CN114204019B - Battery anode material and preparation method and application thereof - Google Patents

Battery anode material and preparation method and application thereof Download PDF

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Publication number
CN114204019B
CN114204019B CN202111397457.7A CN202111397457A CN114204019B CN 114204019 B CN114204019 B CN 114204019B CN 202111397457 A CN202111397457 A CN 202111397457A CN 114204019 B CN114204019 B CN 114204019B
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positive electrode
battery
copper phthalocyanine
electrode material
electrostatic spinning
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CN114204019A (en
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刘熙
张誉元
李彩婷
何芷灵
殷明宇
刘星宇
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Wuyi University
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Wuyi University
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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
    • H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/48—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of halogenated hydrocarbons
    • 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
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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
    • 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

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Electrochemistry (AREA)
  • Textile Engineering (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a battery anode material and a preparation method and application thereof. The method comprises the following steps: and mixing copper phthalocyanine, a conductive matrix and an adhesive to obtain a mixture, and carrying out electrostatic spinning to obtain the battery anode material. The battery anode material prepared by the electrostatic spinning method has high specific capacity and cycle stability after being loaded on a battery anode.

Description

Battery anode material and preparation method and application thereof
Technical Field
The invention belongs to the technical field of positive electrode materials, and particularly relates to a battery positive electrode material, and a preparation method and application thereof.
Background
In recent years, renewable energy sources such as solar energy, wind energy, geothermal energy, tidal energy, etc. have once become a focus of attention, but these energy sources are periodic and intermittent, and the energy generated needs to be stored. Lithium Ion (LIBs) batteries are currently the most promising energy storage technology due to their higher energy density and excellent cycle performance. Lithium batteries are widely used for energy supply of portable devices, electric vehicles and wearable electronic products due to their light weight, long cycle life, high energy density, small memory effect, environmental friendliness and the like. The positive and negative electrode materials, which are the most important components of lithium ion batteries, determine to a large extent the electrochemical performance and cost of the battery.
Currently, commercial lithium ion battery electrodes are generally based on inorganic materials such as the lithium transition metal oxide LiCoO 2、LiMn2O4、LiFePO4. However, these inorganic materials have drawbacks such as limited capacity-increasing space, inability to meet sustainable development requirements, safety risk, high cost, and the like, and their development speed has been slowed down in recent years.
From a sustainable development perspective, organic redox compounds composed of abundant elements (C, H, O, N, etc.) that are renewable in resources should be ideal electrode materials. The organic material can be obtained through a synthesis way with low energy consumption, little waste and potential of potential low cost and environmental friendliness. In addition, the organic electrode can also provide high capacity and meet the requirement of high energy density. More importantly, the voltage of the organic electrode can be flexibly adjusted through molecular design, and can be used as a positive electrode or a negative electrode. In view of the above-mentioned advantages, various organic compounds have been proposed as electrode materials for LIBs.
Unfortunately, despite the numerous advantages described above, the positive electrode materials obtained using conventional abrasive tabletting and slurry coating methods have a relatively low mass fraction (typically only 30%) of active material. In the preparation of lithium battery electrodes, the addition of excessive conductive agent results in a small amount of active material and a low capacity of electrode material, whereas when the mass fraction of active material is attempted to be increased, the conductivity of the electrode is rapidly lowered when the conductive agent is lowered. Therefore, the improvement of the mass fraction of the active material and the utilization rate of the active material are the trend of the future development of the organic positive electrode material of the lithium ion battery.
Disclosure of Invention
The technical problems to be solved by the invention are as follows:
A method of preparing a battery positive electrode material is provided. The battery positive electrode material prepared by the electrostatic spinning method has high active material mass fraction and active material utilization rate after being loaded on a battery positive electrode.
The invention also provides a battery anode material, which is prepared by the method.
The invention also provides a lithium battery, which comprises a battery anode, a lithium sheet cathode and a glass fiber diaphragm, wherein the battery anode comprises the battery anode material.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method of preparing a battery positive electrode material comprising the steps of:
mixing copper phthalocyanine, a conductive matrix and an adhesive to obtain a mixture, and carrying out electrostatic spinning to obtain the battery anode material;
the mass percentage of the copper phthalocyanine in the mixture is less than or equal to 60%.
