CN106129460A - A kind of multicomponent material combination electrode and lithium ion battery thereof - Google Patents
A kind of multicomponent material combination electrode and lithium ion battery thereof Download PDFInfo
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- CN106129460A CN106129460A CN201610727874.6A CN201610727874A CN106129460A CN 106129460 A CN106129460 A CN 106129460A CN 201610727874 A CN201610727874 A CN 201610727874A CN 106129460 A CN106129460 A CN 106129460A
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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
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The present invention relates to a kind of multicomponent material combination electrode and lithium ion battery thereof, its preparation method comprises the following steps: graphite oxide powder is dissolved in deionized water by (1), forms solution A；(2) by manganese salt, polyvinylpyrrolidone, being dissolved in deionized water, mix homogeneously forms solution B；(3) solution A obtained in step (1) being mixed with the solution B obtained in step (2), mix homogeneously forms solution C；(4) solution C obtained in step (3) is mixed with ammonia, mixed solution D；(5) in the solution D that step (4) obtains, sodium borohydride is added；(6), after sucking filtration, washing, alcohol are washed, it is dried, obtains binary composite；(7) above-mentioned binary composite is dissolved in deionized water；It is added thereto to pyrrole monomer again；(8) being added dropwise to ammonium persulfate aqueous solution in the system that step (7) obtains, filtration, alcohol are washed, are washed, and natural drying obtains this product.The present invention improves discharging efficiency first, reduces the capacitance loss rate after repeatedly circulation.
Description
Technical field
The present invention relates to a kind of multicomponent material combination electrode and lithium ion battery thereof, belong to technical field of lithium batteries.
Background technology
Lithium ion battery is a kind of secondary cell, and it relies primarily on lithium ion and moves work between a positive electrode and a negative electrode.
The development of lithium ion battery comes from the nineties in last century, and the most only 20 years, in the past 20 years was once flying of lithium electricity industry
Jump, along with various countries more have, to environment, the attention of new forms of energy, lithium ion battery, the development advanced by leaps and bounds.Presently used lithium electricity
In the material of pond, owing to the layer structure of graphite negative electrodes material is easily caused the common embedding of electrolyte solvent ion, cause graphite linings
Shape structural damage, thus affect cyclical stability and the coulombic efficiency of the chemical property of graphite cathode material.Meanwhile, graphite
Anisotropic structure feature, limit lithium ion free diffusing in graphite-structure, constrain graphite cathode electrochemistry hold
The performance of amount, simultaneously after being recycled for multiple times, the stability of its capacitance can be deteriorated.Hence in so that current material is difficult to full
The lithium battery of foot fast development is for the requirement of respective material.
Summary of the invention
It is an object of the invention to provide a kind of multicomponent material combination electrode and lithium ion battery thereof, in order to improve battery and put
Capacitance loss after electrical efficiency and reduction repeatedly circulation, improves lithium battery using effect.
To achieve these goals, technical scheme is as follows.
A kind of multicomponent material combination electrode and lithium ion battery thereof, its preparation method comprises the following steps:
(1) graphite oxide powder is dissolved in deionized water with the concentration of 2～6g/L, opens ultrasonic equipment, heating
Stirring 30～60min, forms solution A；
(2) by manganese salt with 0.5～1mol/L concentration, polyvinylpyrrolidone with the concentration of 20～40g/L, be dissolved into
In ionized water, opening ultrasonic equipment, heated and stirred 30～60min, mix homogeneously forms solution B；
(3) solution B obtained in the solution A obtained in step (1) and step (2) is mixed according to the volume ratio of 3～8:1
Closing, open ultrasonic equipment, heated and stirred 30～60min, mix homogeneously forms solution C；
(4) solution C obtained in step (3) is mixed according to the volume ratio of 50～100:1 with ammonia, open ultrasound wave and set
Standby, heated and stirred 60～120min, mixed solution D；
(5), after adding sodium borohydride with the concentration of 0.4～0.5g/L in the solution D that step (4) obtains, ultrasound wave is opened
Equipment, stirs 60～80min, reacts 12～28h, naturally cool to room temperature at 180 DEG C～200 DEG C；
(6), after sucking filtration, washing, alcohol are washed, at 80～100 DEG C, it is dried 4～8h, obtains binary composite；
(7) above-mentioned binary composite is dissolved in deionized water, stirs 1～2h, ultrasonic 30min；It is added thereto to again
Pyrrole monomer, and stir 1h, ultrasonic 10min；
(8) under ice bath, magnetic agitation state, in the system that step (7) obtains, it is added dropwise to ammonium persulfate aqueous solution, drips
Having added rear ice bath reaction 4h, filtration, alcohol are washed, are washed, and natural drying obtains this product.
