CN112924434A - Electrochemical cell for in-situ Raman test of flow battery - Google Patents
Electrochemical cell for in-situ Raman test of flow battery Download PDFInfo
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- CN112924434A CN112924434A CN202110079033.XA CN202110079033A CN112924434A CN 112924434 A CN112924434 A CN 112924434A CN 202110079033 A CN202110079033 A CN 202110079033A CN 112924434 A CN112924434 A CN 112924434A
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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
- G01N21/62—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
- 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
- G01N27/403—Cells and electrode assemblies
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/18—Regenerative fuel cells, e.g. redox flow batteries or secondary fuel cells
- H01M8/184—Regeneration by electrochemical means
- H01M8/188—Regeneration by electrochemical means by recharging of redox couples containing fluids; Redox flow type batteries
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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
- G01N21/62—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
- G01N2021/651—Cuvettes therefore
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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Abstract
The invention relates to an electrochemical cell for in-situ Raman testing of a flow battery, which meets the operation requirement of the flow battery, and simultaneously, by selecting glass or a polymer film which does not absorb specific wave bands as a window and integrating the window with a current collector of an electrode to be tested, laser is directly irradiated on a fluid electrode, Raman signals are synchronously collected in the charging and discharging processes of the battery, and the in-situ characterization of the electrochemical reaction process of the flow battery is realized. In addition, the volume of the cavity in the electrochemical cell is adjustable, and the requirement of complex flow channel design can be met. The flow battery in-situ Raman test electrochemical cell provided by the invention has the advantages of simple structure, convenience in assembly, accurate test result, wide application range and the like, and has profound significance for determining the charge and discharge mechanism of the flow battery and exerting the large-scale energy storage application potential of the flow battery.
Description
Technical Field
The invention belongs to the field of electrochemistry, and relates to a flow battery in-situ Raman testing electrochemical cell.
Background
The flow battery is a large-scale and efficient electrochemical energy storage system, and is characterized in that electrode active substances are dissolved or dispersed in electrolyte to form a fluid electrode with fluidity, and mutual conversion between electric energy and chemical energy is carried out through redox reaction to realize storage and release of the electric energy. In the process of charging and discharging the flow battery, an external pump drives a fluid electrode to circulate between the battery pile and the liquid storage tank. The structure that the battery stack and the active material are separated from each other enables the flow battery system to independently design the output power and the energy storage capacity of the battery so as to meet different use requirements. Therefore, the flow battery has long service life, high safety and large-scale energy storage application prospect. In the process of flow battery research, the progress of the characterization technology is important for the performance optimization of the flow battery and the development of a new system flow battery. The Raman spectrum technology is used as a commonly used characterization means in material chemical research, and has the advantages of high analysis speed, high repeatability, capability of performing nondestructive qualitative and quantitative analysis on materials and the like. The Raman spectrum technology can directly obtain the structure, the composition and the chemical bond state of the fluid electrode by detecting molecular vibration, and has important scientific significance and application value for determining the ion removal/insertion process of active substances and further presuming the electrochemical reaction mechanism of the flow battery.
At present, Raman spectrum testing has two modes of in-situ characterization and ex-situ characterization. Because the active substance of the flow battery exists in the flowing electrolyte, the problems of electrolyte solvent volatilization, system pollution, active substance structure damage and the like are easily caused in the sample preparation process by ex-situ characterization, and the accuracy of the test result is influenced. In addition, due to the fact that the charging and discharging states of different batteries are different, a certain error exists in the ex-situ characterization result. In contrast, in-situ Raman characterization can synchronously acquire Raman signals of the material in the battery charging and discharging process, so that the material structure and composition change information is obtained in real time, and the spectrogram accuracy is higher. At present, the common in-situ battery Raman testing devices comprise a button type device and a flange plate type device, but the two devices do not comprise an internal electrolyte flow channel and a circulating device, and the operation requirements of the flow battery cannot be met. In addition, the flow battery electrode is in a flowing state, so that the requirement on the tightness of the testing device is high. Therefore, it is imperative to design an in-situ raman spectroscopy testing device that matches the flow cell system.
