CN112285173A - Method and related device for optical/electrochemical in-situ Raman detection - Google Patents
Method and related device for optical/electrochemical in-situ Raman detection Download PDFInfo
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- CN112285173A CN112285173A CN202011004376.1A CN202011004376A CN112285173A CN 112285173 A CN112285173 A CN 112285173A CN 202011004376 A CN202011004376 A CN 202011004376A CN 112285173 A CN112285173 A CN 112285173A
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- 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
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- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
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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
- G01N2021/0328—Arrangement of two or more cells having different functions for the measurement of reactions
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Abstract
A method for in-situ Raman detection by optical/electrochemical method and its related device features that a special in-situ chemical reaction device is used to connect Raman spectrometer. The designed in-situ reaction tank mainly comprises: the device comprises a reaction cell main body, an electrode connecting hole groove, a light source connecting hole groove, an atmosphere connecting hole groove/solution inlet and outlet hole groove, a quartz optical window, an adaptive electrode, an optical fiber guide pipe, a hole groove gasket and a sealing screw suite, and is suitable for being arranged in a sample bin of a Raman spectrometer and connected with a light source controller or an electrochemical workstation for realizing real-time Raman spectrum analysis of in-situ control light and electric reaction conditions. The invention widens the parameter dimension that the Raman spectrum can only change the laser power and the laser wavelength by controllably adjusting the conditions of external light, electricity, atmosphere and the like, and provides a novel in-situ spectrum experimental technology, thereby being beneficial to more clearly displaying dynamic experimental information and summarizing an exact reaction mechanism.
Description
Technical Field
The invention relates to an in-situ Raman spectrum detection method, designs a related device according to a detection principle and application of the reaction device in a Raman spectrum instrument, and is suitable for in-situ spectrum testing and mechanism research in the fields of chemistry, materials and energy.
Background
In the field of basic research, photochemistry and electrochemistry are widely applied in the directions of new material synthesis, clean energy preparation, high value-added product conversion and the like. The final purpose of the research on the reaction process is to find out the optimized reaction conditions and provide a basis for industrial amplification, so that the professional promotion of the photo-electrochemical technology can replace the traditional high-energy-consumption and high-pollution industry in the future, and further lay a foundation for sustainable social production activities.
The intrinsic kinetics is like a black box, and the reaction mechanism must be studied deeply to reveal the reaction process in order to really understand how the reaction path proceeds. The conventional static microscopic and spectroscopic analysis method can only provide the non-working condition structural information of chemical substances before or after reaction, so that the analysis of the reaction process mainly depends on logical reasoning and imagination, and therefore, the development of a sensitive, efficient and real-time in-situ analysis means for capturing intermediate products and presuming a reaction path is very important. The in-situ Raman technology is a new practical spectrum technology matched with high-level scientific research requirements in recent years, has the advantages of nondestructive measurement, convenient sample preparation, high sample type compatibility, sensitivity to specific signal detection and the like of Raman detection, also has real-time detection and analysis capability, and provides strong support for mechanism research in reaction process science. Based on the above technical current situation, there is no in-situ raman reaction cell suitable for both photochemistry and electrochemistry on the market, so the technology in the field needs to be improved.
Disclosure of Invention
The invention aims to design a device for in-situ Raman detection suitable for photochemical, electrochemical and photoelectrochemical reactions aiming at the problem that the prior electrochemical experiment influences the experiment due to the lack of a corresponding experiment detection device, completes the connection with a Raman spectrometer, realizes in-situ optical/electrochemical Raman detection and provides a corresponding detection method.
One of the technical schemes of the invention is as follows:
a related device for in-situ optical/electrochemical Raman detection comprises an in-situ optical/electrochemical Raman reaction pool which can be used for in-situ photochemical reaction, in-situ electrochemical reaction or in-situ photoelectric reaction, and is characterized by mainly comprising: a reaction cell main body 1, a first electrode connecting hole groove 2-1, a second electrode connecting hole groove 2-2, a third electrode connecting hole groove 2-3, a light source connecting hole groove 3, a first atmosphere connecting hole groove/solution inlet/outlet hole groove 4-1, a second atmosphere connecting hole groove/solution inlet/outlet hole groove 4-2, a quartz optical window 5, a first adaptive electrode 6-1, a second adaptive electrode 6-2, a third adaptive electrode 6-3, an optical fiber conduit 7, a first hole groove gasket and sealing screw suite 8-1, a second hole groove gasket and sealing screw suite 8-2, a third hole groove gasket and sealing screw suite 8-3 and a fourth hole groove gasket and sealing screw suite 8-4, wherein the quartz optical window 5 is arranged on a reaction cell cavity body in the middle of the reaction cell main body 1, the first electrode connecting hole groove 2-3, the second adaptive electrode connecting hole groove/solution inlet/outlet hole groove 4, the quartz optical window 5, The second electrode connecting hole groove 2-2, the third electrode connecting hole groove 2-3 and the light source connecting hole groove 3 are distributed on the periphery of the reaction cell main body 1 and are communicated with the reaction cell cavity, the first hole groove gasket and the sealing screw suite 8-1, the second hole groove gasket and the sealing screw suite 8-2, the third hole groove gasket and the sealing screw suite 8-3 and the fourth hole groove gasket and the sealing screw suite 8-4 can be respectively screwed in the corresponding first electrode connecting hole groove 2-1, the second electrode connecting hole groove 2-2, the third electrode connecting hole groove 2-3 and the light source connecting hole groove 3 for plugging, and the first adaptive electrode 6-1, the second adaptive electrode 6-2, the third adaptive electrode 6-3 and the optical fiber guide tube 7 can penetrate through the corresponding first electrode connecting hole groove 2-1, the corresponding light source connecting hole groove 2-1 and the corresponding optical fiber guide tube 7 during corresponding experiments, The second electrode connecting hole groove 2-2, the third electrode connecting hole groove 2-3 and the light source connecting hole groove 3 enter the reaction tank cavity; the first atmosphere connecting hole groove/solution inlet/outlet hole groove 4-1 and the second atmosphere connecting hole groove/solution inlet/outlet hole groove 4-2 are both communicated with a reaction body cavity of the reaction tank main body 1, and are communicated with corresponding atmosphere sources or solutions through pipelines when the atmosphere sources or solutions are required to be connected.
