CN113611836B - High-power high-energy-density lithium iron phosphate composite electrode material and preparation method thereof - Google Patents
High-power high-energy-density lithium iron phosphate composite electrode material and preparation method thereof Download PDFInfo
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
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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
- H01M4/622—Binders being polymers
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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
- H01M4/624—Electric conductive fillers
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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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a high-power high-energy-density lithium iron phosphate composite electrode material and a preparation method thereof, and belongs to the technical field of functional polymer materials. The composite electrode material comprises the following raw materials in parts by weight: 10-30 parts of free radical ethylene maleic anhydride copolymer, 50-80 parts of lithium iron phosphate and 10-30 parts of carbon nano tube. The invention breaks through the limitations of low power density, high content of inactive ingredients, heavy structure, poor mechanical property, complex process and the like of the traditional lithium iron phosphate composite electrode material, and the prepared composite electrode material has the advantages of good mechanical property, high energy density, high charge and discharge rate, long cycle life and the like when being applied to the anode material of the lithium ion battery.
Description
Technical Field
The invention relates to the technical field of functional polymer materials, in particular to a high-power high-energy-density lithium iron phosphate composite electrode material and a preparation method thereof.
Background
With the development of socioeconomic performance, new and efficient energy storage devices have increasingly stringent development requirements, which place higher demands on energy density, power density, cycle life, portability, and cost. The organic free radical battery is a novel battery using organic free radicals as energy storage active components, and has the advantages of high power density, long cycle life, strong structural modifier of electrode materials, light weight, environmental protection and the like, but has the problems of low energy density and the like. However, the conventional lithium ion battery generally uses a transition metal compound as an electrode material, and has the problems of high energy density, low power density, limited source, non-renewable performance and the like. There have been studies to organically combine the foregoing two battery materials in an effort to develop a high-power high-energy-density electrode. The Vlad et al design and preparation of a composite positive electrode material of a free radical polymer PTMA and lithium iron phosphate realizes rapid charge and discharge at 5 ℃; the composite positive electrode material of PTMA and lithium manganate is studied by Dolphijn and the like, and the composite positive electrode material shows excellent energy-power performance and cycle stability. Such electrode materials are generally prepared by a blade coating method, in which a mixed slurry containing a binder, lithium iron phosphate or lithium manganate, a radical polymer and a conductive carbon material is coated on a substrate such as aluminum foil, and dried. However, the electrode materials prepared by the knife coating method have obvious defects. In addition, the electrode has higher content of inactive ingredients, and a substrate (metal substrates such as aluminum foil are most), a binder (common polyvinylidene fluoride, polyacrylic acid, sodium carboxymethyl cellulose, sodium alginate and the like) has no energy storage function but has higher mass, so that the energy density of the electrode is reduced; the free radical polymer is more in dosage, which is not beneficial to the improvement of energy density; the internal interaction force of the electrode coating is limited, so that the thickness of the coating is limited, and the preparation of the high-load electrode material is not facilitated; and the mechanical property is poor, the electrode coating is not flexible, and the electrode coating is easy to fall off after being bent for many times, so that the application requirement of the novel flexible electronic device cannot be met.
Disclosure of Invention
The invention aims to provide a high-power high-energy-density lithium iron phosphate composite electrode material and a preparation method thereof, so as to solve the problems of low energy density, limited coating thickness, poor mechanical property, no flexibility and the like of an electrode.
In order to achieve the above object, the present invention provides the following solutions:
the invention provides a high-power high-energy-density lithium iron phosphate composite electrode material, which comprises the following raw materials in parts by weight: 10-30 parts of free radical ethylene maleic anhydride copolymer, 50-80 parts of lithium iron phosphate and 10-30 parts of carbon nano tube.
Further, the high-power high-energy-density lithium iron phosphate composite electrode material is of a flexible three-dimensional ternary co-continuous phase structure; the total content of the free radical ethylene maleic anhydride copolymer and the lithium iron phosphate in the composite electrode material is preferably 70-90% wt.
