CN105870404B - Conducting polymer for negative electrode of lithium ion battery coats open celled foam antimony electrode and preparation method thereof - Google Patents
Conducting polymer for negative electrode of lithium ion battery coats open celled foam antimony electrode and preparation method thereof Download PDFInfo
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- CN105870404B CN105870404B CN201610279445.7A CN201610279445A CN105870404B CN 105870404 B CN105870404 B CN 105870404B CN 201610279445 A CN201610279445 A CN 201610279445A CN 105870404 B CN105870404 B CN 105870404B
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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
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- 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
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- 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
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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
- 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
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- H—ELECTRICITY
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- 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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- 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
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- 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 present invention relates to a kind of conducting polymers for negative electrode of lithium ion battery to coat open celled foam antimony electrode and preparation method thereof, belongs to the technical field of improvement of lithium ion battery negative material.Conducting polymer of the present invention for negative electrode of lithium ion battery coats open celled foam antimony electrode, and open celled foam antimony is three-dimensional netted pore structure, and antimony is Hollow Nanoparticles structure, open celled foam antimony surface coated with conductive polymer nanocomposite film.Conducting polymer of the present invention for negative electrode of lithium ion battery coats open celled foam antimony electrode, solves the problems, such as that antimony is the volume expansion of lithium ion battery negative material, improves the cycle performance of battery, extend the service life of battery；Simple for process invention also provides a kind of preparation method, the period is short, and operability is strong.
Description
Technical field
The present invention relates to a kind of conducting polymers for negative electrode of lithium ion battery to coat open celled foam antimony electrode and its system
Preparation Method belongs to the technical field of improvement of lithium ion battery negative material.
Background technology
With the rapid development of the industries such as portable electronic device, space flight and aviation and Military Electronic Equipment, electric vehicle,
More stringent requirements are proposed for capacity and service life to lithium ion battery, cannot meet using graphite as the lithium ion battery of cathode
Its capacity requirement.Therefore, before lithium ion battery of the exploitation with high power capacity and long-life is with important research significance and application
Scape, wherein design new electrode materials and electrode structure are the important research contents for realizing this target.
The research hotspot of lithium ion battery negative material includes nano-carbon material, transition metal oxide, IV races semiconductor
Material, such as silicon substrate, germanium base etc. and novel alloy negative material, such as tinbase.In these materials, V races semi-conducting material
Antimony (Sb) is due to high theoretical capacity (660mAhg-1) and (the highly stable work of offer of flat electrochemical reaction platform
Voltage) and receive significant attention.In addition to this, the intercalation potential of antimony is far above the deposition potential of lithium metal, energy in 0.8V or so
Enough appearance for effectively avoiding Li dendrite, improve battery safety.However, antimony material under the conditions of height embedding de- lithium, exists sternly
The bulk effect of weight causes material structural breakdown and electrode material dusting in charge and discharge process to be peeled off, under battery capacity is rapid
Drop, cyclical stability are poor.
Invention content
The purpose of the present invention is to provide a conducting polymer cladding open celled foam antimony electricity for negative electrode of lithium ion battery
Pole, which solve the volume expansion problems that antimony is lithium ion battery negative material, improve the cycle performance of battery, extend electricity
The service life in pond；Simple for process invention also provides a kind of preparation method, the period is short, and operability is strong.
Conducting polymer of the present invention for negative electrode of lithium ion battery coats open celled foam antimony electrode, open celled foam
Antimony is three-dimensional netted pore structure, and antimony is Hollow Nanoparticles structure, open celled foam antimony surface coated with conductive polymer nanocomposite film.
The aperture of the open celled foam antimony is 100-500 μm.
The ingredient of the Hollow Nanoparticles is antimony, antimony copper or antimony nickel alloy, and the grain size of Hollow Nanoparticles is 100-
200nm, wall thickness 30-80nm.It is controllable hollow by carrying out Research statistics to the volume expansion of lithium ion battery negative material
The grain size and wall thickness of nano particle.