The reaction tank main body 1 is separately externally connected with a light source controller, an electrochemical workstation or is simultaneously connected with the light source controller and the electrochemical workstation, and only is connected with the light source controller when only light reaction is carried out; only connecting the electrochemical workstation when only performing electric reaction; when the photoelectric reaction is carried out, the two are connected at the same time.
The reaction tank main body 1 is of a closed structure, and a quartz light window 5 is arranged in the center of the front side of the reaction tank main body to form a perspective window.
The reaction tank main body 1 should have chemical stability, corrosion resistance, sealing property, high lubrication non-stick property, electrical insulation property and good anti-aging endurance, and includes but is not limited to polytetrafluoroethylene.
The diameter of the quartz optical window 5 should comprehensively consider the sizes of relevant parts of the instrument, on one hand, the diameter of the optical window is not smaller than the diameter of the optical path so as to receive and feed back optical signals to the maximum extent, and on the other hand, a sufficient distance should be reserved between the diameter of the optical window and the boundary of the reaction cell so as to ensure the insertion and fixation of the electrode or the optical fiber catheter.
The heights of the openings of the first electrode connecting hole groove 2-1, the second electrode connecting hole groove 2-2, the third electrode connecting hole groove 2-3 and the light source connecting hole groove 3 are correspondingly staggered so as to control the fixed positions of the optical fiber catheter and the electrode not to interfere with each other and ensure the normal use of the light source and the electrode; all the hole grooves are spirally perforated and are provided with hole groove gaskets and sealing screw kits, so that the good tightness of all parts of the reaction tank is ensured when the reaction tank is used.
The first adaptive electrode 6-1 is arranged right below the perspective window, so that the optical instrument can detect the working electrode through the quartz optical window above the reaction cell body.
The second technical scheme of the invention is as follows:
the in-situ Raman detection method of each category based on the correlation device for in-situ optical/electrochemical Raman detection is characterized by comprising the following corresponding in-situ reaction devices and steps:
1 photochemical reaction in-situ Raman detection method, comprising the following steps: firstly, a first electrode connecting hole groove 2-1, a second electrode connecting hole groove 2-2 and a third electrode connecting hole groove 2-3 are respectively plugged by a first hole groove gasket and a sealing screw suite 8-1, a second hole groove gasket and a sealing screw suite 8-2 and a third hole groove gasket and a sealing screw suite 8-3, a light source connecting hole groove 3 is connected with an optical fiber guide pipe 7, and the optical fiber guide pipe 7 is connected with a light source controller; opening a quartz optical window 5, and filling a reaction sample, wherein a solid sample is placed in the center of the bottom of the reaction tank, and a liquid sample is injected into the cavity of the reaction tank; covering a quartz optical window 5 and screwing to a locking state, connecting the first atmosphere connecting hole groove/solution inlet/outlet hole groove 4-1 and the second atmosphere connecting hole groove/solution inlet/outlet hole groove 4-2 with corresponding gas cylinders or gas bags through gas pipes according to experimental atmosphere requirements, and if no special atmosphere requirement exists, not connecting the gas pipes and the atmosphere with the first atmosphere connecting hole groove/solution inlet/outlet hole groove 4-1 and the second atmosphere connecting hole groove/solution inlet/outlet hole groove 4-2; placing the assembled in-situ photochemical reaction tank in a sample measuring area of a Raman spectrometer, changing illumination parameters by adjusting a light source controller, and sampling data according to a conventional Raman detection method;
2 an electrochemical reaction in-situ raman detection method, comprising the following steps: step one, plugging a light source connecting hole groove 3 by using a fourth hole groove gasket and a sealing screw sleeve 8-4, preparing a first adaptive electrode 6-1, a second adaptive electrode 6-2 and a third adaptive electrode 6-3 according to the requirements of an experimental system sample, respectively connecting the first electrode connecting hole groove 2-1, the second electrode connecting hole groove 2-2 and the third electrode connecting hole groove 2-3 with the first adaptive electrode 6-1, the second adaptive electrode 6-2 and the third adaptive electrode 6-3, and connecting the first adaptive electrode 6-1, the second adaptive electrode 6-2 and the third adaptive electrode 6-3 with an electrochemical workstation; injecting electrolyte into the cavity of the reaction tank through a first atmosphere connecting hole groove/solution inlet/outlet hole groove 4-1 and a second atmosphere connecting hole groove/solution inlet/outlet hole groove 4-2 by using an injector or a pipette; step three, connecting the first atmosphere connecting hole groove/solution inlet/outlet hole groove 4-1 and the second atmosphere connecting hole groove/solution inlet/outlet hole groove 4-2 with corresponding gas cylinders or gas bags through gas pipes according to experimental atmosphere requirements, and if no special atmosphere requirement exists, connecting the gas pipes and the atmosphere in the first atmosphere connecting hole groove/solution inlet/outlet hole groove 4-1 and the second atmosphere connecting hole groove/solution inlet/outlet hole groove 4-2; placing the assembled in-situ electrochemical reaction cell in a sample measuring area of a Raman spectrometer, changing relevant parameters of the electrochemical reaction by setting an electrochemical workstation program, and sampling data according to a conventional Raman detection method;
