CN105870404A - Conducting polymer-coated open-cell foamed antimony electrode for anode of lithium ion battery and preparation method of antimony electrode - Google Patents

Conducting polymer-coated open-cell foamed antimony electrode for anode of lithium ion battery and preparation method of antimony electrode Download PDF

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Publication number
CN105870404A
CN105870404A CN201610279445.7A CN201610279445A CN105870404A CN 105870404 A CN105870404 A CN 105870404A CN 201610279445 A CN201610279445 A CN 201610279445A CN 105870404 A CN105870404 A CN 105870404A
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antimony
lithium ion
conducting polymer
ion battery
celled foam
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CN105870404B (en
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郭美卿
宋辉
王志勇
史振东
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Taiyuan University of Technology
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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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/134—Electrodes based on metals, Si or alloys
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
    • 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
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • 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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • 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
    • 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
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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 relates to a conducting polymer-coated open-cell foamed antimony electrode for an anode of a lithium ion battery and a preparation method of the antimony electrode, and belongs to the technical field of improvement of anode materials of lithium ion batteries. According to the conducting polymer-coated open-cell foamed antimony electrode for the anode of the lithium ion battery, open-cell foamed antimony is of a three-dimensional mesh-cell structure, antimony is of a hollow nanoparticle structure, and the surface of open-cell foamed antimony is coated with a conducting polymer nanofilm. According to the conducting polymer-coated open-cell foamed antimony electrode for the anode of the lithium ion battery, the volume expansion problem occurring when antimony serves as the anode material of the lithium ion battery is solved, the cycling performance of the battery is improved, and the service life of the battery is prolonged; meanwhile, the invention provides the preparation method. The technology is simple, the cycle is short, and the operability is high.

