CN114864946A - Modified reduced graphene oxide binder and preparation method and application thereof - Google Patents
Modified reduced graphene oxide binder and preparation method and application thereof Download PDFInfo
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- CN114864946A CN114864946A CN202210594241.8A CN202210594241A CN114864946A CN 114864946 A CN114864946 A CN 114864946A CN 202210594241 A CN202210594241 A CN 202210594241A CN 114864946 A CN114864946 A CN 114864946A
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J1/00—Adhesives based on inorganic constituents
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—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
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a modified reduced graphene oxide binder and a preparation method and application thereof, wherein graphene oxide is uniformly dispersed in N-methylpyrrolidone (NMP) solution, then ascorbyl palmitate powder is added, or the ascorbyl palmitate powder is pre-dispersed in the NMP solution, the mixture is fully stirred for 2-5h, then the reaction is carried out for 3-5min under the microwave energy of 500W-800W, and the modified reduced graphene oxide binder is obtained after the redundant solution is filtered. According to the invention, the grafting of ester bonds and the excellent properties of graphene enable the graphene to have high mechanical stress and friction coefficient, high defect density and multidimensional conductive network are beneficial to the transmission of lithium ions, the N-L-rGO is used as a binder, the requirement of a production environment can be reduced, the material is uniformly mixed in a high humidity environment, and excellent rate capability and cycle stability are shown in electrochemical performance.
Description
Background
With the rapid development of the lithium ion battery industry, the lithium ion battery is currently the most important portable energy storage device. The most important part of the lithium ion battery belongs to electrode materials, the conventional binder polyvinylidene fluoride (PVDF), a conductive agent and an active material are used for preparing slurry in N-methyl pyrrolidone (NMP) in the production of the positive electrode material and coating the slurry on a current collector, and the conventional binder causes the problems of high production cost, environmental pollution, performance loss of the lithium ion battery and the like due to the following problems
Poor conductivity: PVDF is a non-conductive substance, and lithium ions are difficult to freely move without introducing a conductive agent (acetylene black, Super-P and other conductive carbon black). Only the mass fraction of active substances can be reduced to increase the conductivity, the phase change improves the production cost and reduces the performance of the battery.
The electrode material has high production environment requirement: due to the water-insoluble characteristic of PVDF, the PVDF is easy to solidify when being dispersed in NMP and is not capable of playing the efficacy of the binder, thereby increasing the defective rate in production and reducing the performance of the whole battery. Therefore, the requirement on the environmental humidity is extremely high in the mixing process of the lithium ion battery anode material.
The production of raw materials has high threshold and great environmental pollution: at present, PVDF production mainly comprises two modes, namely emulsion polymerization and suspension polymerization, wherein the two modes both need inert gas atmosphere protection and assistance of a high-temperature and high-pressure environment, a large amount of energy is wasted, and initiators (persulfate, alkyl peroxide and the like) used in the production process have great pollution and high toxicity to the environment.
Disclosure of Invention
Aiming at the problems, the invention provides a modified reduced graphene oxide binder, a preparation method and an application thereof, wherein the binder is low in conductive production environment requirement and green, can provide high interface adhesion, can be uniformly dispersed in an organic solution, and has a lithium ion conductive capability.
The technical scheme of the invention is as follows:
a preparation method of a modified reduced graphene oxide binder comprises the following steps:
uniformly dispersing graphene oxide in N-methyl pyrrolidone (NMP) solution, adding ascorbyl palmitate powder or solution prepared by dispersing ascorbyl palmitate powder in NMP in advance, fully stirring for 2-5h, reacting for 3-5min under 500-800W microwave energy, and filtering the residual solution to obtain the modified reduced graphene oxide binder.
The concentration of the graphene oxide in the NMP solution is 1-2 mg/mL.
The mass ratio of the graphene oxide to the ascorbyl palmitate powder is 1: 5 to 15.
The concentration of the graphene oxide in the NMP solution is 1 mg/mL.