Further, the manganese salt described in step (2) is four to combine water manganous chloride.
Further, the molecular weight of the polyvinylpyrrolidone described in step (3) is 50000.
Further, the mass concentration of the ammonia described in step (4) is 25%.
Further, in step (7), the concentration that the binary composite added is dissolved in deionized water is 1～3g/L.
Further, in step (7), the pyrrole monomer of addition and the mass ratio of binary composite are 3～8:1.
Further, the quality of the Ammonium persulfate. added in step (8) and the quality of the pyrrole monomer of addition in step (7)
Ratio is 1:3～9.
This beneficial effect of the invention is: the lithium battery composite discharge capacity first that the present invention provides is
More than 720mAh/g, discharging efficiency has reached more than 68% first, and the discharge capacity loss rate after 1500 circulations reaches
Less than 4.3%, electric current 30C discharge capacity has reached more than 640mAh/g, electric current 30C discharge capacity rate reached 96.5% with
On.The present invention greatly improves discharging efficiency first, reduces the capacitance loss rate after repeatedly circulation, improves electric discharge and holds
Amount, has the biggest using value.
Detailed description of the invention
Multicomponent material combination electrode in the present invention and lithium ion battery thereof, its preparation method comprises the following steps:
(1) graphite oxide powder is dissolved in deionized water with the concentration of 2～6g/L, opens ultrasonic equipment, heating
Stirring 30～60min, forms solution A；
(2) by manganese salt with 0.5～1mol/L concentration, polyvinylpyrrolidone with the concentration of 20～40g/L, be dissolved into
In ionized water, opening ultrasonic equipment, heated and stirred 30～60min, mix homogeneously forms solution B；
(3) solution B obtained in the solution A obtained in step (1) and step (2) is mixed according to the volume ratio of 3～8:1
Closing, open ultrasonic equipment, heated and stirred 30～60min, mix homogeneously forms solution C；
(4) solution C obtained in step (3) is mixed according to the volume ratio of 50～100:1 with ammonia, open ultrasound wave and set
Standby, heated and stirred 60～120min, mixed solution D；
(5), after adding sodium borohydride with the concentration of 0.4～0.5g/L in the solution D that step (4) obtains, ultrasound wave is opened
Equipment, stirs 60～80min, reacts 12～28h, naturally cool to room temperature at 180 DEG C～200 DEG C；
(6), after sucking filtration, washing, alcohol are washed, at 80～100 DEG C, it is dried 4～8h, obtains binary composite；
(7) above-mentioned binary composite is dissolved in deionized water, stirs 1～2h, ultrasonic 30min；It is added thereto to again
Pyrrole monomer, and stir 1h, ultrasonic 10min；
(8) under ice bath, magnetic agitation state, in the system that step (7) obtains, it is added dropwise to ammonium persulfate aqueous solution, drips
Having added rear ice bath reaction 4h, filtration, alcohol are washed, are washed, and natural drying obtains this product.
Manganese salt described in step (2) is four to combine water manganous chloride.Polyvinylpyrrolidone described in step (3)
Molecular weight is 50000.The mass concentration of the ammonia described in step (4) is 25%.In step (7), the binary added is combined
The concentration that material is dissolved in deionized water is 1～3g/L.In step (7), the pyrrole monomer of addition and the matter of binary composite
Amount ratio is 3～8:1.The quality of the Ammonium persulfate. added in step (8) with the mass ratio of the pyrrole monomer of addition in step (7) is
1:3～9.
Below in conjunction with embodiment, the detailed description of the invention of the present invention is described, in order to be better understood from the present invention.
Embodiment 1
Multicomponent material combination electrode in the present embodiment and lithium ion battery thereof, its preparation method comprises the following steps:
(1) graphite oxide powder is dissolved in deionized water with the concentration of 2g/L, opens ultrasonic equipment, heated and stirred
30min, forms solution A；
(2) by manganese salt with 0.5～1mol/L concentration, polyvinylpyrrolidone with the concentration of 20g/L, be dissolved into deionization
In water, opening ultrasonic equipment, heated and stirred 30min, mix homogeneously forms solution B；
(3) solution B obtained in the solution A obtained in step (1) and step (2) is mixed according to the volume ratio of 3～8:1
Closing, open ultrasonic equipment, heated and stirred 30min, mix homogeneously forms solution C；
(4) solution C obtained in step (3) is mixed according to the volume ratio of 50～100:1 with ammonia, open ultrasound wave and set
Standby, heated and stirred 60～120min, mixed solution D；
(5), after adding sodium borohydride with the concentration of 0.4～0.5g/L in the solution D that step (4) obtains, ultrasound wave is opened
Equipment, stirs 80min, reacts 12h, naturally cool to room temperature at 200 DEG C；
(6), after sucking filtration, washing, alcohol are washed, at 80～100 DEG C, it is dried 6h, obtains binary composite；
(7) above-mentioned binary composite is dissolved in deionized water, stirs 1～2h, ultrasonic 30min；It is added thereto to again
Pyrrole monomer, and stir 1h, ultrasonic 10min；
(8) under ice bath, magnetic agitation state, in the system that step (7) obtains, it is added dropwise to ammonium persulfate aqueous solution, drips
Having added rear ice bath reaction 4h, filtration, alcohol are washed, are washed, and natural drying obtains this product.