3, the photoelectrochemical reaction in-situ Raman detection method comprises the following steps: step one, a light source connecting hole groove 3 is connected with an optical fiber conduit 7, the optical fiber conduit 7 is connected with a light source controller, a first electrode connecting hole groove 2-1, a second electrode connecting hole groove 2-2 and a third electrode connecting hole groove 2-3 are respectively connected with a first adaptive electrode 6-1, a second adaptive electrode 6-2 and a third adaptive electrode 6-3, and the first adaptive electrode 6-1, the second adaptive electrode 6-2 and the third adaptive electrode 6-3 are connected with an electrochemical workstation; opening a quartz optical window 5, loading a reaction sample, placing the reaction sample in the center of the bottom of the reaction tank, covering the quartz optical window 5, screwing the quartz optical window to a locked state, and injecting electrolyte into the cavity of the reaction tank through a first atmosphere connecting hole groove/solution inlet and outlet hole groove 4-1 and a second atmosphere connecting hole groove/solution inlet and outlet hole groove 4-2 by using an injector or a pipette; step three, connecting the first atmosphere connecting hole groove/solution inlet/outlet hole groove 4-1 and the second atmosphere connecting hole groove/solution inlet/outlet hole groove 4-2 with corresponding gas cylinders and gas bags through gas pipes according to experimental atmosphere requirements, and if no special atmosphere requirement exists, connecting the first atmosphere connecting hole groove/solution inlet/outlet hole groove 4-1 and the second atmosphere connecting hole groove/solution inlet/outlet hole groove 4-2) without connecting gas pipes and atmosphere; and step four, placing the assembled in-situ photoelectrochemical reaction tank in a sample measurement area of a Raman spectrometer, changing light reaction parameters by adjusting a light source controller, changing electric reaction parameters by setting an electrochemical workstation program, and sampling data according to a conventional Raman detection method.
The method can be used together with various optical instruments including in-situ Raman spectrum characterization, in-situ infrared spectrum characterization and in-situ ultraviolet-visible spectrum characterization as long as the space of a sample detection area is suitable.
The invention has the beneficial effects that:
the Raman spectrometer sample bin is suitable for being built in the Raman spectrometer sample bin and connected with a light source controller or an electrochemical workstation for realizing real-time Raman spectrum analysis of in-situ control of optical and electric reaction conditions. By controllably adjusting the conditions of external light, electricity, atmosphere and the like, the Raman spectrum is widened, the parameter dimensionality of laser power and laser wavelength can be changed only, and a novel in-situ spectrum experimental technology is provided, so that the dynamic experimental information can be more clearly displayed, and an exact reaction mechanism can be summarized.
The Raman spectrum detection device is simple in structure, easy to realize, capable of carrying out various existing Raman spectrum detections and capable of being conveniently expanded and applied.
Drawings
FIG. 1 is a perspective structural view of an in-situ reaction cell according to the present invention.
Fig. 2 is a schematic top view of the structure of fig. 1.
FIG. 3 is a schematic diagram of the instrument connections for the in situ photochemical Raman test of the present invention.
Fig. 4 is a schematic instrument connection for the in situ electrochemical raman test of the present invention.
FIG. 5 is a schematic instrument connection for the in situ photoelectrochemical Raman test of the present invention.
Detailed Description
The invention will be illustrated in detail below with reference to the drawings and examples, without limiting the invention thereto. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention.
As shown in fig. 1 and 2.
A related device for in-situ optical/electrochemical Raman detection comprises an in-situ optical/electrochemical Raman reaction pool which can be used for in-situ photochemical reaction, in-situ electrochemical reaction or in-situ photoelectric reaction, and mainly comprises: a reaction cell main body 1, a first electrode connection hole groove 2-1, a second electrode connection hole groove 2-2, a third electrode connection hole groove 2-3, a light source connection hole groove 3, a first atmosphere connection hole groove/solution inlet/outlet hole groove 4-1, a second atmosphere connection hole groove/solution inlet/outlet hole groove 4-2, a quartz optical window 5, a first adaptive electrode 6-1, a second adaptive electrode 6-2, a third adaptive electrode 6-3, an optical fiber conduit 7, a first hole groove gasket and sealing screw suite 8-1, a second hole groove gasket and sealing screw suite 8-2, a third hole groove gasket and sealing screw suite 8-3 and a fourth hole groove gasket and sealing screw suite 8-4, as shown in FIG. 2, the quartz optical window 5 is installed on a reaction cell cavity in the middle of the reaction cell main body 1, the first electrode connecting hole groove 2-1, the second electrode connecting hole groove 2-2, the third electrode connecting hole groove 2-3 and the light source connecting hole groove 3 are distributed on the periphery of the reaction tank main body 1 and are communicated with the reaction tank cavity, the first hole groove gasket and the sealing screw suite 8-1, the second hole groove gasket and the sealing screw suite 8-2, the third hole groove gasket and the sealing screw suite 8-3 and the fourth hole groove gasket and the sealing screw suite 8-4 can be respectively screwed in the corresponding first electrode connecting hole groove 2-1, the second electrode connecting hole groove 2-2, the third electrode connecting hole groove 2-3 and the light source connecting hole groove 3 for plugging, and the first adaptive electrode 6-1, the second adaptive electrode 6-2, the third adaptive electrode 6-3 and the optical fiber guide tube 7 can penetrate through the corresponding first electrode connecting hole groove 2-1, the corresponding second electrode connecting hole groove 2-2 and the corresponding optical fiber guide tube 7 during corresponding experiment, The second electrode connecting hole groove 2-2, the third electrode connecting hole groove 2-3 and the light source connecting hole groove 3 enter the reaction tank cavity; the first atmosphere connecting hole groove/solution inlet/outlet hole groove 4-1 and the second atmosphere connecting hole groove/solution inlet/outlet hole groove 4-2 are both communicated with a reaction body cavity of the reaction tank main body 1, and are communicated with corresponding atmosphere sources or solutions through pipelines when the atmosphere sources or solutions are required to be connected. The invention is suitable for in-situ detection devices of photochemical reaction, electrochemical reaction and photoelectrochemical reaction. The heights of the first adaptive electrode 6-1, the second adaptive electrode 6-2, the third adaptive electrode 6-3 and the optical fiber catheter 7 are staggered, as shown in figure 1.
