Electrochemical in-situ ultraviolet-visible-near infrared pumping detection reaction tank

Abstract

The utility model provides an electrochemical in-situ ultraviolet-visible-near infrared pumping detection reaction tank which comprises a reaction tank body, two local reaction tanks communicated by a thin-layer passage are arranged in the reaction tank body, and an electrode group comprising an L-shaped working electrode, a counter electrode and a reference electrode is also arranged in the reaction tank body. A thin-layer passage is arranged in the two local reaction tanks, a thin-layer electrode is arranged in the thin-layer passage, the L-shaped working electrode is connected with the thin-layer electrode, an electrolyte circulating system is arranged between the two local reaction tanks, a circulating pump is arranged in a pipeline of the electrolyte circulating system, and temperature control pipelines are arranged on the outer sides of the tank walls and the tank bottoms of the two local reaction tanks. The two local reaction tanks are provided with reaction tank covers with holes, the reaction tank covers with holes are provided with electrode holes used for supporting the electrode group, pipeline through holes used for being communicated with an electrolyte circulating system pipeline and air holes, and the bottoms of the two local reaction tanks are provided with solid reaction tank bases.

Description

Technical Field

[0001] The utility model relates to the technical field of new energy material catalysis, and particularly relates to an in-situ ultraviolet-visible-near-infrared pump-probe reaction cell for electrochemistry. Background Art

[0002] Ultraviolet-visible-near-infrared (UV-Vis-NIR) pump-probe technology is a spectral analysis method for studying materials by combining an excitation light (pump light) and a probe light. The combination of pump-probe spectral analysis and electrochemistry methods can monitor the dynamic changes in electrochemical reactions in real time, provide spectral information of substances during the reaction process, and reflect important information on electron transfer processes, reaction intermediates, and reaction kinetics. However, traditional electrochemical reaction cells mainly focus on the progress of electrochemical reactions and the configuration of electrodes. When performing spectral analysis, the reaction cell needs to be modified or an additional optical path system needs to be set up, resulting in complex experimental operations and easy introduction of errors, which limits the accuracy and real-time nature of experimental results. Therefore, it is necessary to develop an electrochemical reaction cell suitable for in-situ ultraviolet-visible-near-infrared pump-probe. Summary of the Utility Model

[0003] In order to solve the defects in the prior art, the utility model provides an in-situ ultraviolet-visible-near-infrared pump-probe reaction cell for electrochemistry.

[0004] An in-situ ultraviolet-visible-near-infrared pump-probe reaction cell for electrochemistry of the utility model includes a reaction cell body. A first local reaction cell and a second local reaction cell are arranged in the reaction cell body and are connected by a thin-layer channel. An electrode group including an L-shaped working electrode, a counter electrode, and a reference electrode is also arranged in the reaction cell body. A thin-layer electrode is arranged in the thin-layer channel, and the L-shaped working electrode is connected to the thin-layer electrode.

[0005] There is an electrolyte circulation system between the first local reaction cell and the second local reaction cell, and a circulation pump is arranged in the pipeline of the electrolyte circulation system.

[0006] Temperature control pipelines are arranged on the outer sides of the pool walls and the pool bottoms of the first local reaction cell and the second local reaction cell. The temperature control pipelines have a temperature control water inlet and a temperature control water outlet.

[0007] The first local reaction cell and the second local reaction cell are both provided with reaction cell covers with holes. The reaction cell covers with holes are provided with electrode holes for supporting the electrode group, pipeline through holes for supporting the pipelines of the electrolyte circulation system, and air holes.

[0008] The pool bottoms of the first local reaction cell and the second local reaction cell have solid reaction cell bases.

[0009] Preferably, the reaction cell body is made of quartz glass.

[0010] Preferably, the perforated reaction cell cover is made of polytetrafluoroethylene.

[0011] Preferably, the outer wall of the thin layer passage is a single-layer structure.

[0012] Preferably, the L-shaped working electrode is located on the side of the first local reaction cell, and the reference electrode and the counter electrode are located on the side of the second local reaction cell.

[0013] Preferably, in the electrolyte circulation system, the circulation direction of the electrolyte is from the second local reaction cell to the first local reaction cell. The pipeline through hole of the perforated cell cover of the first local reaction cell is the liquid inlet hole, and the pipeline through hole of the perforated cell cover of the second local reaction cell is the liquid outlet hole. One end of the pipeline of the electrolyte circulation system is inserted into the liquid inlet hole, and the other end is inserted into the liquid outlet hole.

[0014] Preferably, the reaction cell body is equipped with an optical precision displacement stage to meet precise adjustment in space.

[0015] The utility model has the following beneficial effects:

[0016] The reaction cell of the utility model can monitor the spectral changes of species in real time during the electrochemical reaction process, provide dynamic reaction information, and improve the accuracy and real-time performance of experimental results. Moreover, through the temperature control pipeline system, the utility model can carry out electrochemical reactions at a specific temperature. The utility model also has an electrolyte circulation system, which can achieve uniform mixing of the electrolyte and remove the surface bubbles on the thin layer electrode. Description of the Drawings

[0017] Figure 1 is the front view structural schematic diagram of an in-situ ultraviolet-visible-near-infrared pump-probe reaction cell of the utility model.

