CN105742597A - Preparation method for novel negative electrode material of lithium ion battery - Google Patents
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- CN105742597A CN105742597A CN201610141165.XA CN201610141165A CN105742597A CN 105742597 A CN105742597 A CN 105742597A CN 201610141165 A CN201610141165 A CN 201610141165A CN 105742597 A CN105742597 A CN 105742597A
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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
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- 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 preparation method for a novel negative electrode material of a lithium ion battery, belongs to the technical field of a lithium ion battery material, and aims to provide a preparation method for a novel nanometer SnO<2>/C composite negative electrode material of the lithium ion battery. The preparation method for the novel negative electrode material of the lithium ion battery comprises the steps of dissolving a tin source into a mixed acetone water system, stirring until the tin source is fully dissolved, then adding urea and polyvinylpyrrolidone, stirring for 2-5h, then adding expanded graphite, next, moving the solution to a hydrothermal reaction kettle, and performing hydrothermal synthesis at a temperature of 90-130 DEG C for 2-10h, naturally cooling the reaction kettle to the room temperature, and performing suction filtration, washing and drying on the obtained product, and baking under an inert atmosphere at a temperature of 600 DEG C for 3h to obtain the nanometer SnO<2>/C composite negative electrode material of the lithium ion battery.
Description
Technical field
The preparation method that the present invention relates to a kind of Novel cathode material for lithium ion battery, belongs to lithium ion battery material technical field.
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 (energy density per unit volume and specific energy), low self-discharge rate, wide use temperature range, long circulation life, environmental protection, memory-less effect and can the characteristic such as high current charge-discharge, it is widely used in fields such as mobile communication equipment, portable electric appts, electric automobiles rapidly, has become as one of modern and that future is important green energy resource.Wherein, negative material is one of key factor determining lithium ion battery combination property quality.At present, it is poor etc. to there is theoretical capacity low (being about 372mAh/g), high rate performance in commercialization graphite cathode material, can not meet the demand of high-energy-density, high power density lithium ion battery.Therefore, other alternative high power capacity, high cyclical stability, energy fast charging and discharging negative material are explored, it has also become one of focus studied in the world.
SnO2Because having high theoretical capacity (782mAh/g), low cost and the advantage such as have no side effect, and enjoy the concern of researcher.But SnO2The subject matter existed is along with huge change in volume in charge and discharge cycles process, and the easy efflorescence of material, inefficacy, therefore cycle performance is poor.It addition, SnO2Electric conductivity not good, also lead to its high rate performance poor.By SnO2Material nano and carry out compound with material with carbon element and can be obviously improved this change in volume problem, and improve material conductivity.Main reason is that, the stress produced during the change of the particle volume of nanorize is less, and granule is not easy to crush, efflorescence, and can effectively prevent nano SnO with material with carbon element compound2The reunion of granule is grown up, it is provided that conductive network, and change in volume when being buffered in discharge and recharge, and then the stability of material and high rate performance can be greatly improved.
Can be used in the material with carbon element of compound and mainly include amorphous carbon, CNT, Graphene etc..Wherein, the electric conductivity of graphene-based nanometer sheet Yin Qigao, mechanical strength and preferably elasticity be widely used for design high-performance negative material.But, the preparation process of present stage Graphene is complicated, relatively costly, and the requirement for distance commercialization low cost, simple process also has bigger gap.Comparing redox graphene, expanded graphite has that preparation method is simple, with low cost, lamella is big, defect is few, good conductivity and the advantage such as hole is abundant.Although expanded graphite has had application in other fields such as absorption, but seldom has been reported that in lithium ion battery negative material field.
Hydrothermal synthesis method is the conventional synthetic method of field of nanometer material technology, existing nano SnO2Negative material also more adopts this means to prepare.But with regard to current SnO2The present Research of/C composite, prepares SnO2Dispersed and with the effective compound of carbon the negative material of nano-particle is still a relatively larger challenge.Main reason is that mostly material with carbon element is hydrophobic material, be difficult to be flooded profit during reaction in water solution system.So the SnO being obtained by reacting2Nano-particle with carbon compound tense, nano-particle is easily reunited and is grown up, and oarse-grained SnO2It is easy to efflorescence of breaking, so that material capacity declines rapidly when circulation.Therefore, novel processing step be developed into SnO2The important directions of/C composite research.
Summary of the invention
It is an object of the invention to provide a kind of new type lithium ion battery nano SnO2The preparation method of/C composite negative pole material.
In order to achieve the above object, present invention employs techniques below scheme:
A kind of preparation method of Novel cathode material for lithium ion battery, Xi Yuan is dissolved in acetone water mixed system, stirring adds carbamide and polyvinylpyrrolidone after being completely dissolved to Xi Yuan, stirs 2～5 hours, adds expanded graphite, then solution is proceeded in hydrothermal reaction kettle, it is placed in 90～130 DEG C and carries out Hydrothermal Synthesis 2～10 hours, after question response still naturally cools to room temperature, products therefrom is carried out sucking filtration, washing, dries, and in 600 DEG C of inert gas atmosphere roasting 3h, obtain nano SnO2/ C composite lithium ion battery cathode material.
