
In order to achieve effective collection of in-situ infrared signals during electrochemical reactions, redesign of the structure, solution layer thickness, window materials, etc. of the electrochemical infrared in-situ cell is required. The prior art discloses a plurality of electrochemical in-situ infrared spectrum detection reaction tanks, wherein the adopted window sheets are ZnSe window sheets, the electrolytic solution is in a non-compensation mode and the thickness is uncontrollable, in order to meet the requirements of an attenuated total reflection measurement mode (namely, infrared light and ZnSe window sheets are incident at an angle of 45 degrees, emergent infrared spectrum signals are obtained after repeated reflection of ZnSe), the window sheets are designed into a trapezoid structure, the whole infrared spectrum test process is complex in operation and has strict requirements on the optical path, and the acquired infrared signals are easy to introduce the interference of other process signals.
Disclosure of Invention
The main technical problems to be solved by the invention are as follows: solving the problem of solution compensation in the in-situ reaction process; and the extra infrared spectrum loss caused by the absorption of window materials and reaction solution in the in-situ electrochemical infrared spectrum detection process is reduced.
In view of the above, the invention discloses a thin liquid layer electrochemical reaction tank suitable for in-situ infrared detection, which adopts a window material with high infrared transmittance to combine with the ultrathin thickness of a reaction solution layer, thereby greatly reducing the extra loss of infrared light signals in the electrochemical in-situ infrared spectrum detection process; by constructing a liquid storage tank at the periphery of the electrochemical working area, the compensation of electrolyte in the electrochemical reaction area is realized; the window adopts a planar structure design, is suitable for a single incidence-reflection infrared test mode, and reduces interference of signals in other processes in the detection process.
The invention is thatThe technical scheme adopted for solving the technical problems is as follows: a thin liquid layer electrochemical reaction tank suitable for in-situ infrared detection comprises a base, a circular liquid storage groove and a circular plane BaF 2 Window and circular top cover, circular plane BaF 2 The window sheets and the working electrode on the base are assembled in a direct bonding way, the platinum wire counter electrode, the working electrode outgoing line and the reference electrode are distributed and arranged on the circular upper cover, and the working electrode and the circular plane BaF are regulated and controlled by regulating the fastening bolts of the base and the circular upper cover 2 Inter-window solution layer thickness.
Wherein, the round plane BaF 2 BaF with high infrared transmittance is selected as window sheet material 2 And adopts a planar design.
The automatic solution replenishing device is characterized in that a circular solution storage groove with the depth multiplied by the width of 0.5mm multiplied by 1.0mm is arranged on the outer side of the circular groove of the base, and the automatic solution replenishing function in the solution cavity in the in-situ infrared measurement process is realized through the communication design of the solution cavity and the circular solution storage groove.
The principle of the invention is as follows: baF with high infrared transmittance and thickness of 1mm is adopted 2 The crystal is used as a light-passing window to reduce the loss of infrared light passing through the light-passing window; adopting an assembly mode that a window is directly clung to a working electrode, and compressing the thickness of a solution layer in a light path to the micrometer level as far as possible; the method is characterized in that a circular groove with the depth multiplied by the width of 0.5mm multiplied by 1mm is formed in the outer circumference of an electrochemical test area, so that the regulation and compensation of the thickness of the solution in the electrochemical test area are realized; the light transmission window adopts a circular plane structure design, and is suitable for a single incidence-reflection measurement mode of infrared light, so that other signal interference in the measurement process is reduced.
The invention has the advantages and positive effects that:
compared with the electrochemical in-situ infrared spectrum detection reaction tank, the invention can realize real-time compensation of the electrode surface reaction solution, ensure the reality and reliability of the in-situ measurement process, obviously reduce the extra loss of infrared spectrum signals in the in-situ measurement process, and ensure that the detector at the detection end can acquire reliable infrared spectrum signals with high signal-to-noise ratio.
Drawings
FIG. 1 is a schematic diagram of the major components of a thin liquid layer electrochemical reaction cell suitable for in situ infrared detection.
Fig. 2 is a schematic three-dimensional structure of an embodiment of the present invention.
Fig. 3 is a front sectional view of the present embodiment.
Wherein 1 is a base, 2 is a circular liquid storage groove, and 3 is a circular plane BaF 2 The window piece, 4 is circular upper cover, 5 is platinum wire counter electrode, 6 working electrode lead-out wire, 7 is Ag/AgCl reference electrode, 8 is O type sealing ring, 9 is bolt, 10 is working electrode.
Detailed Description
The invention is further described below with reference to the drawings and detailed description.
As shown in fig. 1, the invention provides a thin liquid layer electrochemical reaction cell suitable for in-situ infrared detection, which comprises a base 1; the center of the base is provided with a circular groove, and a working electrode is placed in the circular groove to serve as an electrochemical reaction area; a circular liquid storage groove 2 is formed outside the first circular groove in the center of the base and is used as a reaction solution storage groove; a circular plane BaF is arranged above the first circular groove in the center of the base 2 A window 3, said circular plane BaF 2 The lower surface of the window sheet 3 is directly attached to the upper surface of the electrode to form a micron-sized ultrathin solution cavity; the round plane BaF 2 The upper surface of the window sheet 3 is in direct contact with the round upper cover 4, and the fitting degree of the window sheet and the electrode surface is adjusted through fastening bolts around the upper cover.