If the mass percentage of the copper phthalocyanine in the mixture is more than 60%, the obtained product cannot be subjected to electrostatic spinning, and the consumption of a conductive matrix is reduced, so that the conductivity of the product is reduced; if the copper phthalocyanine mass fraction is less than 60%, the mass fraction of the conductive matrix in the system tends to be increased, and since the conductive matrix is insoluble in an organic solvent, too much conductive matrix may make the product difficult to be electrospun.
The greater the mass percentage of copper phthalocyanine (active material) in the mixture, the higher the active material utilization, and the greater the capacity of the battery after being loaded onto the battery, but the greater the mass percentage of active material, the greater the battery capacity and the active material usage are in a balance.
According to one embodiment of the invention, the mixture is magnetically stirred under the following conditions: the room temperature is 25 ℃, the humidity is 35 percent, the rotating speed is 400r/s, and the stirring time is 12 hours.
The mixture can be more uniform by means of magnetic stirring, so that the obtained electrode material has higher stability.
According to one embodiment of the invention, the spinning rate of the electrospinning is 1-3ML/h. Too fast or too slow spinning rates are detrimental to the formation of a stable positive electrode material for the battery.
The copper phthalocyanine is a planar aromatic macrocyclic molecule and has bipolar characteristics of providing electrons and receiving electrons.
The copper phthalocyanine with a large pi conjugated structure is favorable as a positive electrode material, and the rapid oxidation-reduction reaction, high electrochemical performance and low solubility can be realized.
The copper phthalocyanine has a highly stable carbon-nitrogen bond in a molecular skeleton, so that the copper phthalocyanine has high electrochemical stability and low solubility, and the battery anode material can achieve high reversible capacity and large working voltage.
According to one embodiment of the invention, the mass ratio of the copper phthalocyanine, the conductive matrix and the binder is 4-6:3-5:1, preferably the mass ratio is 6:3:1.
According to one embodiment of the present invention, the conductive matrix comprises at least one of conductive carbon black, acetylene black, graphene, and carbon nanotubes.
The conductive matrix is used to increase the conductivity of the positive electrode, and is preferably conductive carbon black.
According to one embodiment of the present invention, the adhesive comprises at least one of polyvinylidene fluoride, carboxymethyl cellulose, polyacrylic acid, polyacrylonitrile, hydroxypropyl methylcellulose, polyvinyl alcohol, and polyimide.
The binder is preferably polyvinylidene fluoride (PVDF).
According to one embodiment of the present invention, the mixture includes a solvent selected from at least one of Dimethylformamide (DMF) and N, N-dimethylacetamide (DMAc).
According to one embodiment of the invention, the total mass concentration of the copper phthalocyanine, the conductive matrix and the binder in the mixture is 5-7%. Preferably 6%.
According to one embodiment of the present invention, the positive electrode material obtained after the electrospinning is collected with aluminum foil.
The electrode material obtained by electrostatic spinning can fully improve the mass fraction of active substances.
According to one embodiment of the present invention, the electrospinning parameters are: the voltage is 25kV, the spinning speed is 1ML/h, the receiving distance is 15cm, the temperature is 25 ℃, the relative humidity is 35%, the rotating speed of a receiving device is 70r/min, and the receiving device is a metal roller.
According to one embodiment of the invention, the method further comprises the step of vacuum drying the fibers.
The temperature of the vacuum drying is 80 ℃, and the vacuum drying time is 8 hours.
In still another aspect of the present invention, there is provided a battery cathode material prepared by the method.
The battery anode material obtained by the electrostatic spinning method has the advantages that the components are uniformly distributed, the mass fraction of active substances is high, and when the mass fraction of copper phthalocyanine is 60%, the specific capacity can reach 249.5mAh/g.
In still another aspect of the present invention, there is provided a lithium battery including a battery positive electrode including the battery positive electrode material, a lithium sheet negative electrode, and a glass fiber separator.
One of the above technical solutions has at least one of the following advantages or beneficial effects:
1. The copper phthalocyanine is a planar aromatic macrocyclic molecule, has bipolar characteristics of providing electrons and accepting electrons, and the reaction in the battery anode material involves transfer of four electrons, thereby promoting rapid oxidation-reduction reaction. In addition, the highly stable carbon-nitrogen bonds in the backbone provide high electrochemical stability and low solubility, thereby enabling the battery positive electrode material to achieve high reversible capacity and large operating voltages.
2. The battery anode material is prepared by adopting an electrostatic spinning method, the mass fraction of active substances can be improved, when the mass fraction of the active substances is 60%, the specific capacity can reach 249.5mAh/g, and compared with the traditional tabletting and slurry coating method, the copper phthalocyanine anode obtained by the electrostatic spinning method has high specific capacity and cycle stability when the mass fraction of the active substances is the same.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
Fig. 1 is an electrochemical performance test chart of the positive electrode of the battery described in the examples.
Fig. 2 is an SEM image of the positive electrode of the battery obtained by the electrospinning method in the example.