The invention provides a redox flow battery in-situ Raman test electrochemical cell, which can meet the operation requirement of a redox flow battery, can synchronously acquire Raman signals of materials in the charging and discharging processes of the battery, has the advantages of simple structure, convenience in assembly, accurate test result, wide application range and the like, and has profound significance for defining the charging and discharging mechanism of the redox flow battery and exerting the large-scale energy storage application potential of the redox flow battery.
The invention content is as follows:
the invention aims to provide a flow battery in-situ Raman test electrochemical cell aiming at the defects of the existing characterization technology, so as to meet the requirement of the flow battery for synchronously acquiring Raman signals of active substances in the charging and discharging processes and obtain more accurate structure and composition change information of an electrode material.
The technical scheme of the invention is as follows:
an electrochemical cell for in-situ Raman testing of a flow battery comprises a housing, a feed and discharge interface, a window and a current collector. The shell comprises an upper seat, a sealing gasket and a base, and the upper seat, the sealing gasket and the base are connected in a mechanical mode to realize sealing. The material inlet and outlet interfaces are arranged on two sides of the shell and integrated with the sealing gasket. An opening is formed in the middle of the current collector of the electrode to be measured, and glass or a polymer film which does not absorb specific wave bands is carried to serve as a window according to different incident waves, so that laser is directly irradiated onto the fluid electrode to collect Raman signals.
The upper seat and the base do not have side reaction with the electrolyte, and the material can be polytetrafluoroethylene, polymethyl methacrylate, polyethylene terephthalate, polycarbonate resin, polyformaldehyde resin and other high polymer insulating materials.
The sealing gasket is good in elastic deformation and free of side reaction with electrolyte, the material of the sealing gasket can be silica gel, nitrile rubber, isoprene rubber, ethylene propylene rubber and other high polymer insulating materials, and the thickness of the sealing gasket can be adjusted according to the volume requirement of the inner cavity of the fluid electrode.
The mechanical connection mode can realize shell sealing and prevent liquid leakage and can be a connection mode such as rivet connection, screw connection, hole drawing riveting, clamping hook connection, gluing connection, expansion connection, seaming connection and the like.
The material of the feeding and discharging interface has no side reaction with the electrolyte, and can be polymer insulating materials such as polytetrafluoroethylene, polymethyl methacrylate, polyethylene terephthalate, polycarbonate resin, polyformaldehyde resin and the like.
The window has high light transmittance, the material can be quartz, borosilicate glass, sapphire, polyethylene terephthalate and other glass or polymer film which do not absorb the fixed wave band of the incident baud in the test, and the thickness is 0.1-1 mm.
The current collector has excellent conductivity, and the material of the current collector can be metal materials such as aluminum, copper, titanium, nickel, stainless steel and the like.
The invention has the advantages that:
1. the invention provides an electrochemical cell for in-situ Raman testing of a flow battery, wherein the top of the electrochemical cell adopts a window structure, and according to different incident waves, a glass or polymer film which does not absorb a specific wave band is selected as a window, so that Raman testing laser is directly irradiated on a fluid electrode, Raman signals are synchronously acquired in the charging and discharging processes of the flow battery, the information of material structure and composition change is obtained, and the spectrogram accuracy is higher.
2. The invention can be suitable for various water system or non-water system flow battery energy storage systems, such as all-vanadium flow batteries, zinc-bromine flow batteries, lead-acid flow batteries, semi-solid lithium-sulfur flow batteries and the like, and has wide application range.
3. The volume of the cavity in the electrochemical cell can be adjusted by changing the thickness of the sealing gasket, and the requirement of complex flow channel design can be met.
4. The device has simple structure and convenient disassembly and assembly, and can be operated under various working conditions such as a glove box and the like.
Drawings
Fig. 1 is a schematic structural diagram of a flow cell in-situ raman testing electrochemical cell of the present invention.
Fig. 2 is a first-turn constant-current charging and discharging curve of the semi-solid lithium flow battery according to the embodiment of the present invention.
