CN105742597B - A kind of preparation method of lithium ion battery negative material - Google Patents
A kind of preparation method of lithium ion battery negative material Download PDFInfo
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- CN105742597B CN105742597B CN201610141165.XA CN201610141165A CN105742597B CN 105742597 B CN105742597 B CN 105742597B CN 201610141165 A CN201610141165 A CN 201610141165A CN 105742597 B CN105742597 B CN 105742597B
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- lithium ion
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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
- H01M4/364—Composites as mixtures
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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
- H01M4/36—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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- 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
- H01M4/625—Carbon or graphite
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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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- 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 present invention relates to a kind of preparation methods of lithium ion battery negative material, belong to lithium ion battery material technical field.The object of the present invention is to provide a kind of lithium ion cell nano SnO2The preparation method of/C composite negative pole materials.A kind of preparation method of lithium ion battery negative material of the present invention, tin source is dissolved in acetone water mixed system, urea and polyvinylpyrrolidone is added after being completely dissolved to tin source in stirring, stirs 2~5 hours, adds expanded graphite, then solution is transferred in hydrothermal reaction kettle, it is placed in 90~130 DEG C and carries out hydrothermal synthesis 2~10 hours, after reaction kettle cooled to room temperature, products therefrom is filtered, wash, is dried, and 3h is roasted in 600 DEG C of inert gas atmospheres, obtain nano SnO2/ C composite lithium ion battery cathode materials.
Description
Technical field
The present invention relates to a kind of preparation methods of lithium ion battery negative material, belong to lithium ion battery material technology neck
Domain.
Background technology
Lithium ion battery is compared to traditional secondary battery (plumbic acid, ni-mh, nickel chromium triangle) with its high voltage, high-energy density (body
Product is than energy and specific energy), low self-discharge rate, wide use temperature range, long circulation life, environmental protection, memory-less effect with
And it can be obtained in fields such as mobile communication equipment, portable electronic device, electric vehicles rapidly with characteristics such as high current charge-discharges
It is widely applied, has become modern and following important one of the green energy resource.Wherein, negative material is to determine lithium-ion electric
One of the key factor of pond comprehensive performance quality.Currently, commercialization graphite cathode material there are theoretical capacity it is low (about
372mAh/g), high rate performance is poor etc., has been unable to meet the demand of high-energy density, high power density lithium ion battery.Cause
This, explores other alternative high power capacity, high circulation stability, energy fast charging and discharging negative material, it has also become study in the world
One of hot spot.
SnO2Because with high theoretical capacity (782mAh/g), low cost and the advantages such as have no toxic side effect, and receiving and grinding
The concern for the person of studying carefully.But SnO2Existing main problem is charge and discharge cycles in the process along with huge volume change, material appearance
Easy dusting, failure, therefore cycle performance is poor.In addition, SnO2Electric conductivity it is bad, also cause its high rate performance poor.By SnO2
Material nano and with carbon material carry out it is compound can be obviously improved this volume change problem, and improve material conductivity.It is main
It wants the reason is that, the stress that generates is smaller when the particle volume variation of nanosizing, particle does not allow broken, dusting, and and carbon materials
Material compound can effectively prevent nano SnO2The reunion of particle is grown up, and conductive network is provided, and when being buffered in charge and discharge
Volume change, so that the stability of material and high rate performance can greatly improve.
Can be used in compound carbon material mainly includes amorphous carbon, carbon nanotube, graphene etc..Wherein, graphene
The electric conductivity of base nanometer sheet Yin Qigao, mechanical strength and preferably elasticity is widely used for design high-performance negative material.However,
The preparation process of graphene is complicated at this stage, cost is higher, the requirement for distance commercialization low cost, simple process also have compared with
Big gap.Compared to redox graphene, expanded graphite is with preparation method is simple, of low cost, lamella is big, defect is few, leads
The advantages that electrically good and hole is abundant.Although expanded graphite has application in other fields such as absorption, in lithium ion battery
Negative material field seldom has been reported that.