The conducting polymer is polyaniline or polypyrrole, and the thickness of conductive polymer nanometer film is 5-30 μm.
The conducting polymer for negative electrode of lithium ion battery coats the preparation method of open celled foam antimony electrode, including
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 nickel nano thin-film is subjected to high-temperature heat treatment, obtain open celled foam nickel；
(2) open celled foam antimony is prepared by electric current displacement method in restricted clearance；
(3) thin in open celled foam antimony surface coated with conductive polymer nanocomposite by in-situ chemical polymerization in restricted clearance
Film.
In step (1), conductive treatment process is that conducting resinl is coated on open-celled polyurethane foam；The item of high-temperature heat treatment
Part is that in a nitrogen atmosphere, temperature is 400-600 DEG C.
The restricted clearance is three-dimensional netted pore structure.
In step (2), the displacement liquid that electric current displacement method uses is ethylene glycol, ethyl alcohol or the diglycol of antimony trichloride
Solution, a concentration of 10-30g/L of antimony trichloride, time swap 5-20h, displacement temperature are 50-100 DEG C.
In step (3), a concentration of 1-3mL/L of aniline or pyrrole monomer used in conducting polymer, ammonium persulfate concentrations are
2-5g/L, benzene sulfonic acid sodium salt a concentration of 100-300mg/L, polymerization time 3-5h.
Although the present invention prepares open celled foam antimony using common electric current displacement method, also opened using in-situ chemical polymerization
Hole foam antimony surface coated with conductive polymer nanocomposite film, but be all to be respectively in open celled foam nickel and open celled foam antimony
It is carried out in limited three-dimensional netted pore structure, wants complicated many in body surface in three-dimensional netted hole internal ratio, process conditions change
Change plays vital influence for above-mentioned two step, by it was verified that only using above-mentioned process conditions ability
Reach requirement.
Compared with prior art, the present invention having the advantages that：
(1) open-celled structure of foam antimony, the flexible and microcosmic nano particle of external conductive polymer nanocomposite film are utilized
Internal cavity structures solve the problems, such as antimony be lithium ion battery negative material volume expansion, improve the cyclicity of battery
Can, extend the service life of battery；
(2) in restricted clearance, the trepanning with hollow nanostructures is prepared for by controlling electric current conditions of replacement reaction
Foam antimony, and hollow nanostructures pattern can be regulated and controled, and then regulate and control capacity of lithium ion battery by controlling conditions of replacement reaction
And the service life；
(3) in restricted clearance, conductive polymer nanometer film has been coated on open celled foam antimony surface, and control can be passed through
Capsulation condition processed adjusts polymer thickness, and then regulates and controls battery performance；
(4) preparation method of conducting polymer cladding open celled foam antimony electrode, preparation process is simple, and the period is short, operable
Property is strong.
Description of the drawings
Fig. 1 is the charging and discharging curve of conducting polymer cladding open celled foam Sb electrodes prepared by embodiment 1；
Fig. 2 is the coulombic efficiency curve of conducting polymer cladding open celled foam Sb electrodes prepared by embodiment 2；
Fig. 3 is the TEM pictures of the Sb nano particles of open celled foam Sb electrode surfaces prepared by embodiment 1.
Specific implementation mode
With reference to embodiment, the present invention is further illustrated, but it is not intended to limit the implementation of the present invention.
Embodiment 1
It is the foamed polyurethane of 10mm × 10mm × 2mm to take size, after over cleaning, oil removing, coating conducting resinl processing, so
Three-electrode system is used afterwards, reference electrode is saturated calomel electrode, is platinum electrode to electrode, and conductive polyurethane is working electrode,
In Ni2SO4Nickel nano thin-film, and 500 DEG C of heat treatment in a nitrogen atmosphere are prepared in electrolyte.Then, it places it in containing 0.6g
In the ethylene glycol solution of the 50mL of antimony trichloride, under nitrogen protection, 100 DEG C of stirring displacement 10h.Finally, electrode is taken out and is cleaned
After drying, it is placed in the 50mL solution containing 10mg benzene sulfonic acid sodium salts and is ultrasonically treated 30min, pyrrole monomer is pipetted with micropipettor
30 μ L are added in above-mentioned solution, are ultrasonically treated 1h, and ammonium persulfate 0.2g is added under condition of ice bath, are ultrasonically treated 2h.Then
It is dry after using deionized water and absolute ethyl alcohol to be cleaned by ultrasonic respectively.Finally obtain product.