Furthermore, each part of the in-situ reaction tank is designed according to different functions, the reaction tank main body 1 is closed, the center of the front surface is provided with a quartz optical window 5 for forming a perspective window, and the diameter of the quartz optical window is 35mm and is 1 in total; the first electrode connecting hole groove 2-1, the second electrode connecting hole groove 2-2 and the third electrode connecting hole groove 2-3 are used for connecting all functional electrodes, and the diameter is 10 mm, and the number of the functional electrodes is 3; the light source connecting hole grooves 3 are used for connecting optical fiber catheters, the diameter of each light source connecting hole groove is 15 mm, and the number of the light source connecting hole grooves is 1; the first atmosphere connecting hole groove/solution inlet and outlet hole groove 4-1 and the second atmosphere connecting hole groove/solution inlet and outlet hole groove 4-2 are used for connecting gas pipes without atmosphere, the diameter is 3 mm, and 2 gas pipes are arranged in one pipe and one pipe is arranged in the other pipe; when the experimental system is a solution, the atmosphere connecting hole groove can be used as a solution inlet and outlet hole groove at the same time, and the solution or cleaning solution is injected or led out from the holes without being divided into an inlet and an outlet, and the number of the holes is 2; all the holes are provided with hole gaskets and sealing screw kits with corresponding diameters so as to ensure the tightness of the reaction cell main body when the electrode or the optical fiber conduit is fixed, and the number of the holes is 4.
Further, according to the in-situ optical/electrochemical Raman detection method, when only light reaction is carried out, the light source controller is connected; when only the electric reaction is carried out, the electrochemical workstation is connected; when the photoelectric reaction is carried out, the two are connected at the same time. According to the in-situ Raman detection method of each category, the corresponding in-situ reaction device and steps thereof have the following preferred modes:
1) the photochemical reaction in-situ Raman detection method comprises the following steps: step one, plugging an electrode connecting hole groove with a hole groove gasket and a sealing screw sleeve respectively, connecting a light source connecting hole groove 3 with an optical fiber conduit 7, and connecting the optical fiber conduit 7 with a light source controller; opening a quartz optical window 5, and filling a reaction sample, wherein a solid sample is placed in the center of the bottom of the reaction tank, and a liquid sample is injected into the cavity of the reaction tank; covering a quartz optical window 5, screwing to a locking state, connecting the atmosphere connecting hole groove with a corresponding gas cylinder or gas bag through a gas pipe according to experimental atmosphere requirements, wherein the gas speed threshold is 10 mL/min, and if no special atmosphere requirement exists, the atmosphere connecting hole groove does not need to be connected with the gas pipe and atmosphere; and step four, placing the assembled in-situ photochemical reaction tank in a sample measuring area of a Raman spectrometer, changing illumination parameters by adjusting a light source controller, and sampling data according to a conventional Raman detection method.
2) The electrochemical reaction in-situ Raman detection method comprises the following steps: step one, plugging a light source connecting hole groove 3 by using a hole groove gasket and a sealing screw sleeve, preparing a working electrode according to the sample requirement of an experimental system, respectively connecting the electrode connecting hole groove with an adaptive electrode, and connecting the electrode with an electrochemical workstation; injecting electrolyte into the cavity of the reaction tank through the solution inlet and outlet hole groove; connecting the atmosphere connecting hole groove with a corresponding gas bottle or gas bag through a gas pipe according to experimental atmosphere requirements, wherein the gas speed threshold is 10 mL/min, and if no special atmosphere requirement exists, the atmosphere connecting hole groove does not need to be connected with the gas pipe and atmosphere; and step four, placing the assembled in-situ electrochemical reaction cell in a sample measuring area of a Raman spectrometer, changing relevant parameters of the electrochemical reaction by setting an electrochemical workstation program, and sampling data according to a conventional Raman detection method.