Hydrothermal synthesis method is the common synthetic method of field of nanometer material technology, existing nano SnO2Negative material also more to be adopted
It is prepared with this means.But with regard to current SnO2From the point of view of the present Research of/C composite, SnO is prepared2Nano particle is evenly dispersed
And effectively compound negative material is still a bigger challenge with carbon.Main reason is that carbon material is mostly hydrophobic material,
It is difficult to be flooded profit when reacting in water solution system.So SnO obtained by the reaction2Nano particle with carbon compound tense, nanometer
Particle, which is easy to reunite, grows up, and the SnO of bulky grain2It is easy to rupture dusting, so that under material capacity is rapid in cycle
Drop.Therefore, novel processing step is developed into SnO2The important directions of/C composite research.
Invention content
The object of the present invention is to provide a kind of lithium ion cell nano SnO2The preparation method of/C composite negative pole materials.
In order to achieve the above object, present invention employs following technical schemes：
A kind of preparation method of lithium ion battery negative material, tin source is dissolved in acetone water mixed system, stirring to tin
Urea and polyvinylpyrrolidone is added after being completely dissolved in source, stirs 2~5 hours, adds expanded graphite, then turns solution
Enter in hydrothermal reaction kettle, is placed in 90~130 DEG C and carries out hydrothermal synthesis 2~10 hours, it, will after reaction kettle cooled to room temperature
Products therefrom is filtered, is washed, is dried, and roasts 3h in 600 DEG C of inert gas atmospheres, obtains nano SnO2/ C complex lithiums from
Sub- cell negative electrode material.
Tin source of the present invention is stannic chloride pentahydrate or two water stannous chloride.
A concentration of 1.5~250mmol/L of tin source in solution of the present invention.
The volume ratio of acetone and water is 0.1~10 in acetone water mixed system of the present invention.
Urea concentration is 1.2~70g/L in solution of the present invention.
Polyvinylpyrrolidoneconcentration concentration is 1.0~80g/L in solution of the present invention.
A concentration of 0.3~30g/L of expanded graphite in solution of the present invention.
Compared with prior art, the present invention has the advantage that：
1. the present invention replaces the water solution system of conventional hydrothermal method with acetone water mixed system, it is advantageous that, in water
Acetone is added and is equivalent to and is diluted water, so that hydrolysis rate of the tin source in the system declines to a great extent, this is very
Be conducive to the homogeneous nucleation of Sn presomas, while can also effectively control the size of nano-particle, it is avoided to grow up rapidly.
2. since acetone has carbon material excellent wetting property, at the same it is again water-miscible so that during the reaction,
Hydrolyzing obtained Sn presomas can uniformly disperse in expanded graphite substrate, and the reunion between particle is avoided to grow up.
3. nano SnO prepared by the present invention2/ C composite has higher electric conductivity and larger using expanded graphite
The good characteristics such as specific surface area, by ultra-fine nano SnO2In particles supported to the nano-lamellar structure of graphite, alleviate charge and discharge
SnO in the process2Enormousness variation, maintain the stabilization of electrode, improve reversible capacity, improve electrochemistry cyclicity
Energy.
4. the material used in the present invention is cheap and easy to get, simple for process, process is energy-efficient, pollution-free.
Description of the drawings
Fig. 1 is nano SnO2The transmission electron microscope figure of/C composite；
Fig. 2 is nano SnO2The cycle charge discharge electrical property of/C composite.
Specific implementation mode
Embodiment 1
A kind of preparation method of lithium ion battery negative material, takes the SnCl of 0.05g4·5H2O is dissolved in the acetone water of 10ml
In mixed system, wherein acetone and water volume ratio are 1：10, stirring to SnCl4·5H2Urea 0.3g is added after being completely dissolved in O, gathers
Vinylpyrrolidone (PVP) 0.6g is stirred 2 hours, and expanded graphite 0.03g is added, solution is then transferred to 100ml hydro-thermal reactions
In kettle, it is placed in 110 DEG C and carries out hydrothermal synthesis 4 hours, after reaction kettle cooled to room temperature, products therefrom is filtered,
Washing, drying, and 3h are roasted in 600 DEG C of inert gas atmospheres, obtain nano SnO2/ C composite.Sample passes through transmitted electron
Micro- sem observation finds SnO2Nanoparticle size is less than 10nm, and is dispersed on graphite carrier, as shown in Figure 1.Sample
It is tested by charge-discharge performance, capacity is 976mAh/g after 100 cycles, as shown in Figure 2.
