CN108063220A - A kind of lithium ion battery coats copper oxide nano material and preparation method with polypyrrole - Google Patents
A kind of lithium ion battery coats copper oxide nano material and preparation method with polypyrrole Download PDFInfo
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- CN108063220A CN108063220A CN201610983659.2A CN201610983659A CN108063220A CN 108063220 A CN108063220 A CN 108063220A CN 201610983659 A CN201610983659 A CN 201610983659A CN 108063220 A CN108063220 A CN 108063220A
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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
- 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The present invention provides a kind of negative electrode of lithium ion battery polypyrrole cladding copper oxide nano materials and preparation method thereof.This method is in the aqueous solution of surfactant, adds in the copper oxide nano material that has been prepared, and after stirring evenly, by adding in pyrroles, the copper oxide nano material that polypyrrole coats is prepared by chemical oxidative polymerization in dopant, oxidant.It centrifuges after reaction, with washings such as deionized water, ethyl alcohol, CuO PPy composite materials can be prepared in vacuum drying or freeze-drying.Compared to pure CuO as negative electrode of lithium ion battery, CuO@PPy composite materials are as the advantages of negative electrode of lithium ion battery：During using copper oxide as lithium ion battery negative material, capacity begins with larger attenuation after cycling 50 times.CuO@PPy composite materials, since polypyrrole shell plays CuO protective effect, the specific capacity of material has good capacity retention ratio over numerous cycles.
Description
Technical field
The present invention relates to field of lithium ion battery, are related to inorganic semiconductor nanometer material preparing technical field.Mainly relate to
And a kind of polypyrrole cladding copper oxide nano material and preparation method thereof, which is mainly used in negative electrode of lithium ion battery, phase
For uncoated copper oxide nano material, the charge and discharge cycles stability as negative electrode of lithium ion battery can be improved.
Background technology
Lithium ion battery is because with high voltage, high-energy, light weight, small, internal resistance is small, self discharge is few, cycle life
The features such as length, memory-less effect, the fields such as mobile electronic device, spare energy storage are widely used in, have been current new energy materials
One of research hotspot of material.The development of lithium ion battery is largely dependent upon the raising of battery material performance, at present cathode
Material is also an important factor for improving the energy content of battery and cycle life.The lithium ion battery negative material of commercialization is mainly stone
Ink, coke and non-graphitized carbon etc..But theoretical capacity is low, it is difficult to meet the needs of electrical source of power.It is 2000, French
Tarascon seminars have delivered article on Nature Journal, it was recently reported that the transition metal oxide MO of nano-scale (M=Co,
Ni, Cu, Fe etc.) etc. can be used as ion secondary battery cathode material lithium, and show higher specific capacity（> 600 mAhg-
1）, this value is about twice of carbon material theoretical capacity.And propose the discharge and recharge reaction mechanism of this kind of material, different from
Toward deintercalation formula reaction mechanism.In charge and discharge process, with lithium metal redox reaction occurs for transition metal oxide, brings height
Specific capacity, and rate charge-discharge better performances are one of important directions of lithium ion battery development, before having development well
Scape.
Although metal oxide lithium ionic cell cathode has the big advantage of specific capacity, but there is Reversible Cycle ratios
The shortcoming that capacity attenuation is larger, cycle performance is unstable.This is because metal oxide majority is poor half of electric conductivity
Conductor material furthermore the Li2O generated during the reaction is further degrading the electric conductivity of material, causes the electric conductivity of cathode
It is poor.Meanwhile larger volume expansion often occurs for the first time after embedding lithium for transition metal oxide particle, generate it is larger should
The dusting of power, easily generating material can gradually lose electrical contact between particle and between particle and collector in cyclic process；This
Outside, after the insertion of a large amount of lithium ions, volume expansion makes adjacent nano particle add the chance of contact, the original of nano grain surface
Sub mutually bonding and the nano particle of neighbour is made gradually to merge, so as to which so-called electrochemistry be triggered to reunite so that many original work
The particle looses electro-chemical activity of property.Secondly, when discharging for the first time, electrolyte and CuO surfaces react and generate SEI layers
(solid electrolyte interface layer), so as to cause larger irreversible charge/discharge capacity.These are transition metal oxide conducts
Negative electrode of lithium ion battery（Including CuO nano materials）In research the problem of urgent need to resolve.Metal oxide is prepared into core
The composite material of shell structure can improve its reversible specific capacity and cycle performance.This is because shell structure can prevent nuclear structure
Stress variation and rupture event generation, core surface formed layer protective layer, prevent between active material and electrolyte
Reaction.