Manganese salt described in step (2) is four to combine water manganous chloride.Polyvinylpyrrolidone described in step (3)
Molecular weight is 50000.The mass concentration of the ammonia described in step (4) is 25%.In step (7), the binary added is combined
The concentration that material is dissolved in deionized water is 1g/L.In step (7), the pyrrole monomer of addition and the mass ratio of binary composite
For 3:1.The quality of the Ammonium persulfate. added in step (8) is 1:3 with the mass ratio of the pyrrole monomer of addition in step (7).
Embodiment 2
Multicomponent material combination electrode in the present embodiment and lithium ion battery thereof, its preparation method comprises the following steps:
(1) graphite oxide powder is dissolved in deionized water with the concentration of 2～6g/L, opens ultrasonic equipment, heating
Stirring 30～60min, forms solution A；
(2) by manganese salt with 0.5～1mol/L concentration, polyvinylpyrrolidone with the concentration of 30g/L, be dissolved into deionization
In water, opening ultrasonic equipment, heated and stirred 45min, mix homogeneously forms solution B；
(3) solution B obtained in the solution A obtained in step (1) and step (2) is mixed according to the volume ratio of 3～8:1
Closing, open ultrasonic equipment, heated and stirred 30～60min, mix homogeneously forms solution C；
(4) solution C obtained in step (3) is mixed according to the volume ratio of 100:1 with ammonia, opens ultrasonic equipment,
Heated and stirred 120min, mixed solution D；
(5), after adding sodium borohydride with the concentration of 0.4～0.5g/L in the solution D that step (4) obtains, ultrasound wave is opened
Equipment, stirs 60～80min, reacts 12～28h, naturally cool to room temperature at 180 DEG C～200 DEG C；
(6), after sucking filtration, washing, alcohol are washed, at 80～100 DEG C, it is dried 4～8h, obtains binary composite；
(7) above-mentioned binary composite is dissolved in deionized water, stirs 1～2h, ultrasonic 30min；It is added thereto to again
Pyrrole monomer, and stir 1h, ultrasonic 10min；
(8) under ice bath, magnetic agitation state, in the system that step (7) obtains, it is added dropwise to ammonium persulfate aqueous solution, drips
Having added rear ice bath reaction 4h, filtration, alcohol are washed, are washed, and natural drying obtains this product.
Manganese salt described in step (2) is four to combine water manganous chloride.Polyvinylpyrrolidone described in step (3)
Molecular weight is 50000.The mass concentration of the ammonia described in step (4) is 25%.In step (7), the binary added is combined
The concentration that material is dissolved in deionized water is 2g/L.In step (7), the pyrrole monomer of addition and the mass ratio of binary composite
For 5:1.The quality of the Ammonium persulfate. added in step (8) is 1:6 with the mass ratio of the pyrrole monomer of addition in step (7).
Embodiment 3
Multicomponent material combination electrode in the present embodiment and lithium ion battery thereof, its preparation method comprises the following steps:
(1) graphite oxide powder is dissolved in deionized water with the concentration of 6g/L, opens ultrasonic equipment, heated and stirred
60min, forms solution A；
(2) by manganese salt with the concentration of 1mol/L, polyvinylpyrrolidone with the concentration of 40g/L, be dissolved in deionized water,
Opening ultrasonic equipment, heated and stirred 30～60min, mix homogeneously forms solution B；
(3) solution B obtained in the solution A obtained in step (1) and step (2) is mixed according to the volume ratio of 3～8:1
Closing, open ultrasonic equipment, heated and stirred 60min, mix homogeneously forms solution C；
(4) solution C obtained in step (3) is mixed according to the volume ratio of 50～100:1 with ammonia, open ultrasound wave and set
Standby, heated and stirred 120min, mixed solution D；
(5), after adding sodium borohydride with the concentration of 0.4～0.5g/L in the solution D that step (4) obtains, ultrasound wave is opened
Equipment, stirs 80min, reacts 28h, naturally cool to room temperature at 180 DEG C～200 DEG C；
(6), after sucking filtration, washing, alcohol are washed, at 100 DEG C, it is dried 8h, obtains binary composite；
(7) above-mentioned binary composite is dissolved in deionized water, stirs 1～2h, ultrasonic 30min；It is added thereto to again
Pyrrole monomer, and stir 1h, ultrasonic 10min；
(8) under ice bath, magnetic agitation state, in the system that step (7) obtains, it is added dropwise to ammonium persulfate aqueous solution, drips
Having added rear ice bath reaction 4h, filtration, alcohol are washed, are washed, and natural drying obtains this product.