Fig. 3 is an in-situ raman spectrum of the semi-solid lithium flow battery in the first constant current charging and discharging process according to the embodiment of the present invention.
In the figure: 1: window, 2: fluid positive electrode, 3: positive electrode current collector, 4: upper seat, 5: inlet and outlet interface, 6: gasket, 7: negative electrode, 8: base, 9: negative electrode current collector, 10: a diaphragm.
Detailed Description
The invention will be further explained and illustrated with reference to specific examples.
The invention takes a semisolid lithium flow battery as an example, and carries out in-situ Raman characterization on the structural change of a lithium iron phosphate fluid anode in the charging and discharging processes.
Example (b):
as shown in figure 1, the shell of the invention consists of an upper seat 4, a sealing gasket 6 and a base 8, wherein the upper seat 4 and the base 8 are made of polytetrafluoroethylene, the sealing gasket 6 is made of silica gel, and the upper seat 4 and the base 8 are tightly connected through bolts and nuts to realize sealing. The material of the material inlet and outlet interface 5 is polycarbonate resin, is positioned on two sides of the shell, has a height close to that of the inner cavity of the fluid anode 2, is arranged on a reserved hole of the sealing gasket 6, and the joint is sealed by silica gel to prevent slurry leakage. The positive current collector 3 is aluminum foil with a middle design of 0.5 multiplied by 0.5cm2And is opened so that the laser is directly irradiated onto the fluid cathode 2. The window 1 is made of quartz and has a size of 0.8 × 0.8cm2And the thickness is 0.2mm, and the silicon gel is sealed above the opening of the positive current collector 3. The lithium iron phosphate slurry is used as a fluid anode 2, wherein the active material is lithium iron phosphate, the conductive agent is ketjen black, and a mixed solution containing 1mol/L of lithium bis (trifluoromethyl) sulfonimide and 3:7 by volume of ethylene carbonate and dimethyl carbonate is used as an electrolyte. The diaphragm 10 is made of polypropylene diaphragm, the negative electrode 7 is made of lithium sheet, and the negative current collector 9 is made of copper foil.
As different embodiments of the present invention, the materials used for the upper seat 4 and the base 8, the gasket 6, the inlet/outlet port 5, the window 1, and the current collector are not limited to those described in the above embodiments, wherein the materials of the upper seat 4 and the base 8 include but are not limited to a polymer insulating material selected from polytetrafluoroethylene, polymethyl methacrylate, polyethylene terephthalate, polycarbonate, and polyoxymethylene resin; the material of the sealing gasket 6 comprises but is not limited to a high polymer insulating material of silica gel, nitrile rubber, isoprene rubber and ethylene propylene rubber; the material of the inlet and outlet interface 5 includes but is not limited to a high polymer insulating material selected from polytetrafluoroethylene, polymethyl methacrylate, polyethylene terephthalate, polycarbonate and polyoxymethylene resin; the material of the window 1 includes but is not limited to one of quartz, borosilicate glass, sapphire and polyethylene terephthalate; the current collector material includes, but is not limited to, a metal material selected from aluminum, copper, titanium, nickel, stainless steel, etc. The selection of the materials can achieve the purpose of the invention and achieve the technical effect of the invention.
Electrochemical performance of the semi-solid lithium flow battery assembled by using the in-situ Raman testing device is tested, and the graph of FIG. 2 shows that the semi-solid lithium flow battery is 0.2mA/cm2Constant current charge and discharge curve under current density. The specific capacity of the semi-solid lithium flow battery is 131.7mAh/g, which shows that the semi-solid lithium flow battery assembled by the device operates normally. The structural change of the lithium iron phosphate fluid electrode in the charging and discharging process is characterized by using a laser confocal Raman spectrometer, wherein the laser wavelength is 532nm, the laser power is 12.5mW, the single spectrum acquisition time is 4s, and the Raman spectrum is shown in figure 3. Curve 1 is the initial state, curve 2 is the state after the first turn is fully charged, and curve 3 is the state after the first turn is fully discharged. 947cm when fully charged-1And 1085cm-1And a stretching vibration peak of phosphate radical appears, which indicates that lithium ions are separated from the lithium iron phosphate and the lithium iron phosphate is converted into the iron phosphate. And then the battery is completely discharged, and the expansion vibration peak of the phosphate radical disappears, which indicates that lithium ions are inserted into ferric phosphate to form lithium iron phosphate. The in-situ Raman characterization result clearly shows the structural change of the lithium iron phosphate in the charging and discharging processes, and the effectiveness of the in-situ Raman testing electrochemical cell is proved.