For example, our seminars find under study for action, during using copper oxide as lithium ion battery negative material, cycle 50
After secondary, capacity of negative plates begins with larger attenuation.Therefore we are by copper oxide nano material surface aggregate polypyrrole shell,
Charge and discharge cycles stability when improving copper oxide as negative electrode of lithium ion battery.It is also had been reported that in similar way document, such as：
When the auspicious seminars of Chinese Academy of Sciences CAS Institute of Physics Wang Zhao are using NiO as lithium ion battery negative material, reversible specific capacity is about 400 mAh
g-1, after coating by polypyrrole surface and to form nucleocapsid compound, the reversible specific capacity of material rises to 680 mAh g-1。
When doctor Zheng Qingdong et al. studies discovery using CuO as lithium ion battery negative material, reversible specific capacity is about 200 mAh g-1
(10 charge and discharge cycles), after coating by polypyrrole surface and to form nucleocapsid compound, the reversible specific capacity of material increases
To 600 mAhg-1。
In the research of the application patent, we have used the copper oxide patent sample of our seminar's researchs first ---
Octahedra hollow cuprous oxide passes through the copper oxide nano material that calcining is prepared.Secondly in order to improve copper oxide nano material
Charge and discharge cycles stability during as negative electrode of lithium ion battery, we pass through chemical oxidising polymerisation on copper oxide nano material surface
CuO PPy composite nano materials are prepared in method.In this preparation process, we have carried out Improvement to polymerization.
Such as use FeCl3During as oxide, which can react with copper oxide, therefore we have selected oxidisability larger
Persulfate as oxide, but oxidisability crosses conference and the electric conductivity of polypyrrole is caused to decline, and makes copper oxide instead
Chemical property declines, here, we, which have found, to realize that chemical oxidising polymerisation prepares the side of polypyrrole in CuO surface
Method, and CuO@PPy nano materials are prepared, and raising is realized as negative electrode of lithium ion battery charge and discharge cycles stability
Target.
The content of the invention
The object of the present invention is to provide a kind of negative electrode of lithium ion battery polypyrroles to coat copper oxide nano material；The present invention
Another object be to provide the preparation method of the material.
Technical scheme is divided into the preparation of copper oxide nano material and in copper oxide material outer cladding polypyrrole
Two processes.The preparation process of copper oxide nano material is as follows：
Under conditions of alkaline solution, complexing agent ethylenediamine is added in, is complexed with copper ion, so as to fulfill copper ion in alkaline condition
Under good dissolved state, it is hollow when regulation and control copper ion is reduced into cuprous oxide and by the lamellar structure of ethylenediamine
Or porous structure.Afterwards, copper ion solution is added in the solution, is stirred evenly at 30~100 DEG C, add in reducing agent
Hydrazine, continue stirring 10 minutes to 1 it is small when cuprous nano material is prepared.Prepared cuprous nano material is molten
Liquid is centrifuged, and is washed with a large amount of deionized waters and ethyl alcohol, the cuprous nano material purified, it is then dry and
250~900 DEG C of calcinings obtain the copper oxide nano material of black.