To electrode material obtained carries out physical characterization in the process and finally, the aperture of open celled foam antimony is 450 μm；It is hollow
The grain size of nano particle is 130nm, and the thickness of wall thickness 50nm, conductive polymer nanometer film are 18 μm.
By the electrode of preparation for assembling button half-cell and being tested for the property, as shown in Figure 1, the results showed that, cycle
After 100 times, battery reversible capacity is maintained at 550mAhg-1。
Embodiment 2
Experiment condition and operating procedure and embodiment 1 are other same, and the condition of change is as follows：
Nickel nano thin-film is placed in the ethanol solution of the 50mL containing 0.5g antimony trichlorides, under nitrogen protection, 50 DEG C are stirred
Mix displacement 20h.Finally, electrode is taken out after being cleaned and dried, is placed in the 50mL solution containing 5mg benzene sulfonic acid sodium salts and is ultrasonically treated
30min pipettes 30 μ L of pyrrole monomer with micropipettor and is added in above-mentioned solution, is ultrasonically treated 1h, adds under condition of ice bath
Enter ammonium persulfate 0.1g, is ultrasonically treated 3h.
To electrode material obtained carries out physical characterization in the process and finally, the aperture of open celled foam antimony is 320 μm；It is hollow
The grain size of nano particle is 180nm, and the thickness of wall thickness 78nm, conductive polymer nanometer film are 26 μm.
By the electrode of preparation for assembling button half-cell and being tested for the property, as shown in Figure 2, the results showed that, battery
Coulombic efficiency is maintained at 98% or more.
Embodiment 3
Experiment condition and operating procedure and embodiment 1 are other same, and the condition of change is as follows：
Nickel nano thin-film is placed in the diglycol solution of the 50mL containing 1.5g antimony trichlorides, nitrogen protection
Under, 70 DEG C of stirring displacement 5h.Finally, electrode is taken out after being cleaned and dried, is placed in the 50mL solution containing 15mg benzene sulfonic acid sodium salts
It is ultrasonically treated 30min, 30 μ L of aniline monomer is pipetted with micropipettor and is added in above-mentioned solution, 1h is ultrasonically treated, in ice bath
Under the conditions of be added ammonium persulfate 2.5g, be ultrasonically treated 5h.
To electrode material obtained carries out physical characterization in the process and finally, the aperture of open celled foam antimony is 110 μm；It is hollow
The grain size of nano particle is 12nm, and the thickness of wall thickness 32nm, conductive polymer nanometer film are 8 μm.
Open celled foam antimony is subjected to transmission electron microscope characterization, as shown in figure 3, as a result confirming that antimony is Hollow Nanoparticles knot
Structure.
Claims (9)
1. a kind of conducting polymer for negative electrode of lithium ion battery coats open celled foam antimony electrode, it is characterised in that：Trepanning is steeped
Foam antimony is three-dimensional netted pore structure, and antimony is Hollow Nanoparticles structure, and open celled foam antimony surface coated with conductive polymer nanocomposite is thin
Film；
The conducting polymer for negative electrode of lithium ion battery coats the preparation method of open celled foam antimony electrode, including following
Step：
（1）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）Open celled foam antimony is prepared by electric current displacement method in restricted clearance；
（3）By in-situ chemical polymerization in open celled foam antimony surface coated with conductive polymer nanocomposite film in restricted clearance.