3) The photoelectrochemical reaction in-situ Raman detection method comprises the following steps: step one, a light source connecting hole groove 3 is connected with an optical fiber conduit 7, the optical fiber conduit 7 is connected with a light source controller, three electrode connecting hole grooves are respectively connected with three adaptive electrodes, and the three electrodes are all connected with an electrochemical workstation; opening a quartz optical window 5, loading a reaction sample, placing the reaction sample in the center of the bottom of the reaction tank, covering the quartz optical window 5, screwing the quartz optical window to a locked state, and injecting electrolyte into the cavity of the reaction tank through two solution inlet and outlet holes; connecting the two atmosphere connecting hole grooves with corresponding gas cylinders or gas bags through gas pipes according to experimental atmosphere requirements, wherein the gas velocity threshold is 10 mL/min, and if no special atmosphere requirement exists, the two atmosphere connecting hole grooves do not need to be connected with the gas pipes and atmosphere; and step four, placing the assembled in-situ photoelectrochemical reaction tank in a sample measurement area of a Raman spectrometer, changing light reaction parameters by adjusting a light source controller, changing electric reaction parameters by setting an electrochemical workstation program, and sampling data according to a conventional Raman detection method.
The reaction tank main body 1 material, a preferable embodiment, is polytetrafluoroethylene, which has excellent chemical stability, sealing property, corrosion resistance, high lubrication non-stick property, electrical insulation property and good anti-aging endurance.
According to the invention, a hole is formed right above the reaction tank main body 1, a quartz plate is placed as a quartz optical window 5 to form a perspective window, the aperture is larger than the diameter of an ocular lens of a Raman spectrometer, preferably, the aperture is 40 mm, and the diameter of an effective optical path is 35mm, so that optical signals are received and fed back to the maximum extent.
The electrode configuration of the in-situ reaction cell is provided with a first adaptive electrode (working electrode) 6-1, a second adaptive electrode (counter electrode) 6-2 and a third adaptive electrode (reference electrode) 6-3, and can be used for three-electrode experiments. Optionally, the reference electrode is a silver chloride electrode or a silver-silver ion electrode; the counter electrode is a platinum wire electrode; the working electrode clamp can be made of platinum, gold, titanium sheets and the like, and can clamp sheet materials such as sheets, plates, nets or conductive glass and the like. Preferably, in the invention, the reference electrode is a 6 mm silver-silver chloride electrode, the counter electrode is a platinum wire ring electrode with the diameter of 0.5X 37 mm, the working electrode is a platinum electrode clamp, and the size of a platinum sheet is 5X 0.1 mm. Preferably, the working electrode is arranged right below the perspective window, so that the optical instrument can detect the working electrode through the quartz optical window above the reaction cell body.
The height and the mode of the holes of the hole groove of the in-situ reaction pool are preferably selected, the heights of the holes of the first electrode connecting hole groove 2-1, the second electrode connecting hole groove 2-2, the third electrode connecting hole groove 2-3 and the light source connecting hole groove 3 are correspondingly staggered, and the fixed positions of the optical fiber conduit 7 and the first adaptive electrode 6-1, the second adaptive electrode 6-2 and the third adaptive electrode 6-3 are controlled not to interfere with each other, so that the normal use of the light source and the electrodes is ensured; in addition, all the hole grooves (the first electrode connecting hole groove 2-1, the second electrode connecting hole groove 2-2, the third electrode connecting hole groove 2-3, the light source connecting hole groove 3, the first atmosphere connecting hole groove/solution inlet/outlet hole groove 4-1 and the second atmosphere connecting hole groove/solution inlet/outlet hole groove 4-2) are spirally perforated and are provided with a first hole groove gasket and sealing screw suite 8-1, a second hole groove gasket and sealing screw suite 8-2, a third hole groove gasket and sealing screw suite 8-3 and a fourth hole groove gasket and sealing screw suite 8-4 so as to ensure that each part of the reaction tank is well sealed when in use.
The first atmosphere connecting hole groove/solution inlet and outlet hole groove 4-1 and the second atmosphere connecting hole groove/solution inlet and outlet hole groove 4-2 are used for connecting air pipes with different atmospheres, and preferably, air pipes with the diameter of 3 multiplied by 0.5mm are matched.
The device or the method related to the invention can be preferably used together with various optical instruments as long as the space of a sample detection area is suitable, and the device or the method can be preferably used in catalytic in-situ characterization, and comprises but not limited to in-situ Raman spectrum characterization, and can be expanded to in-situ infrared spectrum characterization, in-situ ultraviolet-visible spectrum characterization and the like.
Example 1.
As shown in fig. 3.
Black phosphorus CO2In-situ raman studies of photoreduction.
Experimental apparatus: referring to fig. 3, the instrument connection diagram of the in-situ photochemical raman test includes a laser raman spectrometer, a light source controller and an in-situ photochemical reaction cell connected thereto. All the electrode connecting hole grooves are plugged by using hole groove gaskets and sealing screw kits, the light source connecting hole grooves are inserted into the optical fiber guide pipe and are fixed at a proper position through the gaskets and the sealing screw kits, so that the surface of the sample is ensured to receive illumination; the gas pipe is inserted into the atmosphere connecting hole groove and is connected with corresponding atmosphere through the gas pipe.
