CN111816885A - Lithium ion flow battery positive electrode material and preparation method of slurry thereof - Google Patents
Lithium ion flow battery positive electrode material and preparation method of slurry thereof Download PDFInfo
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- CN111816885A CN111816885A CN202010663735.8A CN202010663735A CN111816885A CN 111816885 A CN111816885 A CN 111816885A CN 202010663735 A CN202010663735 A CN 202010663735A CN 111816885 A CN111816885 A CN 111816885A
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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
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
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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
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
- H01M4/8657—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites layered
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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
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/8663—Selection of inactive substances as ingredients for catalytic active masses, e.g. binders, fillers
- H01M4/8673—Electrically conductive fillers
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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
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
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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
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
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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
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M2004/8678—Inert electrodes with catalytic activity, e.g. for fuel cells characterised by the polarity
- H01M2004/8689—Positive electrodes
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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
Abstract
The invention discloses a lithium ion flow battery positive electrode material and a preparation method of slurry thereof, wherein the positive electrode material is a lithium iron phosphate-Keqin Black (KB) -reduced graphene oxide (rGO) composite material and comprises a conductive network of reduced graphene oxide and lithium iron phosphate and Keqin black which are arranged between the reduced graphene oxide layers, wherein the mass ratio of the lithium iron phosphate to the Keqin black to the reduced graphene oxide is 0.78-0.84:0.13-0.14: 0.01-0.1. When the anode material prepared according to the invention is used for the lithium ion flow battery, the prepared slurry has good suspension property and excellent conductivity, and the cycle stability and the rate capability of the lithium ion flow battery can be obviously improved; the preparation method of the cathode material is simple, convenient and feasible, has good reproducibility, and can be widely used for preparing the reduced graphene oxide-based composite material.
Description
Technical Field
The invention relates to a lithium ion flow battery positive electrode material and a preparation method of slurry thereof, in particular to a lithium iron phosphate-Keqin black-reduced graphene oxide (rGO) composite material and slurry thereof, and belongs to the technical field of flow battery energy storage.
Background
Global energy and climate change issues have accelerated the electrification of motor vehicles by battery technology, and it is now recognized that low cost, scalable energy storage will be the key to the continued development of renewable energy technologies (wind and solar) and increased grid efficiency. Electrochemical energy storage has received much attention due to its high energy density, simplicity and reliability, but existing battery technology has not yet been able to meet many future storage requirements. Therefore, the ministry of the Jiang industry in 2011 proposed the concept of semi-solid flow batteries (SSFC), which skillfully combines the high energy density of rechargeable batteries with the flexible and scalable architecture of fuel cells. Compared with the previously reported flow battery, the energy of the battery system is stored in the solid suspension, the charge transmission is realized through the internal conductive osmotic network, the energy density is ten times higher than that of the water-based flow battery, and the simple and cheap manufacturing process is compared with that of the traditional lithium ion battery.
However, the semi-solid flow battery technology still has a series of problems to be solved, such as suspension property and stability of slurry, sealing property and effectiveness of a reactor, and the like. For the suspension problem of the slurry, a series of intensive studies are carried out by a plurality of scholars, for example, the American Massachusetts institute of technology and technology discloses that a nonionic dispersant PVP is introduced into the slurry, so that the selectivity stability of active material LFP particles can be realized, and the conductive agent KB is not influenced, thereby constructing a two-phase electrode suspension and obtaining good slurry stability and conductivity; in the same year, another nonionic dispersant TX-100 is adopted to regulate the LTO-KB system, so that the viscosity of the system is reduced, the conductivity is increased, and the electrochemical performance is improved.
In the patent aspect, the research on lithium ion flow batteries mostly focuses on the design of a battery reactor and a module, and the preparation of slurry and the design and preparation of solid materials are few, and only Chinese patent (application number: 201510118036.4) proposes that polyvinylidene fluoride-hexafluoropropylene is adopted to improve the stability of a slurry system and avoid the problem of layered settlement when the slurry is used, but the addition of the dispersing agent can destroy the conductive network of the slurry to a certain extent, so that the electrochemical performance of the battery is reduced; in addition, Chinese patent (application number: 201610423193.0) adopts methods such as screening and vacuum baking to pretreat solid particles, is simple and easy to operate, and is suitable for large-scale production, but the solid particles can be agglomerated into larger particles in organic electrolyte to generate sedimentation, so that the problem of slurry sedimentation cannot be fundamentally solved by screening.