Fig. 3 is an SEM image of the positive electrode of the battery obtained by the coating method in the example.
Fig. 4 is an SEM image of the positive electrode of the battery obtained by the tabletting method in the example.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to fall within the scope of the invention.
Example 1
A method of preparing a battery positive electrode material comprising the steps of:
300mg copper phthalocyanine (PTCCu), 150mg conductive carbon black (SP) and 50mg polyvinylidene fluoride (PVDF) were dissolved in 10000mL Dimethylformamide (DMF) solution and magnetically stirred in air for 12 hours;
Carrying out electrostatic spinning on the stirred solution, and setting spinning parameters as follows: the voltage was 25kV, the spinning rate was 1ML/h, and the acceptance distance was 15cm. And baking the obtained positive electrode material in a vacuum oven at 80 ℃ for 8 hours to obtain the battery positive electrode material.
Example 2
A method of preparing a battery positive electrode material comprising the steps of:
200mg copper phthalocyanine (PTCCu), 250mg conductive carbon black (SP) and 50mg polyvinylidene fluoride (PVDF) were dissolved in 10000mL Dimethylformamide (DMF) solution and magnetically stirred in air for 12 hours;
Carrying out electrostatic spinning on the stirred solution, and setting spinning parameters as follows: the voltage was 25kV, the spinning rate was 1ML/h, and the acceptance distance was 15cm. And baking the obtained positive electrode material in a vacuum oven at 80 ℃ for 8 hours to obtain the battery positive electrode material.
Example 3
300Mg copper phthalocyanine (PTCCu), 250mg conductive carbon black (SP) and 50mg polyvinylidene fluoride (PVDF) were dissolved in 10000mL Dimethylformamide (DMF) solution and magnetically stirred in air for 12 hours;
Carrying out electrostatic spinning on the stirred solution, and setting spinning parameters as follows: the voltage was 25kV, the spinning rate was 1ML/h, and the acceptance distance was 15cm. And baking the obtained positive electrode material in a vacuum oven at 80 ℃ for 8 hours to obtain the battery positive electrode material.
Comparative example 1
3Mg of copper phthalocyanine (PTCCu), 1.5mg of conductive carbon black (SP) and 0.5mg of polyvinylidene fluoride (PVDF) are placed in an agate mortar, mixed and ground for 20min, the mixed powder is compressed in a tablet press for 5min after grinding, and the obtained pole piece is baked in a vacuum oven for 8 hours, so that the battery anode material is obtained.
Comparative example 2
The preparation method of the battery anode by adopting the traditional slurry coating method comprises the following steps:
first, 30mg of copper phthalocyanine (PTCCu), 15mg of conductive carbon black (SP) and 5mg of polyvinylidene fluoride (PVDF) were placed in an agate mortar, 2mL of an N-methylpyrrolidone (NMP) solution was added dropwise, and mixed and ground for 40 minutes to obtain a viscous mixed slurry. The mixed slurry was then coated onto an aluminum foil at a thickness of 400 μm and dried and cured in a vacuum oven at 800 deg.c to obtain a battery positive electrode material.
Performance test:
performance tests were performed on the battery cathode materials obtained in examples 1 to 3 and comparative examples 1 to 2.
In an argon glove box, respectively assembling the positive electrode materials obtained by different preparation methods into a lithium battery, taking a lithium sheet as a negative electrode, taking a diaphragm as glass fiber, and taking tetraglycollic dimethyl ether and lithium perchlorate as electrolyte components, wherein the mass concentration of the lithium perchlorate is 1.0M.
And (3) performing a lithium battery charge-discharge curve test in a blue battery test system, wherein the current density of the test is 20mA/g, and the charge-discharge voltage interval is 1.05-3.5V. An electrochemical performance test chart of three battery cathode materials was obtained as shown in fig. 1.
Fig. 1 (a) shows charge and discharge curves of the positive electrode of the battery obtained by the electrospinning method, the tabletting method, and the coating method, respectively, at a current density of 20 mA/g.
When the mass fraction of the same active material is 60%, as can be seen from fig. 1 (a), the specific capacity of the positive electrode material obtained by the electrostatic spinning method can reach 249.5mAh/g, while the specific capacities of the positive electrode materials obtained by the tabletting and slurry coating methods are only 60 mAh/g and 120mAh/g.
It can be seen that the battery positive electrode material obtained by the electrospinning method is a lithium battery electrode with excellent performance.
Characterization of the three methods of positive electrode by SEM testing (as shown in fig. 2-4), fig. 2,3,4 are SEM images of copper phthalocyanine positive electrode obtained by electrospinning, slurry coating, tabletting method at 60% active mass fraction, respectively.
Fig. 2 is an SEM image of the positive electrode of the battery obtained by the electrospinning method.
Wherein, fig. 3 is an SEM image of the battery positive electrode obtained by a coating method;
Fig. 4 is an SEM image of the positive electrode of the battery obtained by the tabletting method.
As can be seen from fig. 2-4: compared with the traditional tabletting and slurry coating methods, the positive electrode material obtained by the electrostatic spinning method has more uniform component distribution.
The effects of examples 2-3 and the microstructure of the resulting product are similar to example 1 and are not shown one by one to avoid redundancy.
In conclusion, a battery positive electrode material with more excellent performance can be prepared by using copper phthalocyanine as a raw material through an electrospinning method.
The foregoing is merely exemplary embodiments of the present invention and are not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention or direct or indirect application in the relevant art are intended to be included in the scope of the present invention.