The mass ratio of the graphene oxide to the ascorbyl palmitate powder is 1: 10.
stirred well for 4h and the microwave energy was applied at 600W for 3 min.
The graphene oxide is powder or aqueous solution.
A modified reduced graphene oxide binder prepared by any one of the above methods.
The application of the modified reduced graphene oxide binder is used for an electrode plate of a lithium ion battery, the obtained modified reduced graphene oxide binder and a positive electrode material are uniformly mixed and stirred in NMP, and a conductive agent is added; the mass percentage of the modified reduced graphene oxide binder solid is 5-20%, and the mass percentage of the conductive agent solid is 0-5%; and (3) fully and uniformly mixing, coating on an aluminum foil, and carrying out vacuum drying at 80-120 ℃ for 6-18 h to obtain the corresponding electrode plate.
The anode material is lithium iron phosphate or a ternary material, and the conductive agent is acetylene black, Super-P or a carbon nano tube.
The graphene oxide in the preparation scheme is usually solid powder or a mixed aqueous solution which is not subjected to freeze drying and vacuum drying, and can be directly reacted in proportion under the condition of known concentration, the modified reduced graphene oxide binder obtained in the preparation scheme can be directly used as a binder to be added into electrode slurry after pumping and filtering redundant solution, drying treatment is not needed, and the modified reduced graphene oxide binder can also be used as solid powder to be added into the electrode slurry after drying.
Compared with the prior art, the invention has the beneficial effects that:
1. selecting reduced modified graphene oxide as a binder
The graphene is sp 2 The hybridized monolayer of carbon atoms is tightly arranged as one allotrope of carbon in a two-dimensional structure. Since the discovery of graphene in 2004, its unique physical, chemical and photoelectric properties have attracted the attention of researchers. Due to the good dispersibility and conductivity, the conductive adhesive can be used as a binder to play a greater role.
2. Ascorbyl palmitate is selected as a reduction auxiliary agent
At present, the reduction auxiliary agents used for reducing graphene oxide by using a chemical reduction method are basically strong reducing agents (hydrazine, sodium borohydride, ascorbic acid and the like), the strong reducing agents contain high toxicity and generate a large amount of tail gas in the reduction process, and freeze drying (or vacuum drying) is still needed after reduction to obtain solid reduced graphene oxide powder. The ascorbyl palmitate is used as a nontoxic green reduction auxiliary agent and can also provide ester bonds for graphene oxide bonding effect.
3. Reduction of graphene oxide using microwave method
The chemical reduction method and the high-temperature reduction method which are industrially used at present for preparing the reduced graphene oxide need the steps of solid-liquid separation, drying and waste liquid recovery and high energy consumption heating functions, and have the advantages of oxygen-free environment protection and longer reduction time. The graphene oxide is directly reduced by adding the reduction additive in the microwave method without long-time high-temperature heating and oxygen-free protection, and the reduction modification of the graphene oxide can be completed in a short time.
4. The use of the modified reduced graphene oxide binder does not require a low humidity environment
The PVDF used as the anode binder needs to be constructed in a drying workshop with ultralow humidity in production, and does not have high requirements on production environment after the modified reduced graphene oxide is used, so that the PVDF can be fully and uniformly mixed in any weather and environment.
5. The N-L-rGO of the invention realizes the effect of a binder in the electrode slurry through rich ester bond groups and excellent conductivity and stability, and the high defect density and the multidimensional conductive network bring good lithium ion conductivity, so that the interface friction force and the affinity with the electrolyte, which are superior to PVDF, can enable the positive electrode material of the lithium ion battery to exert good electrochemical performance. Thus, electrodes prepared with N-L-rGO as binder exhibit good rate performance and cycling stability relative to currently used binders.