Xi Yuan of the present invention is stannic chloride pentahydrate or two water stannum dichloride.
In solution of the present invention, the concentration of Xi Yuan is 1.5～250mmol/L.
In acetone water mixed system of the present invention, the volume ratio of acetone and water is 0.1～10.
In solution 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, expanded graphite concentration is 0.3～30g/L.
Compared with prior art, present invention have 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, water adds acetone be equivalent to dilute water, so that the hydrolysis rate that Xi Yuan is in this system declines to a great extent, this is advantageous to the homogeneous nucleation of Sn presoma, can also effectively control the size of nanoparticle, it is to avoid it is grown up rapidly simultaneously.
2. owing to material with carbon element is had excellent wetting property by acetone, simultaneously water-miscible again so that in course of reaction, the Sn presoma that hydrolysis obtains can disperse uniformly in expanded graphite substrate, it is to avoid the reunion between granule is grown up.
3. the nano SnO that prepared by the present invention2/ C composite utilizes expanded graphite to have the good characteristic such as higher electric conductivity and bigger specific surface area, by ultra-fine nano SnO2Particles supported, to the nano-lamellar structure of graphite, alleviates SnO in charge and discharge process2Enormousness change, maintain stablizing of electrode, improve reversible capacity, improve electrochemistry cycle performance.
4. the material used by the present invention is cheap and easy to get, and technique is simple, and the course of processing is energy-efficient, pollution-free.
Accompanying drawing explanation
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.
Detailed description of the invention
Embodiment 1
The preparation method of a kind of Novel cathode material for lithium ion battery, takes the SnCl of 0.05g4·5H2O is dissolved in the acetone water mixed system of 10ml, and wherein acetone and water volume ratio are 1:10, stirs to SnCl4·5H2O adds carbamide 0.3g after being completely dissolved, polyvinylpyrrolidone (PVP) 0.6g, stir 2 hours, add expanded graphite 0.03g, then solution is proceeded in 100ml hydrothermal reaction kettle, be placed in 110 DEG C and carry out Hydrothermal Synthesis 4 hours, after question response still naturally cools to room temperature, products therefrom is carried out sucking filtration, washing, dries, and in 600 DEG C of inert gas atmosphere roasting 3h, obtain nano SnO2/ C composite.Sample is through transmission electron microscope observation, it has been found that SnO2Nanoparticle size is less than 10nm, and is dispersed on graphite carrier, as shown in Figure 1.Sample is tested through charge-discharge performance, and after 100 circulations, capacity is 976mAh/g, as shown in Figure 2.
Embodiment 2
The preparation method of a kind of Novel cathode material for lithium ion battery, takes the SnCl of 0.3g2·2H2O is dissolved in the acetone water mixed system of 50ml, and wherein acetone and water volume ratio range for 10:3, stirs to SnCl2·2H2O adds carbamide 1.5g after being completely dissolved, polyvinylpyrrolidone (PVP) 1.4g, stir 5 hours, add expanded graphite 0.1g, then solution is proceeded in 100ml hydrothermal reaction kettle, be placed in 130 DEG C and carry out Hydrothermal Synthesis 2 hours, after question response still naturally cools to room temperature, products therefrom is carried out sucking filtration, washing, dries, and in 600 DEG C of inert gas atmosphere roasting 3h, obtain nano SnO2/ C composite.Sample is tested through charge-discharge performance, and after 100 circulations, capacity is 879mAh/g.
Embodiment 3
The preparation method of a kind of Novel cathode material for lithium ion battery, takes the SnCl of 0.5g4·5H2O is dissolved in the acetone water mixed system of 80ml, and wherein acetone and water volume ratio range for 10:1, stirs to SnCl4·5H2O adds carbamide 3.5g after being completely dissolved, polyvinylpyrrolidone (PVP) 2.5g, stir 5 hours, add expanded graphite 0.2g, then solution is proceeded in 100ml hydrothermal reaction kettle, be placed in 90 DEG C and carry out Hydrothermal Synthesis 8 hours, after question response still naturally cools to room temperature, products therefrom is carried out sucking filtration, washing, dries, and in 600 DEG C of inert gas atmosphere roasting 3h, obtain nano SnO2/ C composite.Sample is tested through charge-discharge performance, and after 100 circulations, capacity is 665mAh/g.
Embodiment 4
The preparation method of a kind of Novel cathode material for lithium ion battery, takes the SnCl of 0.5g2·2H2O is dissolved in the acetone water mixed system of 60ml, and wherein acetone and water volume ratio range for 10:4, stirs to SnCl2·2H2O adds carbamide 2.5g after being completely dissolved, polyvinylpyrrolidone (PVP) 4g, stir 5 hours, add expanded graphite 0.15g, then solution is proceeded in 100ml hydrothermal reaction kettle, be placed in 100 DEG C and carry out Hydrothermal Synthesis 6 hours, after question response still naturally cools to room temperature, products therefrom is carried out sucking filtration, washing, dries, and in 600 DEG C of inert gas atmosphere roasting 3h, obtain nano SnO2/ C composite.Sample is tested through charge-discharge performance, and after 100 circulations, capacity is 732mAh/g.