It is as follows in the preparation process of copper oxide material outer cladding polypyrrole：
In the solution containing surfactant（Such as：Benzene sulfonic acid sodium salt）A certain amount of copper oxide material is added in be placed in low temperature, it
Add in pyrrole monomer solution and KCl afterwards, after mixing, controlling reaction temperature is constant, scope be -5 DEG C~50 DEG C between after, by
K is added dropwise in drop2S2O8Solution makes pyrrole polymerize in copper oxide material by chemical oxidization method, continues to stir 10 to 72 small when systems
It is standby to obtain the nano material of polypyrrole cladding copper oxide.Prepared material solution is centrifuged, with a large amount of deionized waters
It is washed with ethyl alcohol, then obtains CuO@PPy composite materials in 60 DEG C of vacuum drying.
In the preparation process of the present invention, surfactant used mainly includes benzene sulfonic acid sodium salt (BSNa), detergent alkylate
Sodium sulfonate (DBSNa), dodecyl sodium sulfate (DSNa), sodiumβ-naphthalenesulfonate (β-NSNa), paratoluenesulfonic acid sodium salt (TSNa) etc..Instead
Answer surfactant in system：Pyrrole monomer：K2S2O8：The amount ratio of the substance of KCl is：1：1~6：1~3：1~10.
Compared to pure CuO as negative electrode of lithium ion battery, the advantages of CuO@PPy composite materials are as negative electrode of lithium ion battery
It is：During using copper oxide as lithium ion battery negative material, capacity begins with larger attenuation after cycling 50 times.CuO@
PPy composite materials, since polypyrrole shell plays CuO protective effect, the specific capacity of material has very over numerous cycles
Good capacity retention ratio.
Description of the drawings
Fig. 1 is the scanning electron microscope image of 1 obtained CuO@PPy composite materials of the embodiment of the present invention.
Fig. 2 is the energy spectrum diagram of 1 obtained CuO@PPy composite materials of the embodiment of the present invention.
Fig. 3 is the energy spectrum diagram of 2 obtained CuO@PPy composite materials of the embodiment of the present invention.
Fig. 4 follows for 2 obtained CuO@PPy composite materials of the embodiment of the present invention as the charge and discharge of negative electrode of lithium ion battery
Ring figure and the charge and discharge cycles figure with pure CuO.
Fig. 5 follows for 3 obtained CuO@PPy composite materials of the embodiment of the present invention as the charge and discharge of negative electrode of lithium ion battery
Ring figure and the charge and discharge cycles figure with pure CuO.
Specific embodiment
With reference to specific embodiment, the present invention will be further explained.But these embodiments are only used for into one
Step illustrate the present invention, and and be not in any way limit the scope of the present invention.
Embodiment 1：
1. following solution is configured first：
Surfactant solution（Such as benzene sulfonic acid sodium salt solution）：It weighs 0.0447 g benzene sulfonic acid sodium salts and is dissolved in the deionized water of 200mL
In, be stirred at room temperature 12 it is small when, surfactant is made fully to dissolve.
K2S2O8Solution:Weigh 0.09747 g K2S2O8And it is dissolved in 20 mL deionized waters.
The preparation of 2.CuO@PPy composite materials：
The CuO powder for weighing the black of 0.2 g is added in prepared surfactant solution, is added after 30 min of magnetic agitation
Enter the KCl of 0.1076 g.Beaker is placed in ice-water bath afterwards, the pyrrole monomer that 50 μ L are pipetted after 20 min of magnetic agitation adds
Enter into mixed liquor.Continue prepared K to stir after 30 min2S2O8Solution is slowly dropped in mixed liquor, magnetic agitation 12
Hour simultaneously ensures that reaction system is constantly in ice-water bath state and obtains CuO PPy composite materials.
3.CuO the purifying of@PPy composite materials：
By the CuO@PPy composite materials prepared at 8000 turns per minute（rpm）Under conditions of centrifuge three times, 5 minutes every time, make
It is alternately washed with deionized water and absolute ethyl alcohol, so eliminates surfactant in unreacted ion and system etc.
Substance, finally by CuO@PPy composite materials in 60 DEG C of vacuum drying or freeze-drying.