Further, the free radical ethylene maleic anhydride copolymer (PETM) has the structural formula:
the free radical ethylene maleic anhydride copolymer contains 1 nitroxide free radical per repeating unit on average and has a theoretical specific capacity of 90mAh/g; the specific preparation process is shown in the patent with the application number of 201711478167.9; the free radical ethylene maleic anhydride copolymer has both the binding function and the energy storage function.
Further, the carbon nanotubes are single-walled carbon nanotubes and/or multi-walled carbon nanotubes.
The invention provides a preparation method of the high-power high-energy-density lithium iron phosphate composite electrode material, which comprises the following steps:
completely dissolving the free radical ethylene maleic anhydride copolymer in an organic solvent; adding lithium iron phosphate powder and carbon nano tubes, uniformly mixing, pouring into a glass mold, and obtaining the high-power high-energy-density lithium iron phosphate composite electrode material with a specific shape after the organic solvent is completely volatilized.
Further, the organic solvent is one or more of N-methyl pyrrolidone, tetrahydrofuran, hexafluoroisopropanol, N-dimethylformamide and dimethyl sulfoxide.
Further, the mass ratio of the free radical ethylene maleic anhydride copolymer to the organic solvent is 5:1000.
Further, the mixing is uniformly stirred and mixed under the ultrasonic condition.
The invention discloses the following technical effects:
(1) The invention utilizes a large amount of carboxyl groups existing on the molecular chain of the free radical ethylene maleic anhydride copolymer to form a composite material with strong interaction between lithium iron phosphate and carbon nano tubes, the carbon nano tubes are fully dispersed and mutually entangled to form a net structure, lithium iron phosphate particles are effectively wound or coated, the free radical ethylene maleic anhydride copolymer plays a role of a binder, and the lithium iron phosphate and the carbon nano tubes are bonded together, so that a uniform and stable three-dimensional ternary co-continuous phase structure is formed. On one hand, the free radical ethylene maleic anhydride copolymer/lithium iron phosphate/carbon nano tube composite electrode material is endowed with good multidirectional conductive property, and an electron/ion channel penetrating through the free radical ethylene maleic anhydride copolymer/lithium iron phosphate is constructed, so that the energy storage function of the free radical ethylene maleic anhydride copolymer and the lithium iron phosphate can be fully exerted; meanwhile, the nitroxide free radical in the free radical ethylene maleic anhydride copolymer has a synergistic effect on the charge and discharge performance of lithium iron phosphate, can effectively improve the charge and discharge platform of the composite electrode material, promotes the rapid transmission of electrons/ions, and finally realizes the charge and discharge performance of high power and high energy density. On the other hand, the free radical ethylene maleic anhydride copolymer/lithium iron phosphate/carbon nano tube composite electrode material is endowed with good mechanical properties, so that the free radical ethylene maleic anhydride copolymer/lithium iron phosphate/carbon nano tube composite electrode material has good flexibility and deformation resistance.
(2) The free radical ethylene maleic anhydride copolymer/lithium iron phosphate/carbon nano tube composite electrode material prepared by the invention has the bonding function and the energy storage function, does not need to additionally add a binder with no energy storage activity or a substrate such as aluminum foil, greatly improves the content of active ingredients in the composite electrode material, and obviously improves the energy density of the electrode material.
(3) The free radical ethylene maleic anhydride copolymer/lithium iron phosphate/carbon nano tube composite electrode material prepared by the invention is a flexible self-supporting composite material, is not limited by the thickness of a coating of a knife coating method, is beneficial to preparing a high-load composite electrode material, and has important practical value; the composite material has good flexibility and deformation resistance, so that the composite material has important application prospect in flexible portable electronic equipment.