Description

Conducting polymer for lithium ion battery negative is coated with open celled foam antimony electrode and preparation method thereof
Technical field
The present invention relates to a kind of conducting polymer for lithium ion battery negative and be coated with open celled foam antimony electrode and preparation method thereof, Belong to the technical field of improvement of lithium ion battery negative material.
Background technology
Along with developing rapidly, to lithium of portable electric appts, space flight and aviation and the industry such as Military Electronic Equipment, electric vehicle Capacity and the life-span of ion battery have higher requirement, and the lithium ion battery with graphite as negative pole can not meet its capacity Demand.Therefore, exploitation has high power capacity and long-life lithium ion battery has important Research Significance and application prospect, wherein Design new electrode materials and electrode structure are the important research contents realizing this target.
The study hotspot of lithium ion battery negative material includes nano-carbon material, transition metal oxide, IV race semi-conducting material, As silica-based, germanio etc., and novel alloy negative material, such as tinbase etc..In the middle of these materials, V race semi-conducting material antimony (Sb) owing to having high theoretical capacity (660mAhg-1) and smooth electrochemical reaction platform (provide highly stable work Make voltage) and receive significant attention.In addition, the intercalation potential of antimony is at about 0.8V, far above the deposition potential of lithium metal, The appearance of Li dendrite can be prevented effectively from, improve battery safety.But, antimony material, under the conditions of the embedding de-lithium of height, exists Serious bulk effect, causes material structural breakdown and electrode material efflorescence in charge and discharge process to be peeled off, under battery capacity is rapid Fall, cyclical stability is poor.
Summary of the invention
It is an object of the invention to provide one for lithium ion battery negative conducting polymer be coated with open celled foam antimony electrode, its solve Antimony of having determined is the volumetric expansion problem of lithium ion battery negative material, improves the cycle performance of battery, extends the life-span of battery； Invention also provides a kind of preparation method, technique is simple, and the cycle is short, workable.
Conducting polymer for lithium ion battery negative of the present invention is coated with open celled foam antimony electrode, and open celled foam antimony is three Dimension networked pore structures, antimony is Hollow Nanoparticles structure, open celled foam antimony Surface coating conductive polymer nanometer thin film.
The aperture of described open celled foam antimony is 100-500 μm.
The composition of described Hollow Nanoparticles is antimony, antimony copper or antimony nickel alloy, and the particle diameter of Hollow Nanoparticles is 100-200nm, Wall thickness is 30-80nm.By the volumetric expansion of lithium ion battery negative material being carried out Research statistics, controllable hollow nanometer The particle diameter of grain and wall thickness.
Described conducting polymer is polyaniline or polypyrrole, and the thickness of conductive polymer nanometer thin film is 5 30 μm.
The described conducting polymer for lithium ion battery negative is coated with the preparation method of open celled foam antimony electrode, including following step Rapid:
(1) by after open-celled polyurethane foam conductive treatment, nickel nano thin-film is prepared by being electrochemically-deposited in its surface, and will Nickel nano thin-film carries out high-temperature heat treatment, obtains open celled foam nickel；
(2) in restricted clearance, open celled foam antimony is prepared by electric current displacement method；
(3) in restricted clearance, in-situ chemical polymerization is passed through at open celled foam antimony Surface coating conductive polymer nanometer thin film.
In step (1), conductive treatment process is coating conducting resinl on open-celled polyurethane foam；The condition of high-temperature heat treatment is In a nitrogen atmosphere, temperature is 400-600 DEG C.
Described restricted clearance is three-dimensional netted pore structure.
In step (2), the displacement liquid that electric current displacement method uses is the ethylene glycol of Butter of antimony., ethanol or diglycol solution, The concentration of Butter of antimony. is 10-30g/L, and time swap is 5-20h, and displacement temperature is 50-100 DEG C.
In step (3), aniline or pyrrole monomer concentration used by conducting polymer are 1-3mL/L, and ammonium persulfate concentrations is 2-5g/L, Benzene sulfonic acid sodium salt concentration is 100-300mg/L, and polymerization time is 3-5h.
Although the present invention uses conventional electric current displacement method to prepare open celled foam antimony, also use in-situ chemical polymerization at open celled foam Antimony Surface coating conductive polymer nanometer thin film, but be respectively in open celled foam nickel and open celled foam antimony, the most all limited Carrying out in three-dimensional netted pore structure, want complicated a lot of in three-dimensional netted hole internal ratio at body surface, process conditions change for above-mentioned Two steps play vital impact, by it was verified that only use above-mentioned process conditions to can be only achieved requirement.
The present invention compared with prior art, has the advantages that