Drawings
FIGS. 1(a), (c) are X-ray photoelectron spectroscopy tests of Graphene Oxide (GO) and N-L-rGO; (b) x-ray diffraction tests for GO and N-L-rGO; (d) x-ray diffraction tests of GO and N-L-rGO are carried out; thus, the GO is proved to be reduced and grafted with ester bond groups after reaction;
FIG. 2(a) viscosity display of N-L-rGO after filtration of excess liquid; (b) scanning an electron microscope picture on the vertical surface of the coated pole piece; (c) a schematic view of sufficient stirring of the electrode material, the conductive agent and the binder; (d) performing contact angle test on the same anode material (lithium iron phosphate) pole piece; (e) the friction coefficient of PVDF (polyvinylidene fluoride) and N-L-rGO which are commonly used as binders at present is tested;
FIG. 3 is a pictorial representation: respectively testing the mixing condition of common binder PVDF and N-L-rGO under high humidity in a sealed environment; (a-l) are scanning electron microscope images of the pole pieces obtained by mixing materials at different proportions;
FIG. 4 shows that the mass ratio of N-L-rGO to lithium iron phosphate in example 1 is 1: 9, testing a rate performance graph at 0.2, 0.5, 1, 2 and 5C;
FIG. 5 shows that the mass ratio of N-L-rGO to lithium iron phosphate in example 1 is 1: 9, respectively carrying out 200-circle charge-discharge test graphs at 1C and 5C;
FIG. 6 is a graph showing that the mass ratio of N-L-rGO to lithium iron phosphate in example 2 is 2: 8, testing a rate performance graph at 0.2, 0.5, 1, 2 and 5C;
FIG. 7 shows the mass ratio of N-L-rGO to lithium iron phosphate in example 3 is 0.5: testing a rate performance graph at 0.2, 0.5, 1, 2 and 5 ℃ at 9.5;
FIG. 8 shows that the mass ratio of N-L-rGO, Super-P and lithium iron phosphate in example 4 is 0.5: 0.1: testing a rate performance graph at 0.2, 0.5, 1, 2 and 5 ℃ at 9.4;
FIG. 9 shows that the mass ratio of N-L-rGO, Super-P and lithium iron phosphate in example 5 is 0.5: 0.3: testing a rate performance graph at 0.2, 0.5, 1, 2 and 5 ℃ at 9.2;
FIG. 10 shows that the mass ratio of N-L-rGO, Super-P and lithium iron phosphate in example 5 is 0.5: 0.3: at 9.2, respectively carrying out 500-circle charge-discharge test graphs at 1C and 5C;
FIG. 11 shows that the mass ratio of N-L-rGO, Super-P and lithium iron phosphate in example 5 is 0.5: 0.3: 9.2, disassembling the cycled battery into a pole piece real object image and a scanning electron microscope image;
FIG. 12 shows that the mass ratio of N-L-rGO, Super-P and lithium iron phosphate in example 6 is 0.5: 0.5: 9, testing a rate performance graph at 0.2, 0.5, 1, 2 and 5C;
FIG. 13 shows that in comparative example 1, the binder is PVDF, and the mass ratio of Super-P, PVDF to lithium iron phosphate is 1: 1: 8, testing a rate performance graph at 0.2, 0.5, 1, 2 and 5C;
FIG. 14 shows that in comparative example 1, the binder is PVDF, the mass ratio of Super-P, PVDF to lithium iron phosphate is 1: 1: 8, respectively carrying out 500-circle charge-discharge test graphs at 1C and 5C;
fig. 15 is a graph of rate performance measured at 0.2, 0.5, 1, 2, and 5C, respectively, in example 7, with the active material of examples 1, 2, 3, and 5 replaced with a ternary material (NCM) from lithium iron phosphate;
fig. 16 is a graph of rate performance measured at 0.2, 0.5, 1, 2, 5C in example 7 after replacing the active material in comparative example 1 with lithium iron phosphate for a ternary material (NCM).
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
Example 1:
uniformly dispersing 100mg of graphene oxide powder in 100mL of NMP solution, performing ultrasonic treatment for 2 hours, adding 1g of ascorbyl palmitate powder into the solution, stirring for 4 hours till the solution is uniform, putting the solution into a microwave reactor, reacting for 3 minutes at the power of 600W, standing to room temperature, filtering redundant liquid with an organic filter membrane, collecting a product, filtering with water again, and performing freeze drying to obtain a powder sample.