Embodiment 2
A kind of preparation method of lithium ion battery negative material, takes the SnCl of 0.3g2·2H2The acetone water that O is dissolved in 50ml is mixed
In zoarium system, wherein acetone and water volume ratio ranging from 10:3, stirring to SnCl2·2H2Urea 1.5g is added after being completely dissolved in O,
Polyvinylpyrrolidone (PVP) 1.4g is stirred 5 hours, and expanded graphite 0.1g is added, it is anti-that solution is then transferred to 100ml hydro-thermals
It answers in kettle, is placed in 130 DEG C and carries out hydrothermal synthesis 2 hours, after reaction kettle cooled to room temperature, products therefrom is taken out
Filter, washing, drying, and 3h are roasted in 600 DEG C of inert gas atmospheres, obtain nano SnO2/ C composite.Sample passes through charge and discharge
Electric performance test, 100 times cycle after capacity be 879mAh/g.
Embodiment 3
A kind of preparation method of lithium ion battery negative material, takes the SnCl of 0.5g4·5H2The acetone water that O is dissolved in 80ml is mixed
In zoarium system, wherein acetone and water volume ratio ranging from 10：1, stirring to SnCl4·5H2Urea 3.5g is added after being completely dissolved in O,
Polyvinylpyrrolidone (PVP) 2.5g is stirred 5 hours, and expanded graphite 0.2g is added, it is anti-that solution is then transferred to 100ml hydro-thermals
It answers in kettle, is placed in 90 DEG C and carries out hydrothermal synthesis 8 hours, after reaction kettle cooled to room temperature, products therefrom is filtered,
Washing, drying, and 3h are roasted in 600 DEG C of inert gas atmospheres, obtain nano SnO2/ C composite.Sample is electrical by charge and discharge
It can test, capacity is 665mAh/g after 100 cycles.
Embodiment 4
A kind of preparation method of lithium ion battery negative material, takes the SnCl of 0.5g2·2H2The acetone water that O is dissolved in 60ml is mixed
In zoarium system, wherein acetone and water volume ratio ranging from 10：4, stirring to SnCl2·2H2Urea 2.5g is added after being completely dissolved in O,
Polyvinylpyrrolidone (PVP) 4g is stirred 5 hours, and expanded graphite 0.15g is added, solution is then transferred to 100ml hydro-thermal reactions
In kettle, it is placed in 100 DEG C and carries out hydrothermal synthesis 6 hours, after reaction kettle cooled to room temperature, products therefrom is filtered,
Washing, drying, and 3h are roasted in 600 DEG C of inert gas atmospheres, obtain nano SnO2/ C composite.Sample is electrical by charge and discharge
It can test, capacity is 732mAh/g after 100 cycles.
Embodiment 5
A kind of preparation method of lithium ion battery negative material, takes the SnCl of 0.1g4·5H2The acetone water that O is dissolved in 50ml is mixed
In zoarium system, wherein acetone and water volume ratio ranging from 3：10, stirring to SnCl4·5H2Urea 0.5g is added after being completely dissolved in O,
Polyvinylpyrrolidone (PVP) 0.1g is stirred 3 hours, and expanded graphite 0.3g is added, it is anti-that solution is then transferred to 100ml hydro-thermals
It answers in kettle, is placed in 120 DEG C and carries out hydrothermal synthesis 4 hours, after reaction kettle cooled to room temperature, products therefrom is taken out
Filter, washing, drying, and 3h are roasted in 600 DEG C of inert gas atmospheres, obtain nano SnO2/ C composite.Sample passes through charge and discharge
Electric performance test, 100 times cycle after capacity be 976mAh/g.