Claims (7)

1. A method for preparing a battery positive electrode material, characterized by: the method comprises the following steps:
mixing copper phthalocyanine, a conductive matrix, an adhesive and a solvent to obtain a mixture, and carrying out electrostatic spinning to obtain the battery anode material;
the mass percentage of the copper phthalocyanine in the copper phthalocyanine, the conductive matrix and the adhesive is equal to 60%;
The parameters of the electrostatic spinning are as follows: the voltage is 25kV, the spinning speed is 1ML/h, and the receiving distance is 15cm;
The total mass concentration of the copper phthalocyanine, the conductive matrix and the binder in the mixture is 5-7%.
2. The method according to claim 1, characterized in that: the conductive matrix includes at least one of conductive carbon black, acetylene black, graphene, and carbon nanotubes.
3. The method according to claim 1, characterized in that: the solvent is at least one selected from dimethylformamide and N, N-dimethylacetamide.
4. The method according to claim 1, characterized in that: and collecting the anode material obtained after the electrostatic spinning by using aluminum foil.
5. The method according to claim 4, wherein: and the method further comprises the step of vacuum drying the positive electrode material.
6. A battery positive electrode material, characterized in that: the battery positive electrode material is prepared by the method of any one of claims 1 to 5.
7. A lithium battery, characterized in that: comprising a battery positive electrode comprising the battery positive electrode material of claim 6, a lithium sheet negative electrode, and a glass fiber separator.
CN202111397457.7A 2021-11-23 2021-11-23 Battery anode material and preparation method and application thereof Active CN114204019B (en)

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