[0018] Figure 2 is the top view structural schematic diagram of an in-situ ultraviolet-visible-near-infrared pump-probe reaction cell of the utility model. Detailed Embodiments

[0019] The following will describe the embodiments of the utility model in conjunction with the drawings of the specification. It should be noted that the embodiments involved in this specification are not exhaustive and do not represent the only embodiments of the utility model. The following corresponding embodiments are only for clearly explaining the utility model content of the utility model patent and do not limit its embodiments. For those of ordinary skill in the art, different forms of changes and modifications can also be made on the basis of the description of these embodiments. Any changes or modifications that belong to the technical concept and utility model content of the utility model and are obvious are also within the protection scope of the utility model.

[0020] The following will combine with Figure 1-2 to describe the preferred embodiments of the present utility model in detail. An in-situ electrochemical ultraviolet-visible-near infrared pump-probe reaction cell of the present utility model includes a reaction cell body. A first local reaction cell A and a second local reaction cell B are arranged in the reaction cell body, and the two local reaction cells are connected by a thin-layer channel 6. The reaction cell is a three-electrode system. Therefore, an electrode group including an L-shaped working electrode 3, a counter electrode 4, and a reference electrode 5 is arranged in the reaction cell body. A thin-layer electrode 7 is arranged in the thin-layer channel 6, and the L-shaped working electrode 3 is connected to the thin-layer electrode 7 to serve as an electrochemical reaction electrode. The thin-layer electrode 7 is arranged at the center of the thin-layer channel 6 for easy testing. Preferably, the reaction cell body is made of quartz glass, which can ensure the lossless passage of ultraviolet-visible-near infrared light and improve the quality of spectral data. More preferably, the outer wall of the thin-layer channel 6 is a single-layer structure. Compared with the double-layer structure, the thin-wall channel 6 with a single-layer structure can reduce light loss and the interference of the air layer on the light path, thereby improving the detection signal intensity and accuracy.

[0021] The first local reaction cell A is provided with a first perforated reaction cell cover 1A, and the second local reaction cell B is provided with a second perforated reaction cell cover 1B. The perforated reaction cell cover is made of polytetrafluoroethylene. The reaction cell cover made of this material has the characteristics of high temperature resistance, corrosion resistance, good insulation, and processability. Both of the two perforated reaction cell covers are provided with electrode holes for supporting the electrode group, pipeline through holes for connecting the electrolyte circulation system pipeline, and air holes. The air holes are used to balance the pressure inside and outside the reaction cell and meet the ventilation requirements of some electrochemical reactions, such as passing nitrogen to remove oxygen in the electrolyte. Specifically, as Figure 2 shown in the top view of the reaction cell cover in, the number of holes on the first perforated reaction cell cover 1A is 3, which are respectively: the working electrode hole 1A1 on the reaction cell cover, the air hole 1A2 on the reaction cell cover, and the liquid inlet hole 1A3 for the electrolyte circulation system pipeline; the number of holes on the second perforated reaction cell cover 1B is 4, which are respectively: the counter electrode hole 1B1 on the reaction cell cover, the reference electrode hole 1B2 on the reaction cell cover, the liquid outlet hole 1B3 for the electrolyte circulation system pipeline, and the air hole 1B4 on the reaction cell cover.

[0022] In each preferred embodiment, there is an electrolyte circulation system 10 between the first local reaction cell A and the second local reaction cell B, and a circulation pump M is provided in the pipeline of the electrolyte circulation system. Preferably, the electrolyte circulation direction in the electrolyte circulation system is from the second local reaction cell B to the first local reaction cell A, that is, the pipeline through hole of the perforated cell cover of the first local reaction cell A is the liquid inlet hole 1A3, and the pipeline through hole of the perforated cell cover of the second local reaction cell B is the liquid outlet hole 1B3. In this way, the electrolyte in the second local reaction cell B can be extracted from the pipeline inserted into the liquid outlet hole 1B3 of the electrolyte circulation system, and the electrolyte can be input into the first local reaction cell A through the pipeline inserted into the liquid inlet hole 1A3 of the electrolyte circulation system. The electrolyte in the first local reaction cell A then enters the second local reaction cell B through the thin layer passage 6 to form a cycle, so as to realize the uniform mixing of the electrolyte and remove the surface bubbles on the thin layer electrode 7.

[0023] In each preferred embodiment, the outer sides of the pool walls and the pool bottoms of the first local reaction cell A and the second local reaction cell B are both provided with temperature control pipelines 9, and the temperature control pipelines 9 have a temperature control water inlet 2A and a temperature control water outlet 2B. The temperature control pipeline 9 is connected to an external temperature control device (not shown), and water circulation is carried out through the temperature control water inlet 2A and the temperature control water outlet 2B, so as to control the temperature of the electrolyte in the first local reaction cell A and the second local reaction cell B, and the electrochemical reaction can be realized at a specific temperature.