Disclosure of Invention
Aiming at the problems in the design aspect of lithium ion flow battery slurry, the invention aims to provide a positive electrode material for a lithium ion flow battery and a preparation method of the slurry, in order to improve the suspension stability of the slurry and not influence the electrochemical performance of the slurry, and particularly relates to a lithium iron phosphate-Keqin black-reduced graphene oxide (rGO) composite material.
The invention also aims to provide a lithium iron phosphate-Keqin black-reduced graphene oxide (rGO) composite material used as a positive electrode material of the lithium ion flow battery so as to improve the stability and the conductivity of the slurry.
In order to solve the problems, the technical scheme is as follows:
the positive electrode material is a lithium iron phosphate-Keqin black-reduced graphene oxide (rGO) composite material, and comprises a conductive network of reduced graphene oxide (rGO), and lithium iron phosphate and Keqin black which are arranged between rGO layers.
The lithium iron phosphate-Keqin black-reduced graphene oxide composite material is characterized in that the mass ratio of the lithium iron phosphate to the Keqin black to the rGO is 0.78-0.84:0.13-0.14:0.01-0.1, wherein the content of the lithium iron phosphate is not less than 50%.
The lithium iron phosphate-Keqin black-reduced graphene oxide composite material is characterized in that: the rGO and the ketjen black form an effective conductive network, the effective conductive network penetrates through the whole composite material system, and the lithium iron phosphate is uniformly dispersed among the conductive networks.
The preparation method of the lithium iron phosphate-Keqin black-reduced graphene oxide composite material is characterized by comprising the following steps of:
weighing 0.6-1.2g of lithium iron phosphate, 0.1-0.2g of Ketjen black and 0.07-0.14g of graphene oxide solution in a beaker;
adding a proper amount of deionized water into the beaker in the step (1);
performing ultrasonic dispersion on the mixture obtained in the step (2);
placing the mixture obtained in the step (3) in a hydrothermal kettle to hydrothermally reduce graphene oxide;
and (4) freeze-drying the solid obtained in the step (4) to obtain the composite material.
The preparation method of the lithium iron phosphate-Ketjen black-reduced graphene oxide composite material is characterized in that the graphene oxide is prepared according to a Hummer method, the concentration of the graphene oxide is 0.5-3mg/g, and the mass of the contained graphene oxide is 1% -10% of the total mass of the lithium iron phosphate and the Ketjen black.
The preparation method of the lithium iron phosphate-Ketjen black-reduced graphene oxide composite material is characterized in that the addition amount of the deionized water is ensured to be 1cm higher than the liquid level so as to ensure a good dispersing effect.
The preparation method of the lithium iron phosphate-Keqin black-reduced graphene oxide composite material is characterized in that the ultrasonic dispersion time is 30-120 min.
The preparation method of the lithium iron phosphate-Ketjen black-reduced graphene oxide composite material is characterized in that the hydrothermal reduction temperature is 100-300 ℃, and the time is 6-12 h.
The preparation method of the lithium iron phosphate-Ketjen black-reduced graphene oxide composite material is characterized in that the freeze drying time is 24-72 hours until a sample is completely dried.
When the lithium iron phosphate-Keqin black-reduced graphene oxide (rGO) composite material is used for a flow battery, the lithium iron phosphate-Keqin black-reduced graphene oxide (rGO) composite material is mixed with electrolyte to prepare slurry.
The electrolyte consists of a solvent and lithium salt, wherein the solvent is two or more of ethylene carbonate, ethyl methyl carbonate, propylene carbonate, diethyl carbonate and the like; the lithium salt being LiPF6One or more of LiTFSI, LiFSI, LiDFOB and the like; the concentration of lithium salt is 0.8-1.5 mol/L.