(1) open-celled structure of foam antimony, the flexibility of external conductive polymer nanocomposite thin film and the inside of microcosmic nano-particle are utilized Cavity structure solves the volumetric expansion problem that antimony is lithium ion battery negative material, improves the cycle performance of battery, extends The life-span of battery；
(2) in restricted clearance, by controlling the open celled foam antimony that electric current conditions of replacement reaction is prepared for having hollow nanostructures, And hollow nanostructures pattern can be regulated and controled by controlling conditions of replacement reaction, and then regulate and control capacity of lithium ion battery and life-span；
(3) in restricted clearance, the conductive polymer nanometer thin film at open celled foam antimony Surface coating, it is possible to wrapped by control Patch part, regulates polymer thickness, and then regulation and control battery performance；
(4) preparation method of conducting polymer cladding open celled foam antimony electrode, preparation technology is simple, and the cycle is short, workable.
Accompanying drawing explanation
Fig. 1 is the charging and discharging curve of the conducting polymer cladding open celled foam Sb electrode of embodiment 1 preparation；
Fig. 2 is the coulombic efficiency curve of the conducting polymer cladding open celled foam Sb electrode of embodiment 2 preparation；
Fig. 3 is the TEM picture of the Sb nano-particle of the open celled foam Sb electrode surface of embodiment 1 preparation.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further illustrated, but it is not limiting as the enforcement of the present invention.
Embodiment 1
Take the foamed polyurethane of a size of 10mm × 10mm × 2mm, after over cleaning, oil removing, coating conducting resinl process, so Rear employing three-electrode system, reference electrode is saturated calomel electrode, is platinum electrode to electrode, and conductive polyurethane is working electrode, At Ni2SO4Electrolyte is prepared nickel nano thin-film, and 500 DEG C of heat treatments in a nitrogen atmosphere.Then, it is placed on containing 0.6g In the ethylene glycol solution of the 50mL of Butter of antimony., under nitrogen protection, 100 DEG C of stirring displacement 10h.Finally, electrode is taken out clearly Wash dried, be placed in supersound process 30min in the 50mL solution containing 10mg benzene sulfonic acid sodium salt, pipette pyrroles with micropipettor Monomer 30 μ L joins in above-mentioned solution, supersound process 1h, adds Ammonium persulfate. 0.2g, supersound process 2h under condition of ice bath. The most respectively with after deionized water and dehydrated alcohol ultrasonic cleaning, it is dried.Finally obtain product.
The electrode material during to and finally prepared carries out physical characterization, and the aperture of open celled foam antimony is 450 μm；Hollow nanometer The particle diameter of granule is 130nm, and wall thickness is 50nm, and the thickness of conductive polymer nanometer thin film is 18 μm.
It is used for the electrode of preparation assembling button half-cell and carrying out performance test, as it is shown in figure 1, result shows, circulates 100 After secondary, battery reversible capacity is maintained at 550mAhg-1。
Embodiment 2
Other are identical for experiment condition and operating procedure and embodiment 1, and the condition of change is as follows:
Being placed in by nickel nano thin-film in the ethanol solution of the 50mL containing 0.5g Butter of antimony., under nitrogen protection, 50 DEG C of stirrings are put Change 20h.Finally, after electrode is taken out cleaning-drying, it is placed in supersound process 30min in the 50mL solution containing 5mg benzene sulfonic acid sodium salt, Pipette pyrrole monomer 30 μ L with micropipettor and join in above-mentioned solution, supersound process 1h, under condition of ice bath, add over cure Acid ammonium 0.1g, supersound process 3h.
The electrode material during to and finally prepared carries out physical characterization, and the aperture of open celled foam antimony is 320 μm；Hollow nanometer The particle diameter of granule is 180nm, and wall thickness is 78nm, and the thickness of conductive polymer nanometer thin film is 26 μm.
It is used for the electrode of preparation assembling button half-cell and carrying out performance test, as in figure 2 it is shown, result shows, battery coulomb Efficiency is maintained at more than 98%.
Embodiment 3
Other are identical for experiment condition and operating procedure and embodiment 1, and the condition of change is as follows:
Nickel nano thin-film is placed in the diglycol solution of the 50mL containing 1.5g Butter of antimony., under nitrogen protection, 70 DEG C Stirring displacement 5h.Finally, after electrode is taken out cleaning-drying, it is placed in the 50mL solution containing 15mg benzene sulfonic acid sodium salt ultrasonic Processing 30min, pipette aniline monomer 30 μ L with micropipettor and join in above-mentioned solution, supersound process 1h, at ice bath bar Ammonium persulfate. 2.5g, supersound process 5h is added under part.
The electrode material during to and finally prepared carries out physical characterization, and the aperture of open celled foam antimony is 110 μm；Hollow nanometer The particle diameter of granule is 12nm, and wall thickness is 32nm, and the thickness of conductive polymer nanometer thin film is 8 μm.
Open celled foam antimony is carried out transmission electron microscope sign, as it is shown on figure 3, result confirms that antimony is Hollow Nanoparticles structure.