Preparing an electrode: mixing N-L-rGO and lithium iron phosphate in a proportion of 1: and stirring the mixture 9 in an NMP solution for 3 hours, coating the mixture on an aluminum foil, and performing vacuum drying at 120 ℃ for 12 hours to obtain a corresponding pole piece.
Assembling the battery: the electrode was cut into 12mm diameter disks, the lithium sheet was the counter electrode, and CR2032 type coin cells were assembled in an argon atmosphere glove box. The electrolyte is 1M LiPF 6 (EC: DMC: EMC: 1: 1). As shown in FIG. 4, the multiplying power was measured at 0.2, 0.5, 1, 2, 5CEnergy is saved; as shown in fig. 5, 200 cycles of charge and discharge tests were performed at 1C and 5C, respectively;
example 2:
the embodiment is basically the same as the embodiment 1, and the difference is that the mass ratio of the N-L-rGO to the lithium iron phosphate is 2: 8. the rate performance was tested at 0.2, 0.5, 1, 2, 5C, as shown in fig. 6.
Example 3:
the embodiment is basically the same as the embodiment 1, and the difference is that the mass ratio of the N-L-rGO to the lithium iron phosphate is 0.5: 9.5. The rate performance was tested at 0.2, 0.5, 1, 2, 5C, as in fig. 7.
Example 4:
the embodiment is basically the same as the embodiment 1, and is different in that a conductive agent (Super-P) is added during electrode preparation, and the mass ratio of N-L-rGO to Super-P to lithium iron phosphate is 0.5: 0.1: 9.4. the rate performance was tested at 0.2, 0.5, 1, 2, 5C, as shown in fig. 8.
Example 5:
the embodiment is basically the same as the embodiment 4, but the difference is that the mass ratio of N-L-rGO, Super-P and lithium iron phosphate is 0.5: 0.3: 9.2. rate performance was tested at 0.2, 0.5, 1, 2, 5C, as in fig. 9; 500 cycles of charge and discharge tests were performed at 1C and 5C, respectively, as shown in fig. 10; the actual image and the scanning electron microscope image of the pole piece after the battery after the cycle was disassembled are shown in fig. 11.
Example 6:
the embodiment is basically the same as the embodiment 4, but the difference is that the mass ratio of N-L-rGO, Super-P and lithium iron phosphate is 0.5: 0.5: 9. the rate performance was tested at 0.2, 0.5, 1, 2, 5C, as in fig. 12.
Comparative example 1:
this example is substantially the same as example 4 except that: the binder is PVDF, the mass ratio of Super-P, PVDF to lithium iron phosphate is 1: 1: 8. rate performance was tested at 0.2, 0.5, 1, 2, 5C, as in fig. 13; the 500-cycle charge and discharge test was performed at 1C and 5C, respectively, as shown in fig. 14.
Example 7:
this example is substantially the same as examples 1, 2, 3, 5 and comparative example 1, except that the active material was replaced with a ternary material (NCM) from lithium iron phosphate. The rate performance was tested at 0.2, 0.5, 1, 2, 5C, respectively, as shown in fig. 15, 16.
The invention achieves the following technical effects in the above embodiments:
the mixed material is uniformly coated in a high humidity environment, and when the lithium iron phosphate is used as the positive electrode material, the content of the binder is only 10 percent, and the lithium iron phosphate respectively reaches 160,157,155,150 and 110mAh g under the charge-discharge multiplying power of 0.2, 0.5, 1, 2 and 5C without introducing a conductive agent -1 The specific capacity of the resin still has 145 mAh g and 105mAh g after circulating for 200 circles under 1C and 5C -1 The specific capacity and the capacity retention rate reach 93 percent and 100 percent; when the mass of the binder is reduced to 5%, 3% of conductive agent is introduced, and the charge-discharge multiplying power of the binder reaches 162,160,155,150,115mAh g under the charge-discharge multiplying power of 0.2, 0.5, 1, 2 and 5C respectively -1 The specific capacity of the resin still has 150 and 100mAh g after circulating for 500 circles under 1C and 5C -1 The specific capacity and the capacity retention rate are as high as 95 percent. Still performs well in ternary materials.