The mixing method is one or more of magnetic stirring, ball milling, ultrasonic, cell crushing and the like; the mixing time is 30-240 min.
The invention has the advantages of
Compared with the prior art, the technical scheme adopted by the invention has the following technical effects: the positive electrode material for the lithium ion flow battery, prepared by the invention, is applied to flow battery slurry and has excellent suspension stability, conductivity and electrochemical performance. The preparation method of the cathode material provided by the invention is generally suitable for preparing the composite material for the lithium ion flow battery, is simple and easy to obtain, and has good repeatability. The specific capacity of the slurry can reach 160mAh/g, and the slurry has good cycling stability and rate capability.
Drawings
Fig. 1 is a scanned view of a positive electrode composite material prepared in example 1.
Fig. 2 is a comparison graph of cyclic voltammetry of the positive electrode slurry prepared in example 1 and a comparative example.
Fig. 3 is a constant rate (0.5C) cycle comparison graph of the positive electrode slurry prepared in example 1 and the comparative example.
Fig. 4 is a graph showing a ratio (0.1-5.0C) cycle comparison of the positive electrode slurry prepared in example 1 with the comparative example.
Detailed Description
In order to better illustrate the present invention and facilitate the understanding of the technical solutions of the present invention, the present invention is further described in detail below. However, the following examples are only simple examples of the present invention and do not represent or limit the scope of the present invention, which is defined by the claims. The prepared positive electrode composite material and the slurry thereof were tested as follows:
(1) and (3) testing by a scanning electron microscope: the model of a Scanning Electron Microscope (SEM) instrument is SU 8020. And drying the anode composite material to prepare a sample, and carrying out scanning electron microscope test.
(2) Cyclic voltammetry testing: use chenhua test system, the instrument model is: IM6e, test parameters adopted a voltage interval of 2-4.2V, and a scanning rate of 0.1 mV/s.
(3) Constant multiplying power test: the blue Bo battery test system is used, and the instrument model is as follows: CT2001A, test parameters adopted 2-4.2V voltage interval, current density was 0.5C.
(4) And (3) rate testing: the blue Bo battery test system is used, and the instrument model is as follows: CT2001A, test parameters adopted 2-4.2V voltage interval, and current density was 0.1C, 0.5C, 1C, 2C, 5C.
Example 1
Respectively weighing 0.6g of lithium iron phosphate and 0.12 g of Ketjen black, and adding the weighed materials into a beaker containing 0.08g of graphene oxide solution; adding 20mL of deionized water into the beaker; placing the beaker containing the mixture in a cell crusher and performing ultrasonic treatment for 60min to disperse; placing the dispersed mixture in a 100mL hydrothermal kettle for reaction at 180 ℃ for 9 h; freeze-drying the solid obtained by hydrothermal reaction to obtain the anode composite material; and mixing the obtained positive electrode composite material with electrolyte to prepare positive electrode slurry.
Further, the cathode composite material obtained in the example was subjected to microstructure observation using SEM, and the result is shown in fig. 1. Fig. 1 is a scanned image of the cathode composite material prepared in this example 1, and it can be seen from the SEM atlas that the obtained cathode composite material is formed by uniformly dispersing lithium iron phosphate in a conductive network formed by reduced graphene oxide and ketjen black. Fig. 2 is a comparison graph of cyclic voltammetry of the cathode slurry prepared in this example 1 and the comparative example, and it can be seen from fig. 2 that the prepared cathode slurry has a higher peak current, indicating that it has a better electrochemical activity. Fig. 3 is a constant rate (0.5C) cycle comparison graph of the positive electrode slurry prepared in example 1 and the comparative example. The result shows that the prepared composite material has the specific capacity of 159mAh/g after 200 cycles, the capacity retention rate of 98.4 percent and higher capacity retention rate. Fig. 4 is a graph comparing the positive electrode slurry prepared in example 1 with the comparative example in the ratio (0.1-5.0C) cycle, and the ratio test shows that the capacity of the positive electrode composite material is about 152mAh/g at the current density of 0.1C, the capacity is still about 136mAh/g when the current density is increased to 1C, and the capacity returns to about 149mAh/g after the high ratio cycle, which shows that the prepared positive electrode composite material has excellent ratio performance.