As shown in the figure：Fig. 1 is the scanning electron microscope image of the CuO@PPy composite materials prepared in the present embodiment.Fig. 2 is this reality
Apply the energy spectrum diagram of the CuO@PPy composite materials of example preparation.Polypyrrole is can see from the N element peak in the power spectrum and C element peak
The presence of ingredient.This method has the characteristics that simple, flexible, required production equipment is simple it can be seen from method made above.
Surfactant in embodiment 1：Pyrrole monomer：K2S2O8：The amount ratio of the substance of KCl is 1：3：1.5：9.
Embodiment 2：
The CuO powder for weighing the black of 0.2 g is added in prepared surfactant solution, is added after 30 min of magnetic agitation
Enter the KCl of 0.01076 g.Beaker is placed in ice-water bath afterwards, the pyrrole monomer that 5 μ L are pipetted after 20 min of magnetic agitation adds
Enter into mixed liquor.Continue prepared K to stir after 30 min2S2O8Solution is slowly dropped in mixed liquor, magnetic agitation 12
Hour simultaneously ensures that reaction system is constantly in ice-water bath state and obtains CuO PPy composite materials.
As shown in the figure：Fig. 3 is the scanning electron microscope image of the CuO@PPy composite materials prepared in the present embodiment.Fig. 4 is this reality
Apply charge and discharge of the CuO@PPy composite materials prepared in example as the charge and discharge cycles figure of negative electrode of lithium ion battery and with pure CuO
Electricity Xun Huan figure.As can be seen that when negative electrode of lithium ion battery is used as after being prepared into the CuO@PPy composite materials of nucleocapsid, Xun Huan
Stability is significantly improved.
Surfactant in embodiment 2：Pyrrole monomer：K2S2O8：The amount ratio of the substance of KCl is 1：0.3：0.15：0.9.
Embodiment 3：
The CuO powder for weighing the black of 0.2 g is added in prepared surfactant solution, is added after 30 min of magnetic agitation
Enter the KCl of 0.03228 g.Beaker is placed in ice-water bath afterwards, the pyrrole monomer that 15 μ L are pipetted after 20 min of magnetic agitation adds
Enter into mixed liquor.Continue prepared K to stir after 30 min2S2O8Solution is slowly dropped in mixed liquor, magnetic agitation 12
Hour simultaneously ensures that reaction system is constantly in ice-water bath state and obtains CuO PPy composite materials.
As shown in the figure：Fig. 5 is charge and discharge of the CuO@PPy composite materials prepared in the present embodiment as negative electrode of lithium ion battery
Electricity Xun Huan figure and the charge and discharge cycles figure with pure CuO.As can be seen that after being prepared into the CuO@PPy composite materials of nucleocapsid
During as negative electrode of lithium ion battery, cyclical stability is significantly improved.
Surfactant in embodiment 3：Pyrrole monomer：K2S2O8：The amount ratio of the substance of KCl is 1：1：0.5：3.
Embodiment 4：
The CuO powder for weighing the black of 0.2 g is added in prepared surfactant solution, is added after 30 min of magnetic agitation
Enter the KCl of 0.06456 g.Beaker is placed in ice-water bath afterwards, the pyrrole monomer that 30 μ L are pipetted after 20 min of magnetic agitation adds
Enter into mixed liquor.Continue prepared K to stir after 30 min2S2O8Solution is slowly dropped in mixed liquor, magnetic agitation 12
Hour simultaneously ensures that reaction system is constantly in ice-water bath state and obtains CuO PPy composite materials.
Surfactant in embodiment 4：Pyrrole monomer：K2S2O8：The amount ratio of the substance of KCl is 1：2：1：6.
Embodiment 5：
The CuO powder for weighing the black of 0.2 g is added in prepared surfactant solution, is added after 30 min of magnetic agitation
Enter the KCl of 0.1076 g.Beaker is placed in ice-water bath afterwards, the pyrrole monomer that 100 μ L are pipetted after 20 min of magnetic agitation adds
Enter into mixed liquor.Continue prepared K to stir after 30 min2S2O8Solution is slowly dropped in mixed liquor, magnetic agitation 12
Hour simultaneously ensures that reaction system is constantly in ice-water bath state and obtains CuO PPy composite materials.