(4) The invention breaks through the limitations of low power density, high content of inactive ingredients, heavy structure, poor mechanical property, complex process and the like of the traditional lithium iron phosphate composite electrode material, and the prepared composite electrode material has high content of active ingredients, easy regulation and control of the structure and the performance of the composite material, good mechanical property, excellent electrochemical performance, convenient operation and mass preparation, and provides a beneficial reference for the development of novel high-power high-energy density flexible electronic devices.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph showing the energy density of constant current charge and discharge at 0.1C for example 1, example 2 and comparative example 1;
FIG. 2 is a photograph showing the appearance of 10% wt of the free radical ethylene maleic anhydride copolymer/80% wt of lithium iron phosphate/10% carbon nanotube composite electrode material prepared in example 1;
FIG. 3 is a physical diagram of an assembled button cell lighting LED of example 1;
FIG. 4 is a graph showing the change in resistance of 10% wt of the free radical ethylene maleic anhydride copolymer/80% wt of lithium iron phosphate/10% of the carbon nanotube composite electrode material prepared in example 1 with the number of bending times;
FIG. 5 is an electron photograph of bending deformation of 10% wt of the free radical ethylene maleic anhydride copolymer/80% wt of lithium iron phosphate/10% carbon nanotube composite electrode material prepared in example 1;
FIG. 6 is a plot of cyclic voltammograms at a sweep rate of 0.1mV/s for example 1, example 2, and comparative example 1;
FIG. 7 is a cycle chart of constant current charge and discharge at 5C for example 1, example 2 and comparative example 1;
FIG. 8 is a cycle chart of constant current charge and discharge at 10C for example 1, example 2 and comparative example 1;
fig. 9 is a graph of the rate performance of example 1, example 2, and comparative example 1.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the invention described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present invention. The specification and examples of the present invention are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
Example 1
Dissolving 10 parts of free radical ethylene maleic anhydride copolymer in N-methyl pyrrolidone, wherein the mass ratio of the free radical ethylene maleic anhydride copolymer to the N-methyl pyrrolidone is 5:1000, adding 10 parts of single-wall carbon nanotubes and 80 parts of lithium iron phosphate under the condition of ultrasonic stirring, fully mixing to obtain a homogeneous free radical ethylene maleic anhydride/lithium iron phosphate/carbon nanotube composite material, pouring the homogeneous free radical ethylene maleic anhydride/lithium iron phosphate/carbon nanotube composite material into a glass mold, and obtaining the 10%wt free radical ethylene maleic anhydride copolymer/80%wt lithium iron phosphate/10%carbon nanotube composite electrode material with a specific shape after the volatilization of an organic solvent is completed. The free radical ethylene maleic anhydride copolymer, lithium iron phosphate and carbon nano tube in the composite electrode material form a three-dimensional ternary co-continuous phase structure.
Example 2
And (3) dissolving 20 parts of free radical ethylene maleic anhydride copolymer in N-methyl pyrrolidone, wherein the mass ratio of the free radical ethylene maleic anhydride copolymer to the N-methyl pyrrolidone is 5:1000, adding 20 parts of single-wall carbon nanotubes and 60 parts of lithium iron phosphate under the condition of ultrasonic stirring, fully mixing to obtain a homogeneous free radical ethylene maleic anhydride/lithium iron phosphate/carbon nanotube composite material, pouring the homogeneous free radical ethylene maleic anhydride/lithium iron phosphate/carbon nanotube composite material into a glass mold, and obtaining the 20%wt free radical ethylene maleic anhydride copolymer/60%wt lithium iron phosphate/20%carbon nanotube composite electrode material with a specific shape after the volatilization of an organic solvent is completed. The free radical ethylene maleic anhydride copolymer, lithium iron phosphate and carbon nano tube in the composite electrode material form a three-dimensional ternary co-continuous phase structure.