The experimental method comprises the following steps: in the example, a Thermo-fisher DXR laser micro-confocal Raman spectrometer, a 250W xenon lamp medical cold light source controller and the in-situ reaction tank provided by the invention are selected as experimental instruments. The experimental steps are as follows: firstly, 10mg of black phosphorus is put into an in-situ photochemical reaction tank provided by the invention; installing a first hole groove gasket and a sealing screw suite 8-1, a second hole groove gasket and a sealing screw suite 8-2, a third hole groove gasket and a sealing screw suite 8-3 corresponding to the first electrode connecting hole groove 2-1, the second electrode connecting hole groove 2-2 and the third electrode connecting hole groove 2-3, connecting an optical fiber guide pipe 7 and calibrating light spots, and enabling the light spots to be irradiated at the position of a catalyst in an experiment; injecting 10mL of acetonitrile, 2mL of secondary water and 1mL of triethanolamine into the first atmosphere connecting hole groove/solution inlet and outlet hole groove 4-1; CO 22The atmosphere is connected into the solution through an atmosphere connecting hole groove by a gas pipe with the diameter of 3 multiplied by 0.5mm, a gas inlet is a first atmosphere connecting hole groove/solution inlet and outlet hole groove 4-1, and a gas outlet is a second atmosphere connecting hole groove/solution inlet and outlet hole groove 4-2; placing the connected in-situ photochemical reaction tank in an observation area of a Raman spectrometer, adjusting the position of an ocular lens to align with a quartz optical window 5 and focusing a sample; pre-introducing CO2Controlling the flow rate to be 30-40mL/min under the atmosphere, ventilating for 5min to remove system air, and collecting a precursor system Raman signal as a comparison sample at the beginning of an experiment; turning on a light source controller, setting the intensity of a light source to be 50%, and performing Raman sampling every 2min, wherein relevant parameters are as follows: the Raman laser wavelength is 532 nm, the laser power is 2mW, the exposure time is 2s, and the exposure frequency is 50 times.
Example 2.
As shown in fig. 4.
Two-electrode in-situ Raman electrochemical test surface state change experiment.
Experimental apparatus: referring to fig. 4, the instrument connection diagram of the in-situ electrochemical raman test includes a laser raman spectrometer, an electrochemical workstation and the in-situ reaction cell provided by the present invention. The light source connecting hole groove is plugged by a hole groove gasket and a sealing screw suite, the electrode connecting hole groove is respectively connected with corresponding electrodes, the electrodes are connected with an electrochemical workstation, and the electrodes are fixed at proper positions by the hole groove gasket and the sealing screw suite, so that the normal use of each electrode is ensured; the gas pipe is inserted into the atmosphere connecting hole groove and is connected with corresponding atmosphere through the gas pipe.
The experimental method comprises the following steps: in this example, a Thermo-fisher DXR laser micro-confocal raman spectrometer, a shanghai Huachi 660e electrochemical workstation, and an in-situ reaction cell provided by the present invention were selected as experimental instruments. Sodium alginate is used as a precursor to prepare the C-based composite material active substance, and the C-based composite material active substance is used for a lithium ion electrode negative electrode material. Specifically, 8 mgC-based composite material, 1mg PVDF and 1mg superconducting carbon black are mixed and added with NMP solution to be ground uniformly to prepare slurry, the slurry is uniformly coated on a copper foil, and the slurry is dried in vacuum for later use; li is prepared by taking Li sheets as a counter electrode and a reference electrode 2-1 and taking the electrode sheets prepared by the method as working electrodes+A half cell; lithium hexafluorophosphate is used as electrolyte and is placed in the in-situ reaction tank provided by the invention, the No. 2 to the No. 2 is used as a positive electrode, the No. 2 to the No. 3 is connected with a negative electrode, and the charge and discharge test is carried out at the current density of 0.1A/g; raman sampling is carried out every 2min, and the related parameters are as follows: the wavelength of the Raman laser is 532 nm, the laser power is 2mW, the exposure time is 2s, and the exposure times are 50 times.
Example 3.
As shown in fig. 5.
Research on an in-situ mechanism of photoelectrocatalysis degradation RhB.
Experimental apparatus: referring to fig. 5, the instrument connection diagram of the in-situ photoelectrochemical raman test includes a laser raman spectrometer, an electrochemical workstation, a light source controller and an in-situ reaction cell connected thereto. The light source connecting hole slot is inserted into the optical fiber conduit and is fixed at a proper position through a gasket and a sealing screw sleeve, so that the surface of the sample is ensured to receive illumination; connecting the electrode connecting hole grooves with corresponding electrodes respectively, connecting the electrodes with an electrochemical workstation, and fixing the electrodes at proper positions through hole groove gaskets and sealing screw kits so as to ensure that each electrode is normally used; the gas pipe is inserted into the atmosphere connecting hole groove and is connected with corresponding atmosphere through the gas pipe.
The experimental method comprises the following steps: in this example, a Thermo-fisher DXR laser micro-confocal raman spectrometer, a 250W xenon lamp medical cold light source controller, a shanghai Huachi 660e electrochemical workstation and the in-situ reaction cell provided by the present invention were selected as experimental instruments. Fe prepared by experiment2O3The photoelectric electrode is an anode and is connected with 2-2, Pt is a cathode and is connected with 2-3, and the silver-silver chloride electrode is a reference electrode and is connected with 2-1; connecting the optical fiber conduit 7, checking air tightness and calibrating light spots so as to enable the light spots to be irradiated at the positions of the photoelectrode in the experiment; injecting 10mL 5 mg.L initial concentration into the first atmosphere connection hole groove/solution inlet/outlet hole groove 4-1-1The RhB model pollutant is probe molecule, air atmosphere is connected to the solution through an air pipe with the diameter of 3 multiplied by 0.5mm from an atmosphere connecting hole groove, an air inlet is a first atmosphere connecting hole groove/solution inlet and outlet hole groove 4-1, an air outlet is a second atmosphere connecting hole groove/solution inlet and outlet hole groove 4-2, air needs to be continuously introduced in the reaction process, and the flow is controlled to be 0.1 L.min-1(ii) a An electrochemical workstation of Chenghuchi 660e is used for providing an external bias voltage, recording the real-time change of functional groups on the surface of the catalyst under different bias voltage conditions, and recording the change of photocurrent in the reaction process; raman sampling is carried out every 1min under each bias condition, and relevant parameters are as follows: the wavelength of the Raman laser is 633 nm, the laser power is 5mW, the exposure time is 1s, and the exposure times are 30 times.