Manganese salt described in step (2) is four to combine water manganous chloride.Polyvinylpyrrolidone described in step (3)
Molecular weight is 50000.The mass concentration of the ammonia described in step (4) is 25%.In step (7), the binary added is combined
The concentration that material is dissolved in deionized water is 3g/L.In step (7), the pyrrole monomer of addition and the mass ratio of binary composite
For 8:1.The quality of the Ammonium persulfate. added in step (8) is 1:9 with the mass ratio of the pyrrole monomer of addition in step (7).
The above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications are also considered as
Protection scope of the present invention.
Claims (7)
1. a multicomponent material combination electrode and lithium ion battery thereof, it is characterised in that: its preparation method comprises the following steps:
(1) graphite oxide powder is dissolved in deionized water with the concentration of 2～6g/L, opens ultrasonic equipment, heated and stirred
30～60min, form solution A；
(2) by manganese salt with 0.5～1mol/L concentration, polyvinylpyrrolidone with the concentration of 20～40g/L, be dissolved into deionization
In water, opening ultrasonic equipment, heated and stirred 30～60min, mix homogeneously forms solution B；
(3) solution A obtained in step (1) is mixed according to the volume ratio of 3～8:1 with the solution B obtained in step (2), open
Opening ultrasonic equipment, heated and stirred 30～60min, mix homogeneously forms solution C；
(4) solution C obtained in step (3) is mixed according to the volume ratio of 50～100:1 with ammonia, opens ultrasonic equipment,
Heated and stirred 60～120min, mixed solution D；
(5), after adding sodium borohydride with the concentration of 0.4～0.5g/L in the solution D that step (4) obtains, open ultrasound wave and set
Standby, stir 60～80min, at 180 DEG C～200 DEG C, react 12～28h, naturally cool to room temperature；
(6), after sucking filtration, washing, alcohol are washed, at 80～100 DEG C, it is dried 4～8h, obtains binary composite；
(7) above-mentioned binary composite is dissolved in deionized water, stirs 1～2h, ultrasonic 30min；It is added thereto to pyrroles again
Monomer, and stir 1h, ultrasonic 10min；
(8) under ice bath, magnetic agitation state, in the system that step (7) obtains, it is added dropwise to ammonium persulfate aqueous solution, drips
After one-tenth, ice bath reacts 4h, and filtration, alcohol are washed, washed, and natural drying obtains this product.
Multicomponent material combination electrode the most according to claim 1 and lithium ion battery thereof, it is characterised in that: in step (2)
Described manganese salt is four to combine water manganous chloride.
Multicomponent material combination electrode the most according to claim 1 and lithium ion battery thereof, it is characterised in that: in step (3)
The molecular weight of described polyvinylpyrrolidone is 50000.
Multicomponent material combination electrode the most according to claim 1 and lithium ion battery thereof, it is characterised in that: in step (4)
The mass concentration of described ammonia is 25%.
Multicomponent material combination electrode the most according to claim 1 and lithium ion battery thereof, it is characterised in that: in step (7),
The concentration that the binary composite added is dissolved in deionized water is 1～3g/L.
Multicomponent material combination electrode the most according to claim 1 and lithium ion battery thereof, it is characterised in that: in step (7),
The pyrrole monomer added is 3～8:1 with the mass ratio of binary composite.
Multicomponent material combination electrode the most according to claim 1 and lithium ion battery thereof, it is characterised in that: in step (8)
The quality of the Ammonium persulfate. added is 1:3～9 with the mass ratio of the pyrrole monomer of addition in step (7).
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105244483A (en) * | 2015-09-16 | 2016-01-13 | 常州大学 | Preparation method modified manganese-based composite material used for lithium ion battery |
| CN105789569A (en) * | 2014-12-19 | 2016-07-20 | 中国科学院大连化学物理研究所 | Multilevel structure composite material as well as preparation and application thereof |
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- 2016-08-24 CN CN201610727874.6A patent/CN106129460A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105789569A (en) * | 2014-12-19 | 2016-07-20 | 中国科学院大连化学物理研究所 | Multilevel structure composite material as well as preparation and application thereof |
| CN105244483A (en) * | 2015-09-16 | 2016-01-13 | 常州大学 | Preparation method modified manganese-based composite material used for lithium ion battery |
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