Claims (10)

1. the conducting polymer cladding open celled foam antimony electrode for lithium ion battery negative, it is characterised in that: open celled foam Antimony is three-dimensional netted pore structure, and antimony is Hollow Nanoparticles structure, open celled foam antimony Surface coating conductive polymer nanometer thin film.
Conducting polymer for lithium ion battery negative the most according to claim 1 is coated with open celled foam antimony electrode, and it is special Levy and be: the aperture of open celled foam antimony is 100-500 μm.
Conducting polymer for lithium ion battery negative the most according to claim 1 is coated with open celled foam antimony electrode, and it is special Levy and be: the composition of Hollow Nanoparticles is antimony, antimony copper or antimony nickel alloy.
Conducting polymer for lithium ion battery negative the most according to claim 1 is coated with open celled foam antimony electrode, and it is special Levying and be: the particle diameter of Hollow Nanoparticles is 100-200nm, wall thickness is 30-80nm.
Conducting polymer for lithium ion battery negative the most according to claim 1 is coated with open celled foam antimony electrode, and it is special Levying and be: conducting polymer is polyaniline or polypyrrole, the thickness of conductive polymer nanometer thin film is 5-30 μm.
6. the arbitrary described conducting polymer for lithium ion battery negative of claim 1-5 is coated with open celled foam antimony electrode Preparation method, it is characterised in that comprise the following steps:
(1) by after open-celled polyurethane foam conductive treatment, nickel nano thin-film is prepared by being electrochemically-deposited in its surface, and will Nickel nano thin-film carries out high-temperature heat treatment, obtains open celled foam nickel；
(2) in restricted clearance, open celled foam antimony is prepared by electric current displacement method；
(3) in restricted clearance, in-situ chemical polymerization is passed through at open celled foam antimony Surface coating conductive polymer nanometer thin film.
Conducting polymer for lithium ion battery negative the most according to claim 6 is coated with the preparation of open celled foam antimony electrode Method, it is characterised in that: in step (1), conductive treatment process is coating conducting resinl on open-celled polyurethane foam；High temperature The condition of heat treatment is in a nitrogen atmosphere, and temperature is 400-600 DEG C.
Conducting polymer for lithium ion battery negative the most according to claim 6 is coated with the preparation of open celled foam antimony electrode Method, it is characterised in that: restricted clearance is three-dimensional netted pore structure.
Conducting polymer for lithium ion battery negative the most according to claim 6 is coated with the preparation of open celled foam antimony electrode Method, it is characterised in that: in step (2), the displacement liquid that electric current displacement method uses is the ethylene glycol of Butter of antimony., ethanol or one Diglycol ethylene solution, the concentration of Butter of antimony. is 10-30g/L, and time swap is 5-20h, and displacement temperature is 50-100 DEG C.
Conducting polymer for lithium ion battery negative the most according to claim 6 is coated with the system of open celled foam antimony electrode Preparation Method, it is characterised in that: in step (3), aniline or pyrrole monomer concentration used by conducting polymer are 1-3mL/L, mistake Ammonium sulfate concentrations is 2-5g/L, and benzene sulfonic acid sodium salt concentration is 100-300mg/L, and polymerization time is 3-5h.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108539189A (en) * 2018-04-20 2018-09-14 太原理工大学 Nanocrystalline cladding carbon micro-spheres core-shell structure of a kind of antimony for negative electrode of lithium ion battery and preparation method thereof
CN110767878A (en) * 2019-09-23 2020-02-07 合肥国轩高科动力能源有限公司 Conductive polymer coated silicon-based negative electrode plate and preparation method and application thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108539189A (en) * 2018-04-20 2018-09-14 太原理工大学 Nanocrystalline cladding carbon micro-spheres core-shell structure of a kind of antimony for negative electrode of lithium ion battery and preparation method thereof
CN110767878A (en) * 2019-09-23 2020-02-07 合肥国轩高科动力能源有限公司 Conductive polymer coated silicon-based negative electrode plate and preparation method and application thereof
CN110767878B (en) * 2019-09-23 2022-06-14 合肥国轩高科动力能源有限公司 Conductive polymer coated silicon-based negative electrode plate and preparation method and application thereof

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