Embodiment 6
A kind of preparation method of lithium ion battery negative material, takes the SnCl of 0.25g4·5H2O is dissolved in the acetone water of 80ml
In mixed system, wherein acetone and water volume ratio ranging from 10：8, stirring to SnCl4·5H2Urea is added after being completely dissolved in O
0.8g, polyvinylpyrrolidone (PVP) 3.2g are stirred 2 hours, and expanded graphite 0.08g is added, solution is then transferred to 100ml
In hydrothermal reaction kettle, be placed in 100 DEG C and carry out hydrothermal synthesis 6 hours, after reaction kettle cooled to room temperature, by products therefrom into
Row is filtered, is washed, is dry, and roasting 3h in 600 DEG C of inert gas atmospheres, obtains nano SnO2/ C composite.Sample passes through
Charge-discharge performance is tested, and capacity is 889mAh/g after 100 cycles.
Claims (4)
1. a kind of preparation method of lithium ion battery negative material, it is characterised in that：Tin source is dissolved in acetone water mixed system,
Urea and polyvinylpyrrolidone is added after being completely dissolved to tin source in stirring, stirs 2~5 hours, adds expanded graphite, then
Solution is transferred in hydrothermal reaction kettle, 90~130 DEG C is placed in and carries out hydrothermal synthesis 2~10 hours, wait for that reaction kettle naturally cools to
After room temperature, products therefrom is filtered, washed, is dried, and 3h is roasted in 600 DEG C of inert gas atmospheres, obtains nano SnO2/
C composite lithium ion battery cathode materials；The tin source is stannic chloride pentahydrate or two water stannous chloride, tin source in the solution
A concentration of 1.5~250mmol/L, the volume ratio of acetone and water is 0.1~10 in the acetone water mixed system.
2. a kind of preparation method of lithium ion battery negative material according to claim 1, it is characterised in that：The solution
Middle urea concentration is 1.2~70g/L.
3. a kind of preparation method of lithium ion battery negative material according to claim 1, it is characterised in that：The solution
Middle polyvinylpyrrolidoneconcentration concentration is 1.0~80g/L.
4. a kind of preparation method of lithium ion battery negative material according to claim 1, it is characterised in that：The solution
Middle a concentration of 0.3~30g/L of expanded graphite.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107799750A (en) * | 2017-10-27 | 2018-03-13 | 广东工业大学 | A kind of tin ash/N doping exfoliated-graphite composite and preparation method thereof |
| CN108163887A (en) * | 2018-01-05 | 2018-06-15 | 宁波工程学院 | Water-soluble SnO2The preparation method of inorganic semiconductor nanometer material and application |
| CN109148845B (en) * | 2018-08-07 | 2021-03-02 | 欣旺达电子股份有限公司 | Nano-tin-modified nitrogen-doped carbon negative electrode material and preparation method thereof |
| CN109546099B (en) * | 2018-10-16 | 2021-08-31 | 中航锂电（洛阳）有限公司 | Graphite composite negative electrode material, preparation method thereof and lithium ion battery |
| CN112234196B (en) * | 2020-09-04 | 2022-11-08 | 陕西科技大学 | Sn nano half-moon tooth particle-2 DLMG composite material synthesized by organic molecule constrained reaction and method |
| CN113562719A (en) * | 2021-06-25 | 2021-10-29 | 鞍钢化学科技有限公司 | Nano SnO2Preparation method of water-soluble asphalt carbon composite electrode negative electrode material |
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| CN104953103A (en) * | 2015-07-09 | 2015-09-30 | 山西大学 | Method for preparing Fe2O3 and expanded graphite composite material of lithium ion battery |
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| US20130337335A1 (en) * | 2011-02-25 | 2013-12-19 | Gwangju Institute of Science and Techology | Negative electrode material for a secondary battery and method for manufacturing same |
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| CN104953103A (en) * | 2015-07-09 | 2015-09-30 | 山西大学 | Method for preparing Fe2O3 and expanded graphite composite material of lithium ion battery |
Non-Patent Citations (1)
| Title |
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| Preparation of SnO2-graphite nanocomposite anodes by urea-mediated hydrolysis;Yong Wang等;《Electrochemistry Communications》;20030403;第5卷(第4期);摘要，第292页右栏第17行至第293页左栏第15行 * |
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