Comparative example 1
10 parts of polyvinylidene fluoride is dissolved in N-methyl pyrrolidone, the mass ratio of the polyvinylidene fluoride to the N-methyl pyrrolidone is 20:1000, 10 parts of single-wall carbon nanotubes and 80 parts of lithium iron phosphate are added, and the uniform stirring is carried out fully, so that the homogeneous 10%wt polyvinylidene fluoride/80%wt lithium iron phosphate/10%wt carbon nanotube composite slurry is obtained. The composite electrode slurry is uniformly coated on aluminum foil, and the solvent is dried to obtain 10%wt polyvinylidene fluoride/80%wt lithium iron phosphate/10%wt carbon nano tube composite electrode material.
The deformation resistance of the composite electrode material prepared in the embodiment 1 is characterized (the motion controller NL01C01 of Beijing Zhuo Boyu opto-mechanical and electronic equipment and the electrochemical workstation of Shanghai Chenhua), and the test shows that the resistance of the composite electrode material is little changed after 4500 times of bending tests, and the excellent deformation resistance property is shown. Fig. 1 shows a graph of energy density comparisons of examples 1, 2 and comparative example 1 at 0.1C for constant current charge and discharge, with the energy density of example 1 being about 3 times as high as that of comparative example 1.
Examples 1 to 2 and comparative example 1 were subjected to cyclic voltammetry using an electrochemical workstation (Shanghai Chenhua CHI 660E), as shown in FIG. 6, examples 1 and 2 showed distinct reduction peaks around 3.6V, corresponding to characteristic peaks of nitroxide radicals, whereas comparative example 1 did not. Constant current charge and discharge tests (CT 3001, blue electric electronics inc. In marten) were performed on examples 1, 2 and comparative example 1 at 5C and 10C, respectively. Examples 1 and 2 each showed good cycling stability over 2000 constant current charges and comparative example 1 showed significant decay (fig. 7 and 8). The rate performance of examples 1, 2 and comparative example 1 (fig. 9) were characterized, and the three had relatively close performance at low rates, but the capacity of comparative example 1 was significantly reduced at 20C, indicating that examples 1 and 2 had excellent rate performance. (the specific capacities were calculated based on the radical ethylene maleic anhydride copolymer and lithium iron phosphate as active ingredients, the content of the active ingredient was 90% in example 1, the theoretical specific capacity was 161mAh/g, the active ingredient was 80% in example 2, the theoretical specific capacity was 150mAh/g, and the active ingredient was 80% in comparative example 1, the theoretical specific capacity was 170 mAh/g).
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (4)
1. The high-power high-energy-density lithium iron phosphate composite electrode material is characterized by comprising the following raw materials in parts by weight: 10-30 parts of free radical ethylene maleic anhydride copolymer, 50-80 parts of lithium iron phosphate and 10-30 parts of carbon nano tube;
the structural formula of the free radical ethylene maleic anhydride copolymer is as follows:
；
the preparation method comprises the following steps:
completely dissolving the free radical ethylene maleic anhydride copolymer in an organic solvent; adding lithium iron phosphate and carbon nano tubes, uniformly mixing, pouring into a mold, and obtaining a high-power high-energy-density lithium iron phosphate composite electrode material after the organic solvent is completely volatilized;
the high-power high-energy-density lithium iron phosphate composite electrode material is of a flexible three-dimensional ternary co-continuous phase structure;
the mass ratio of the free radical ethylene maleic anhydride copolymer to the organic solvent is 5:1000.
2. The high power high energy density lithium iron phosphate composite electrode material according to claim 1, wherein the carbon nanotubes are single-walled carbon nanotubes and/or multi-walled carbon nanotubes.
3. The high-power high-energy-density lithium iron phosphate composite electrode material according to claim 1, wherein the organic solvent is one or more of N-methylpyrrolidone, tetrahydrofuran, hexafluoroisopropanol, N-dimethylformamide and dimethyl sulfoxide.
4. The high-power high-energy-density lithium iron phosphate composite electrode material according to claim 1, wherein the materials are uniformly mixed under ultrasonic conditions during mixing.
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