Surfactant in embodiment 5：Pyrrole monomer：K2S2O8：The amount ratio of the substance of KCl is 1：6：3：9.
Above-described embodiment is described in detail by：In the method in surfactant solution, by adding in pyrroles, doping
Polypyrrole is prepared by chemical oxidative polymerization on the copper oxide nano material surface being prepared in agent, oxidant
The copper oxide nano material of cladding.Polypyrrole cladding copper oxide nano material prepared by the present invention has good electric conductivity,
In the application as negative electrode of lithium ion battery, there is good charge and discharge cycles stability.Prepare the oxidation of polypyrrole cladding
The suitable condition of copper nano material is 1：1~6：1~3：1~10.
Claims (4)
1. a kind of preparation method of polypyrrole cladding copper oxide nano material, it is characterised in that include the following steps：It weighs certain
Amount CuO powder is added in prepared surfactant solution, and magnetic agitation adds in a certain amount of KCl after a certain period of time；It
Beaker is placed in ice-water bath afterwards, pipetting pyrrole monomer after magnetic agitation is uniform is added in mixed liquor；Continue after stirring evenly
K is slowly added dropwise2S2O8Solution, stir and react 10 to 72 it is small when CuO PPy composite materials are prepared.
2. by the preparation method of CuO@PPy composite materials described in claim 1, it is characterised in that：Table in the reaction system
Face activating agent：Pyrrole monomer：K2S2O8：The amount ratio of the substance of KCl is：1：1~6：1~3：1~10.
3. by the preparation method of CuO@PPy composite materials described in claim 1, it is characterised in that：Surfactant master used
To include benzene sulfonic acid sodium salt (BSNa), neopelex (DBSNa), dodecyl sodium sulfate (DSNa), sodiumβ-naphthalenesulfonate
(β-NSNa), paratoluenesulfonic acid sodium salt (TSNa) etc., between range of reaction temperature is -5 DEG C~50 DEG C.
4. the method in claim, the copper oxide nano material for the polypyrrole cladding being prepared.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111317706A (en) * | 2020-04-24 | 2020-06-23 | 云南伦扬科技有限公司 | Wet tissue with moisturizing, moistening and sterilizing functions and preparation method thereof |
| CN112538163A (en) * | 2019-09-23 | 2021-03-23 | Tcl集团股份有限公司 | Composite material, preparation method thereof and quantum dot light-emitting diode |
| CN113975979A (en) * | 2021-08-16 | 2022-01-28 | 深圳中拓天达环境工程有限公司 | Oil-water separation membrane material and preparation method and application thereof |
-
2016
- 2016-11-09 CN CN201610983659.2A patent/CN108063220A/en active Pending
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| ZHIGANG YIN等: "CuO/polypyrrole core–shell nanocomposites as anode materials for lithium-ion batteries", 《ELECTROCHEMISTRY COMMUNICATIONS》 * |
| 于丽华 等: "水溶液中以无机阴离子为掺杂剂动电位法合成聚吡咯", 《大连交通大学学报》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112538163A (en) * | 2019-09-23 | 2021-03-23 | Tcl集团股份有限公司 | Composite material, preparation method thereof and quantum dot light-emitting diode |
| CN112538163B (en) * | 2019-09-23 | 2023-08-29 | Tcl科技集团股份有限公司 | Composite material, preparation method thereof and quantum dot light emitting diode |
| CN111317706A (en) * | 2020-04-24 | 2020-06-23 | 云南伦扬科技有限公司 | Wet tissue with moisturizing, moistening and sterilizing functions and preparation method thereof |
| CN113975979A (en) * | 2021-08-16 | 2022-01-28 | 深圳中拓天达环境工程有限公司 | Oil-water separation membrane material and preparation method and application thereof |
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