It should be noted that by referring to the exemplary embodiments, substitutions and modifications can be made according to ordinary skill in the art and conventional means without departing from the above-described ideas of the present invention and within the scope of the claims of the present invention, and the present invention can be extended to all applications of the same function. All other embodiments obtained by a person skilled in the art without making any inventive step are intended to be included within the scope of protection of the present invention.
The present invention is not concerned with parts which are the same as or can be implemented using prior art techniques.
Claims (9)
1. A related device for in-situ optical/electrochemical Raman detection comprises an in-situ optical/electrochemical Raman reaction pool which can be used for in-situ photochemical reaction, in-situ electrochemical reaction or in-situ photoelectric reaction, and is characterized by mainly comprising: a reaction cell main body (1), a first electrode connecting hole groove (2-1), a second electrode connecting hole groove (2-2), a third electrode connecting hole groove (2-3), a light source connecting hole groove (3), a first atmosphere connecting hole groove/solution inlet and outlet hole groove (4-1), a second atmosphere connecting hole groove/solution inlet and outlet hole groove (4-2), a quartz optical window (5), a first adaptive electrode (6-1), a second adaptive electrode (6-2), a third adaptive electrode (6-3), an optical fiber conduit (7), a first hole groove gasket and sealing screw suite (8-1), a second hole groove gasket and sealing screw suite (8-2), a third hole groove gasket and sealing screw suite (8-3) and a fourth hole groove gasket and sealing screw suite (8-4), the quartz optical window (5) is arranged on a reaction tank cavity in the middle of the reaction tank main body (1), the first electrode connecting hole groove (2-1), the second electrode connecting hole groove (2-2), the third electrode connecting hole groove (2-3) and the light source connecting hole groove (3) are distributed on the periphery of the reaction tank main body (1) and are communicated with the reaction tank cavity, the first hole groove gasket and the sealing screw suite (8-1), the second hole groove gasket and the sealing screw suite (8-2), the third hole groove gasket and the sealing screw suite (8-3) and the fourth hole groove gasket and the sealing screw suite (8-4) can be respectively screwed in the corresponding first electrode connecting hole groove (2-1), the second electrode connecting hole groove (2-2), the third electrode connecting hole groove (2-3) and the light source connecting hole groove (3) for plugging, the first adaptive electrode (6-1), the second adaptive electrode (6-2), the third adaptive electrode (6-3) and the optical fiber conduit (7) can penetrate through the corresponding first electrode connecting hole groove (2-1), the second electrode connecting hole groove (2-2), the third electrode connecting hole groove (2-3) and the light source connecting hole groove (3) to enter the cavity of the reaction tank during corresponding experiments; the first atmosphere connecting hole groove/solution inlet and outlet hole groove (4-1) and the second atmosphere connecting hole groove/solution inlet and outlet hole groove (4-2) are communicated with a reaction body cavity of the reaction tank main body (1), and are communicated with corresponding atmosphere sources or solutions through pipelines when the atmosphere sources or solutions need to be connected.
2. The apparatus as claimed in claim 1, wherein the reaction cell body (1) is separately connected to a light source controller, an electrochemical workstation or both, and is connected to only the light source controller during the light reaction; only connecting the electrochemical workstation when only performing electric reaction; when the photoelectric reaction is carried out, the two are connected at the same time.
3. The apparatus as claimed in claim 1, wherein the reaction cell body (1) is a closed structure, and the front center is a quartz window (5) for forming a see-through window.
4. The device as claimed in claim 1, wherein the reaction chamber body (1) is made of a material having chemical stability, corrosion resistance, sealing property, high lubrication non-sticking property, electrical insulation property and good aging resistance, including but not limited to polytetrafluoroethylene.
5. The apparatus as claimed in claim 1, wherein the diameter of the quartz optical window (5) is determined by taking the size of the related components of the apparatus into consideration, on one hand, the diameter of the optical window is not smaller than the diameter of the optical path to maximize the receiving and feedback of the optical signal, and on the other hand, the diameter of the optical window is spaced from the boundary of the reaction cell by a sufficient distance to ensure the insertion and fixation of the electrode or the optical fiber catheter.
6. The apparatus as claimed in claim 1, wherein the height of the first electrode connecting hole (2-1), the second electrode connecting hole (2-2), the third electrode connecting hole (2-3), and the light source connecting hole (3) are staggered to control the fixing positions of the fiber optic catheter and the electrode not to interfere with each other, so as to ensure the normal use of the light source and the electrode; all the hole grooves are spirally perforated and are provided with hole groove gaskets and sealing screw kits, so that the good tightness of all parts of the reaction tank is ensured when the reaction tank is used.
7. The apparatus as claimed in claim 1, wherein the first adaptive electrode (6-1) is disposed directly below the see-through window, so that the optical instrument can detect the working electrode through the quartz window above the reaction cell body.