The invention provides a thin liquid layer electrochemical reaction tank suitable for in-situ infrared detection, which comprises a main body comprising a base 1 and a circular plane BaF 2 The window 3 and the circular top cover 4 are three parts, in one embodiment both the base 1 and the circular top cover 4 are plexiglas. As shown in fig. 2 and 3, the working electrode 10 is horizontally arranged in the first circular groove of the base, and the upper surface of the working electrode 10 is directly connected with a circular plane BaF with the thickness of 1mm 2 The window sheet 3 contacts, circular upper cover 4 is placed to the window sheet upper surface, passes through bolt 9 fixed connection between base 1 and the circular upper cover 4. Three through holes are distributed on the round upper cover 4, which are a platinum wire Counter Electrode (CE) 5, a working electrode outgoing line (WK) 6 and A respectivelyg/AgCl Reference Electrode (RE) 7 placed. FIG. 3 is a detailed sectional view of FIG. 2, in which a circular liquid storage groove 2 having a depth by width dimension of 0.5mm by 1.0mm is provided outside the first circular groove of the base for storing the reaction solution. In the experimental process, after the electrode is placed, the base 1 and the round upper cover 4 are tightly connected through the bolts 9, then the reaction solution is injected into the reaction solution cavity from the platinum wire counter electrode 5 hole of the round upper cover 4, and the solution permeates to the surface of the working electrode along the round liquid storage groove 2 through capillary action; the tightness degree of the base 1 and the upper cover fastening bolt 9 can be adjusted to effectively regulate the thickness of the solution between the window and the working electrode. After the solution injection is finished, a complete three-electrode electrochemical reaction in-situ cell system can be formed by inserting a platinum wire counter electrode 5 and an Ag/AgCl reference electrode 7 into corresponding counter electrode holes and reference electrode holes on the round upper cover 4, and an in-situ infrared spectrum detection experiment is started.
Claims (2)
1. A thin liquid layer electrochemical reaction tank suitable for in-situ infrared detection is characterized in that: comprises a base (1), a circular liquid storage groove (2) and a circular plane BaF 2 The window piece (3) and the circular upper cover (4), the circular plane BaF2 window piece (3) and the working electrode (10) on the base (1) are assembled in a direct bonding way, the platinum wire counter electrode (5), the working electrode outgoing line (6) and the reference electrode (7) are distributed and arranged on the circular upper cover (4), and the working electrode (10) and the circular plane BaF are regulated and controlled by regulating the fastening bolts (9) of the base (1) and the circular upper cover (4) 2 The thickness of the solution layer between the window sheets (3);
the center of the base (1) is provided with a first circular groove, and a working electrode is placed in the first circular groove to serve as an electrochemical reaction area; a circular liquid storage groove (2) is formed outside the first circular groove in the center of the base and is used as a reaction solution storage groove; a circular plane BaF is arranged above the first circular groove in the center of the base 2 A window pane (3), said circular plane BaF 2 The lower surface of the window sheet (3) is directly attached to the upper surface of the electrode to form a micron-sized ultrathin solution cavity; the round plane BaF 2 The upper surface of the window sheet (3) is directly contacted with the round upper cover (4) through the fastening bolts around the upper coverAdjusting the fitting degree of the window sheet and the electrode surface;
the working electrode (10) is horizontally arranged in the first circular groove of the base, and the upper surface of the working electrode (10) is directly connected with a circular plane BaF with the thickness of 1mm 2 The method comprises the steps that a window sheet (3) is contacted, a circular upper cover (4) is placed on the upper surface of the window sheet, three through holes are distributed on the circular upper cover (4) and are respectively the positions where a platinum wire counter electrode (5), a working electrode outgoing line (6) and an Ag/AgCl reference electrode (7) are placed, in the experimental process, after the working electrode is placed, a base (1) is fixedly connected with the circular upper cover (4) through bolts (9), then a reaction solution is injected into a reaction solution storage tank through the platinum wire counter electrode (5) holes of the circular upper cover (4), and the solution permeates to the surface of the working electrode through capillary action along a circular liquid storage groove (2); the tightness degree of the fastening bolts (9) of the base (1) and the round upper cover is adjusted and controlled to regulate the thickness of the solution between the window and the working electrode; after the solution injection is finished, a complete three-electrode electrochemical reaction in-situ cell system can be formed by inserting a platinum wire counter electrode (5) and an Ag/AgCl reference electrode (7) into corresponding counter electrode holes and reference electrode holes on a circular upper cover (4), a reflection mode in-situ infrared spectrum detection experiment is started, and the change of key intermediate products of a working electrode solid-liquid surface interface is tracked in real time.
2. The thin liquid layer electrochemical reaction cell suitable for in situ infrared detection of claim 1, wherein: the outside of the circular groove of the base (1) is designed with a circular liquid storage groove (2) with the depth multiplied by the width of 0.5mm multiplied by 1.0mm, and the automatic replenishing function of the solution in the solution cavity in the in-situ infrared measurement process is realized through the communication design of the solution cavity and the circular liquid storage groove (2).
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| CN109001271B true CN109001271B (en) | 2024-03-29 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106290161B (en) * | 2016-09-08 | 2024-01-12 | 刘雳 | Sample cell for dynamic absorption spectrum 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 |
| 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 |
| 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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| JP2004177278A (en) * | 2002-11-27 | 2004-06-24 | Mitsubishi Chemicals Corp | Small-sized reaction analytical apparatus |
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| US8585880B2 (en) * | 2011-09-27 | 2013-11-19 | Battelle Memorial Institute | Method and apparatus for simultaneous spectroelectrochemical analysis |
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| CN103033474A (en) * | 2012-12-10 | 2013-04-10 | 中南大学 | Electrochemical-optical combined in-situ study spectral cell |
| CN105352917A (en) * | 2015-10-19 | 2016-02-24 | 哈尔滨工业大学 | In-situ electrochemical infrared spectroscopic-mass spectrometric detection system and method |
| CN106885774A (en) * | 2017-01-13 | 2017-06-23 | 华南理工大学 | A kind of thin-layer spectral electrochemical detection means with sandwich structure |
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