Embodiment 5
The preparation method of a kind of Novel cathode material for lithium ion battery, takes the SnCl of 0.1g4·5H2O is dissolved in the acetone water mixed system of 50ml, and wherein acetone and water volume ratio range for 3:10, stirs to SnCl4·5H2O adds carbamide 0.5g after being completely dissolved, polyvinylpyrrolidone (PVP) 0.1g, stir 3 hours, add expanded graphite 0.3g, then solution is proceeded in 100ml hydrothermal reaction kettle, be placed in 120 DEG C and carry out Hydrothermal Synthesis 4 hours, after question response still naturally cools to room temperature, products therefrom is carried out sucking filtration, washing, dries, and in 600 DEG C of inert gas atmosphere roasting 3h, obtain nano SnO2/ C composite.Sample is tested through charge-discharge performance, and after 100 circulations, capacity is 976mAh/g.
Embodiment 6
The preparation method of a kind of Novel cathode material for lithium ion battery, takes the SnCl of 0.25g4·5H2O is dissolved in the acetone water mixed system of 80ml, and wherein acetone and water volume ratio range for 10:8, stirs to SnCl4·5H2O adds carbamide 0.8g after being completely dissolved, polyvinylpyrrolidone (PVP) 3.2g, stir 2 hours, add expanded graphite 0.08g, then solution is proceeded in 100ml hydrothermal reaction kettle, be placed in 100 DEG C and carry out Hydrothermal Synthesis 6 hours, after question response still naturally cools to room temperature, products therefrom is carried out sucking filtration, washing, dries, and in 600 DEG C of inert gas atmosphere roasting 3h, obtain nano SnO2/ C composite.Sample is tested through charge-discharge performance, and after 100 circulations, capacity is 889mAh/g.
Claims (7)
1. the preparation method of a Novel cathode material for lithium ion battery, it is characterized in that: Jiang Xiyuan is dissolved in acetone water mixed system, stirring adds carbamide and polyvinylpyrrolidone after being completely dissolved to Xi Yuan, stir 2～5 hours, add expanded graphite, then solution is proceeded in hydrothermal reaction kettle, it is placed in 90～130 DEG C and carries out Hydrothermal Synthesis 2～10 hours, after question response still naturally cools to room temperature, products therefrom is carried out sucking filtration, washing, dries, and in 600 DEG C of inert gas atmosphere roasting 3h, obtain nano SnO2/ C composite lithium ion battery cathode material.
2. the preparation method of a kind of Novel cathode material for lithium ion battery according to claim 1, it is characterised in that: described Xi Yuan is stannic chloride pentahydrate or two water stannum dichloride.
3. the preparation method of a kind of Novel cathode material for lithium ion battery according to claim 1, it is characterised in that: in described solution, the concentration of Xi Yuan is 1.5～250mmol/L.
4. the preparation method of a kind of Novel cathode material for lithium ion battery according to claim 1, it is characterised in that: in described acetone water mixed system, the volume ratio of acetone and water is 0.1～10.
5. the preparation method of a kind of Novel cathode material for lithium ion battery according to claim 1, it is characterised in that: in described solution, urea concentration is 1.2～70g/L.
6. the preparation method of a kind of Novel cathode material for lithium ion battery according to claim 1, it is characterised in that: in described solution, polyvinylpyrrolidoneconcentration concentration is 1.0～80g/L.
7. the preparation method of a kind of Novel cathode material for lithium ion battery according to claim 1, it is characterised in that: in described solution, expanded graphite concentration is 0.3～30g/L.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109148845A (en) * | 2018-08-07 | 2019-01-04 | 欣旺达电子股份有限公司 | The nitrogen-doped carbon negative electrode material and preparation method thereof of nanometer tin modification |
| CN109546099A (en) * | 2018-10-16 | 2019-03-29 | 中航锂电（洛阳）有限公司 | A kind of composite cathode material of silicon/carbon/graphite and preparation method thereof, lithium ion battery |
| CN112234196A (en) * | 2020-09-04 | 2021-01-15 | 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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| 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 |
| 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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2016
- 2016-03-11 CN CN201610141165.XA patent/CN105742597B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| 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)
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| YONG WANG等: "Preparation of SnO2-graphite nanocomposite anodes by urea-mediated hydrolysis", 《ELECTROCHEMISTRY COMMUNICATIONS》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109148845A (en) * | 2018-08-07 | 2019-01-04 | 欣旺达电子股份有限公司 | The nitrogen-doped carbon negative electrode material and preparation method thereof of nanometer tin modification |
| 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 |
| CN109546099A (en) * | 2018-10-16 | 2019-03-29 | 中航锂电（洛阳）有限公司 | A kind of composite cathode material of silicon/carbon/graphite and preparation method thereof, lithium ion battery |
| CN112234196A (en) * | 2020-09-04 | 2021-01-15 | 陕西科技大学 | Sn nano half-moon tooth particle-2 DLMG composite material synthesized by organic molecule constrained reaction and method |
| 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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