The above examples are only intended to illustrate the present description and should not be construed as imposing any limitation on the scope of the present description. Also, it will be apparent to those skilled in the art that various equivalent changes, modifications and improvements not described herein can be made to the present invention without departing from the spirit and principles of the invention.
Claims (9)
1. The electrochemical cell for the in-situ Raman test of the flow battery is characterized by comprising a shell, a feeding and discharging interface, a window and a current collector, wherein the shell comprises an upper seat, a sealing gasket and a base, the upper seat, the sealing gasket and the base are tightly connected in a mechanical mode and realize sealing, the feeding and discharging interface is installed on two sides of the shell and integrated with the sealing gasket, an opening is formed in the middle of the current collector of an electrode to be tested, glass or a polymer film which does not absorb specific wave bands is carried as the window according to different incident waves, laser is directly irradiated onto the fluid electrode to collect Raman signals, and in-situ characterization is realized.
2. The electrochemical cell for in-situ raman testing of flow batteries according to claim 1, suitable for use in a variety of aqueous or non-aqueous flow battery energy storage systems, including but not limited to all-vanadium flow batteries, zinc-bromine flow batteries, lead-acid flow batteries, semi-solid lithium-sulfur flow batteries.
3. The electrochemical cell for in-situ raman testing of flow batteries according to claim 1, wherein the upper and base are free of side reactions with electrolytes including but not limited to a polymer insulating material selected from the group consisting of polytetrafluoroethylene, polymethylmethacrylate, polyethylene terephthalate, polycarbonate, polyoxymethylene resin.
4. The electrochemical cell for in-situ raman testing of flow batteries according to claim 1, wherein the gasket is elastically deformed without side reaction with an electrolyte, including but not limited to a polymer insulating material selected from the group consisting of silica gel, nitrile rubber, isoprene rubber, and ethylene propylene rubber, and the thickness thereof is adjusted according to the volume requirement of the inner cavity of the fluid electrode.
5. The electrochemical cell for in situ raman testing of flow cells of claim 1, wherein the mechanical connection of the upper seat, the gasket, and the base of the housing enables the housing to be sealed against fluid leakage, including but not limited to one of a pop-up connection, a screw connection, a pop-up rivet connection, a snap-in connection, an adhesive connection, an expansion joint, and a snap-in connection.
6. The electrochemical cell for in-situ raman testing of flow batteries of claim 1, wherein the inlet and outlet ports are free of side reactions with electrolytes, including but not limited to a polymer insulating material selected from the group consisting of polytetrafluoroethylene, polymethylmethacrylate, polyethylene terephthalate, polycarbonate, polyoxymethylene resin.
7. The electrochemical cell for in-situ raman testing of flow cells of claim 1 wherein the window has a high light transmittance, including but not limited to one of quartz, borosilicate glass, sapphire, polyethylene terephthalate, a glass or polymer film that is non-absorbing in the fixed band of the incident baud in the test, and has a thickness between 0.1 and 1 mm.
8. The electrochemical cell for in-situ raman testing of flow batteries according to claim 1, wherein the current collector has excellent electrical conductivity including but not limited to one of the metal materials of aluminum, copper, titanium, nickel, stainless steel.
9. The electrochemical cell for in-situ raman testing of flow batteries according to claim 1, wherein the current collector comprises a positive current collector and a negative current collector, the bottom of the positive current collector is a fluid positive electrode, the upper of the negative current collector is a negative electrode, and a separator is disposed between the fluid positive electrode and the negative electrode.
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