Example 2
Respectively weighing 1.0g of lithium iron phosphate and 0.15 g of Ketjen black, and adding the weighed materials into a beaker containing 0.1g of graphene oxide solution; adding 50mL of deionized water into the beaker; placing the beaker containing the mixture under the ultrasonic power of 200W for ultrasonic treatment for 120min for dispersion; placing the dispersed mixture in a 100mL hydrothermal kettle to react for 12h at 150 ℃; freeze-drying the solid obtained by hydrothermal reaction to obtain the anode composite material; and mixing the obtained positive electrode composite material with electrolyte to prepare positive electrode slurry.
Example 3
Respectively weighing 1.2g of lithium iron phosphate and 0.2g of Ketjen black, and adding the weighed materials into a beaker containing 0.14g of graphene oxide solution; adding 70mL of deionized water into the beaker; putting the beaker containing the mixture into a ball milling tank for ball milling for 4 hours; placing the dispersed mixture in a 100mL hydrothermal kettle to react for 10h at 200 ℃; freeze-drying the solid obtained by hydrothermal reaction to obtain the anode composite material; and mixing the obtained positive electrode composite material with electrolyte to prepare positive electrode slurry.
The embodiments of the present invention have been described in detail, but the embodiments are merely examples, and the present invention is not limited to the above-described embodiments. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Therefore, any equivalent substitutions and modifications made without departing from the spirit and scope of the present invention are included in the protection scope of the present invention.
Claims (9)
1. A preparation method of a positive electrode material and slurry thereof for a lithium ion flow battery is characterized by comprising the following steps: (1) respectively weighing a certain amount of lithium iron phosphate and Keqin black, and adding the lithium iron phosphate and the Keqin black into a beaker containing a graphene oxide solution; (2) adding a proper amount of deionized water into the beaker in the step (1); (3) dispersing the mixture of the step (2); (4) placing the mixture obtained in the step (3) in a hydrothermal kettle to hydrothermally reduce graphene oxide; (5) freezing and drying the solid obtained in the step (4) to obtain the anode composite material; (6) mixing the anode composite material obtained in the step (5) with electrolyte to prepare slurry; the anode material is a lithium iron phosphate-Keqin black-reduced graphene oxide (rGO) composite material and comprises a conductive network of the reduced graphene oxide (rGO) and lithium iron phosphate and Keqin black which are arranged between the reduced graphene oxide layers.
2. The method according to claim 1, wherein the graphene oxide is prepared according to a Hummer method, the concentration of the graphene oxide is 0.5-3mg/g, and the mass of the graphene oxide is 1% -10% of the total mass of the lithium iron phosphate and the ketjen black.
3. The method according to claim 1, wherein the amount of deionized water added is ensured to be 1cm above the liquid level to ensure good dispersion.
4. The method according to claim 1, wherein the dispersing method is one or more of magnetic stirring, ball milling, ultrasound, cell crushing and the like; the dispersion time is 30-240 min.
5. The method as claimed in claim 1, wherein the hydrothermal reduction temperature is 100 ℃ and 300 ℃ and the time is 6-12 h.
6. The method of claim 1, wherein the freeze-drying time is 24-72 hours until the sample is completely dried.
7. The method according to claim 1, wherein the mass ratio of the lithium iron phosphate to the ketjen black to the reduced graphene oxide is 0.78-0.84:0.13-0.14: 0.01-0.1.
8. The method of claim 1, wherein the electrolyte is composed of a solvent and a lithium salt, wherein the solvent is two or more selected from ethylene carbonate, ethyl methyl carbonate, propylene carbonate, diethyl carbonate, etc.; the lithium salt being LiPF6One or more of LiTFSI, LiFSI, LiDFOB and the like; the concentration of lithium salt is 0.8-1.5 mol/L.
9. The method of claim 1, wherein: the reduced graphene oxide and the ketjen black form an effective conductive network, the effective conductive network penetrates through the whole composite material system, and the lithium iron phosphate is uniformly dispersed among the conductive networks.
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