In conclusion, the N-L-rGO realizes the effect of a binder in the electrode slurry through rich ester bond groups and excellent conductivity and stability, and the high defect density and the multidimensional conductive network bring good lithium ion conductivity, so that the interface friction force and the affinity with the electrolyte, which are superior to those of PVDF, can enable the positive electrode material of the lithium ion battery to exert good electrochemical performance. Thus, electrodes prepared with N-L-rGO as binder exhibit good rate performance and cycling stability relative to currently used binders.
The invention provides an environment-friendly high-conductivity modified reduced graphene oxide binder for a lithium ion battery positive electrode material, a preparation method thereof and an electrode plate, wherein the production environment requirement is reduced. The preparation method comprises the steps of dispersing graphene oxide in N-methyl pyrrolidone, uniformly mixing the graphene oxide with ascorbyl palmitate, reacting for 3-5min under 500-800W microwave energy, filtering redundant solution, and drying solid to obtain modified reduced graphene oxide (N-L-rGO). Due to grafting of ester bonds and excellent properties of graphene, the graphene has high mechanical stress and friction coefficient, high defect density and a multidimensional conductive network are beneficial to transmission of lithium ions, the requirement on production environment can be lowered by taking N-L-rGO as a binder, the material is still uniformly mixed in a high-humidity environment, and excellent rate capability and cycle stability are shown in electrochemical performance.
Claims (10)
1. A preparation method of a modified reduced graphene oxide binder is characterized by comprising the following steps:
uniformly dispersing graphene oxide in N-methyl pyrrolidone (NMP) solution, adding ascorbyl palmitate powder or solution prepared by dispersing ascorbyl palmitate powder in NMP in advance, fully stirring for 2-5h, reacting for 3-5min under 500-800W microwave energy, and filtering the residual solution to obtain the modified reduced graphene oxide binder.
2. The method for preparing the modified reduced graphene oxide binder according to claim 1, wherein the concentration of the graphene oxide in the NMP solution is 1-2 mg/mL.
3. The method for preparing the modified reduced graphene oxide binder according to claim 1, wherein the mass ratio of the graphene oxide to the ascorbyl palmitate powder is 1: 5 to 15.
4. The method of claim 1, wherein the graphene oxide is present in a concentration of 1mg/mL in the NMP solution.
5. The method for preparing the modified reduced graphene oxide binder according to claim 1, wherein the mass ratio of the graphene oxide to the ascorbyl palmitate powder is 1: 10.
6. the method for preparing the modified reduced graphene oxide binder according to claim 1, wherein the mixture is fully stirred for 4 hours, and the microwave energy is applied at 600W for 3 minutes.
7. The method of claim 1, wherein the graphene oxide is in the form of a powder or an aqueous solution.
8. A modified reduced graphene oxide binder prepared by the method of any one of claims 1 to 7.
9. The application of the modified reduced graphene oxide binder is characterized in that the modified reduced graphene oxide binder is used for an electrode plate of a lithium ion battery, the obtained modified reduced graphene oxide binder and a positive electrode material are uniformly mixed and stirred in NMP, and a conductive agent is added; the mass percentage of the modified reduced graphene oxide binder solid is 5-20%, and the mass percentage of the conductive agent solid is 0-5%; and (3) fully and uniformly mixing, coating on an aluminum foil, and carrying out vacuum drying at 80-120 ℃ for 6-18 h to obtain the corresponding electrode plate.
10. The application of the modified reduced graphene oxide binder according to claim 9, wherein the positive electrode material is lithium iron phosphate or a ternary material, and the conductive agent is acetylene black, Super-P or carbon nanotubes.
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