8. The in-situ Raman detection method of each category based on the correlation device for in-situ optical/electrochemical Raman detection is characterized by comprising the following corresponding in-situ reaction devices and steps:
1) the photochemical reaction in-situ Raman detection method comprises the following steps: firstly, a first electrode connecting hole groove (2-1), a second electrode connecting hole groove (2-2) and a third electrode connecting hole groove (2-3) are respectively plugged by a first hole groove gasket and a sealing screw suite (8-1), a second hole groove gasket and a sealing screw suite (8-2), a third hole groove gasket and a sealing screw suite (8-3), a light source connecting hole groove (3) is connected with an optical fiber guide pipe (7), and the optical fiber guide pipe (7) is connected with a light source controller; opening a quartz optical window (5), and filling a reaction sample, wherein the solid sample is placed in the center of the bottom of the reaction tank, and the liquid sample is injected into the cavity of the reaction tank; covering a quartz optical window (5) and screwing to a locking state, connecting the first atmosphere connecting hole groove/solution inlet and outlet hole groove (4-1) and the second atmosphere connecting hole groove/solution inlet and outlet hole groove (4-2) with corresponding gas cylinders or gas bags through gas pipes according to experimental atmosphere requirements, and if no special atmosphere requirement exists, connecting the gas pipes and the atmosphere with the first atmosphere connecting hole groove/solution inlet and outlet hole groove (4-1) and the second atmosphere connecting hole groove/solution inlet and outlet hole groove (4-2); placing the assembled in-situ photochemical reaction tank in a sample measuring area of a Raman spectrometer, changing illumination parameters by adjusting a light source controller, and sampling data according to a conventional Raman detection method;
2) the electrochemical reaction in-situ Raman detection method comprises the following steps: step one, plugging a light source connecting hole groove (3) by using a fourth hole groove gasket and a sealing screw sleeve member (8-4), preparing a first adaptive electrode (6-1), a second adaptive electrode (6-2) and a third adaptive electrode (6-3) according to the requirements of an experimental system sample, respectively connecting the first electrode connecting hole groove (2-1), the second electrode connecting hole groove (2-2) and the third electrode connecting hole groove (2-3) with the first adaptive electrode (6-1), the second adaptive electrode (6-2) and the third adaptive electrode (6-3), and connecting the first adaptive electrode (6-1), the second adaptive electrode (6-2) and the third adaptive electrode (6-3) with an electrochemical workstation; injecting electrolyte into the cavity of the reaction tank through a first atmosphere connecting hole groove/solution inlet and outlet hole groove (4-1) and a second atmosphere connecting hole groove/solution inlet and outlet hole groove (4-2) by using an injector or a pipette; step three, connecting the first atmosphere connecting hole groove/solution inlet and outlet hole groove (4-1) and the second atmosphere connecting hole groove/solution inlet and outlet hole groove (4-2) with corresponding gas cylinders or gas bags through gas pipes according to experimental atmosphere requirements, and if no special atmosphere requirement exists, connecting the first atmosphere connecting hole groove/solution inlet and outlet hole groove (4-1) and the second atmosphere connecting hole groove/solution inlet and outlet hole groove (4-2) without connecting the gas pipes and the atmosphere; placing the assembled in-situ electrochemical reaction cell in a sample measuring area of a Raman spectrometer, changing relevant parameters of the electrochemical reaction by setting an electrochemical workstation program, and sampling data according to a conventional Raman detection method;
3) the photoelectrochemical reaction in-situ Raman detection method comprises the following steps: the method comprises the following steps that firstly, a light source connecting hole groove (3) is connected with an optical fiber conduit (7), the optical fiber conduit (7) is connected with a light source controller, a first electrode connecting hole groove (2-1), a second electrode connecting hole groove (2-2) and a third electrode connecting hole groove (2-3) are respectively connected with a first adaptive electrode (6-1), a second adaptive electrode (6-2) and a third adaptive electrode (6-3), and the first adaptive electrode (6-1), the second adaptive electrode (6-2) and the third adaptive electrode (6-3) are connected with an electrochemical workstation; opening a quartz optical window (5), loading a reaction sample, placing the reaction sample in the center of the bottom of the reaction tank, covering the quartz optical window (5), screwing the quartz optical window to a locked state, and injecting electrolyte into the cavity of the reaction tank through a first atmosphere connecting hole groove/solution inlet and outlet hole groove (4-1) and a second atmosphere connecting hole groove/solution inlet and outlet hole groove (4-2) by using an injector or a pipette; step three, connecting the first atmosphere connecting hole groove/solution inlet and outlet hole groove (4-1) and the second atmosphere connecting hole groove/solution inlet and outlet hole groove (4-2) with corresponding gas cylinders and gas bags through gas pipes according to experimental atmosphere requirements, and if no special atmosphere requirement exists, connecting the first atmosphere connecting hole groove/solution inlet and outlet hole groove (4-1) and the second atmosphere connecting hole groove/solution inlet and outlet hole groove (4-2) without connecting the gas pipes and atmosphere; and step four, placing the assembled in-situ photoelectrochemical reaction tank in a sample measurement area of a Raman spectrometer, changing light reaction parameters by adjusting a light source controller, changing electric reaction parameters by setting an electrochemical workstation program, and sampling data according to a conventional Raman detection method.
9. The method of claim 8, wherein the method is used with a variety of optical instruments as long as the sample detection region is spatially appropriate, including in situ raman spectroscopy, in situ infrared spectroscopy, and in situ uv-vis spectroscopy.
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