2. the conducting polymer according to claim 1 for negative electrode of lithium ion battery coats open celled foam antimony electrode,
It is characterized in that：The aperture of open celled foam antimony is 100-500 μm.
3. the conducting polymer according to claim 1 for negative electrode of lithium ion battery coats open celled foam antimony electrode,
It is characterized in that：The ingredient of Hollow Nanoparticles is antimony, antimony copper or antimony nickel alloy.
4. the conducting polymer according to claim 1 for negative electrode of lithium ion battery coats open celled foam antimony electrode,
It is characterized in that：The grain size of Hollow Nanoparticles is 100-200nm, wall thickness 30-80nm.
5. the conducting polymer according to claim 1 for negative electrode of lithium ion battery coats open celled foam antimony electrode,
It is characterized in that：Conducting polymer is polyaniline or polypyrrole, and the thickness of conductive polymer nanometer film is 5-30 μm.
6. the conducting polymer according to claim 1 for negative electrode of lithium ion battery coats open celled foam antimony electrode,
It is characterized in that：Step（1）In, conductive treatment process is that conducting resinl is coated on open-celled polyurethane foam；High-temperature heat treatment
Condition is that in a nitrogen atmosphere, temperature is 400-600 DEG C.
7. the conducting polymer according to claim 1 for negative electrode of lithium ion battery coats open celled foam antimony electrode,
It is characterized in that：Restricted clearance is three-dimensional netted pore structure.
8. the conducting polymer according to claim 1 for negative electrode of lithium ion battery coats open celled foam antimony electrode,
It is characterized in that：Step（2）In, the displacement liquid that electric current displacement method uses is ethylene glycol, ethyl alcohol or the contracting diethyl two of antimony trichloride
Alcoholic solution, a concentration of 10-30g/L of antimony trichloride, time swap 5-20h, displacement temperature are 50-100 DEG C.
9. the conducting polymer according to claim 1 for negative electrode of lithium ion battery coats open celled foam antimony electrode,
It is characterized in that：Step（3）In, a concentration of 1-3mL/L of aniline or pyrrole monomer used in conducting polymer, ammonium persulfate concentrations are
2-5g/L, benzene sulfonic acid sodium salt a concentration of 100-300mg/L, polymerization time 3-5h.
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| CN201610279445.7A CN105870404B (en) | 2016-04-29 | 2016-04-29 | Conducting polymer for negative electrode of lithium ion battery coats open celled foam antimony electrode and preparation method thereof |
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| CN108539189B (en) * | 2018-04-20 | 2020-08-04 | 太原理工大学 | Antimony nanocrystalline coated carbon micron spherical shell core structure for lithium ion battery cathode and preparation method 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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| CN102332570A (en) * | 2011-08-04 | 2012-01-25 | 佛山市邦普循环科技有限公司 | Method for manufacturing tin-stibium-nickel alloy cathode material of lithium ion battery |
| CN103730630A (en) * | 2013-12-25 | 2014-04-16 | 北京大学深圳研究生院 | Combined electrode of battery and preparation method thereof |
| CN103825011A (en) * | 2014-02-28 | 2014-05-28 | 苏州路特新能源科技有限公司 | Preparation method of tin of lithium ion battery and conductive polymer composite cathode material membrane |
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| US8936874B2 (en) * | 2008-06-04 | 2015-01-20 | Nanotek Instruments, Inc. | Conductive nanocomposite-based electrodes for lithium batteries |
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| CN102332570A (en) * | 2011-08-04 | 2012-01-25 | 佛山市邦普循环科技有限公司 | Method for manufacturing tin-stibium-nickel alloy cathode material of lithium ion battery |
| CN103730630A (en) * | 2013-12-25 | 2014-04-16 | 北京大学深圳研究生院 | Combined electrode of battery and preparation method thereof |
| CN103825011A (en) * | 2014-02-28 | 2014-05-28 | 苏州路特新能源科技有限公司 | Preparation method of tin of lithium ion battery and conductive polymer composite cathode material membrane |
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