[0024] In each preferred embodiment, the bottoms of the first local reaction cell A and the second local reaction cell B have solid reaction cell bases 8, specifically below the temperature control pipelines 9 at the pool bottoms. The solid reaction cell bases 8 are beneficial to the balance and stability of the reaction cell body. Preferably, the reaction cell body of the present utility model can be paired with an optical precision displacement stage (not shown) to meet the precise adjustment in space and realize the precise alignment of the pump light and the probe light on the thin layer electrode 7.

[0025] The following details the usage method of an electrochemical in-situ ultraviolet-visible-near-infrared pump-probe reaction cell of the present utility model, including the following steps:

[0026] 1. Add the electrolyte into the first local reaction cell A, and the electrolyte flows into the second local reaction cell B through the single-layer thin layer passage 6. After the liquid levels of the two local reaction cells A and B are stable, ensure that the electrolyte liquid level is higher than the top of the single-layer thin layer passage 6.

[0027] 2. Coat the surface of the thin layer electrode 7 with the material to be measured for the electrochemical reaction. After the material is stable on the electrode surface, insert the L-shaped working electrode 3 connected to the thin layer electrode 7 into the working electrode hole 1A1 of the perforated cell cover 1A, and cover the perforated cell cover 1A on the first local reaction cell A and fix it to ensure that the material coated on the thin layer electrode 7 is at the center of the single-layer thin layer passage 6.

[0028] 3. Connect the main body of the reaction cell to an external temperature control device through the internal temperature control pipeline 9 to achieve precise temperature control.

[0029] 4. Insert the pipelines of the electrolyte circulation system 10 into the electrolyte liquid level through the liquid inlet hole 1A3 and the liquid outlet hole 1B3, and turn on the circulation pump M to circulate the electrolyte between the first local reaction cell A and the second local reaction cell B, so as to achieve the effects of uniform mixing of the electrolyte in the reaction cell and removing the surface bubbles on the thin-layer electrode 7.

[0030] 5. Place the main body of the reaction cell on an optical precision displacement stage, connect the L-shaped working electrode 3, counter electrode 4, and reference electrode 5 with an electrochemical workstation, and perform an electrochemical reaction.

[0031] 6. Move the optical precision displacement stage to make the pump light and the probe light coincide at the coating material of the thin-layer electrode 7, and detect the spectral characteristic changes of the material in real time in-situ.

[0032] Obviously, those of ordinary skill in the art should recognize that the above embodiments are only used to illustrate the present invention, rather than to limit the present invention. As long as it is within the scope of the spirit of the present invention, changes and modifications to the above embodiments will fall within the scope of the claims of the present invention.

Claims

1. An electrochemical in-situ ultraviolet-visible-near infrared pump detection reaction cell, characterized in that: The invention comprises a reaction pool body, wherein a first local reaction pool and a second local reaction pool connected by a thin layer passage are arranged in the reaction pool body, an electrode group including an L-shaped working electrode, a counter electrode and a reference electrode is also arranged in the reaction pool body, a thin layer electrode is arranged in the thin layer passage, and the L-shaped working electrode is connected to the thin layer electrode. An electrolyte circulation system is provided between the first partial reaction pool and the second partial reaction pool, and a circulation pump is provided in the pipeline of the electrolyte circulation system. The first partial reaction pool and the second partial reaction pool are provided with temperature control pipelines on the outer sides of the pool wall and the pool bottom, and the temperature control pipelines are provided with temperature control water inlets and temperature control water outlets. The first partial reaction pool and the second partial reaction pool are both provided with a reaction pool cover with holes, and the reaction pool cover with holes is provided with electrode holes for supporting the electrode group, pipeline through holes for supporting the electrolyte circulation system pipeline, and air holes, The first partial reaction tank and the second partial reaction tank have a solid reaction tank base at the bottom.

2. The electrochemical in-situ UV-visible-near infrared pump detection reaction cell according to claim 1, characterized in that: The reaction cell body is made of quartz glass.

3. The electrochemical in-situ UV-visible-near infrared pump detection reaction cell according to claim 1, characterized in that: The reaction pool cover with holes is made of polytetrafluoroethylene.

4. The electrochemical in-situ UV-visible-near infrared pump detection reaction cell according to claim 1, characterized in that: The outer wall of the thin layer passage is a single-layer structure.

5. The electrochemical in-situ UV-visible-near infrared pump detection reaction cell according to claim 1, characterized in that: The L-shaped working electrode is located on the first local reaction cell side, and the reference electrode and the counter electrode are located on the second local reaction cell side.

6. The electrochemical in-situ UV-visible-near infrared pump detection reaction cell according to claim 1, characterized in that: The electrolyte circulation direction in the electrolyte circulation system is from the second local reaction pool to the first local reaction pool, the pipe through hole of the perforated pool cover of the first local reaction pool is the liquid inlet hole, and the pipe through hole of the perforated pool cover of the second local reaction pool is the liquid outlet hole, one end of the pipe of the electrolyte circulation system is inserted into the liquid inlet hole, and the other end is inserted into the liquid outlet hole.

7. The electrochemical in-situ UV-visible-near infrared pump detection reaction cell according to claim 1, characterized in that: The reaction pool body is equipped with an optical precision translation stage to enable precise adjustment in space.

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