CN105895874B - The method for preparing graphene/tin dioxide quantal-point lithium ion battery negative material - Google Patents
The method for preparing graphene/tin dioxide quantal-point lithium ion battery negative material Download PDFInfo
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- CN105895874B CN105895874B CN201610260682.9A CN201610260682A CN105895874B CN 105895874 B CN105895874 B CN 105895874B CN 201610260682 A CN201610260682 A CN 201610260682A CN 105895874 B CN105895874 B CN 105895874B
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- lithium ion
- ion battery
- tin dioxide
- negative material
- battery negative
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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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- 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 methods preparing graphene/tin dioxide quantal-point lithium ion battery negative material comprising following processing step：1）, glucose and stannous chloride are mixed, ground in the agate mortar；2）, sodium chloride and potassium chloride are mixed, through ball mill ball milling；3）, by step 1）With 2）Material be uniformly mixed, and the pre-heat treatment；4）, the mixing material after the pre-heat treatment is placed in rectangular porcelain boat, porcelain boat is placed in tube furnace, is passed through inert gas shielding, is calcined；5）, isothermal holding is carried out after calcining；6）, under inert gas protection, it is naturally cooling to room temperature, takes out sample；7）, gained sample is cleaned with dilute hydrochloric acid, and material is obtained by vacuum filtration.The present invention is realized extensive synthesizing graphite alkene/tin dioxide quantal-point lithium ion battery negative material, can be widely applied in current lithium ion battery using a single-step solid phase reaction synthetic method using cheap glucose as carbon source.
Description
Technical field
The present invention relates to a kind of preparation methods of lithium ion battery negative material, and in particular to a kind of to prepare graphene/bis-
The method of tin oxide quantum dot lithium ion battery negative material, belongs to novel energy resource material technology field.
Background technology
Lithium ion battery has operating voltage higher, than energy higher, safer and memoryless compared with conventional batteries
Etc. advantages.Since 21 century, environmental pollution getting worse, energy shortage has become the weight for restricting progress of human society development
Problem is wanted, this just forces people urgently to develop the life mode of transportation for producing and being more energy-saving and environmentally friendly, to reduce the petrochemical industry class energy
A large amount of uses, wherein the large-scale use of all kinds of electric vehicles be exactly it is a kind of it is important can reduce environmental pollution replace
Charg`e d'affaires's method.In addition to this, to ensure good cruising ability, each electric appliances in daily life are existing also most using lithium
Ion battery, such as mobile phone, laptop, digital camera and video recorder.Develop high energy storage density and long circulating
The new type lithium ion battery in service life has been a kind of urgent social demand, is the needs of current social development.
The theoretical specific capacity of stannic oxide is 783mAh/g, and specific capacity is high and cheap, is negative electrode of lithium ion battery material
The ideal chose of material.However, stannic oxide is in lithium ion intercalation/deintercalation, it may occur that larger volume expansion/diminution causes
The drastically decline of shorter battery life and capacity.Generally use stannic oxide and graphene are compound at present, pass through the packet of graphene
Volume expansion problem can be alleviated to a certain extent by covering, and significantly improve the electrochemical stability of stannic oxide negative material.
Graphene is a kind of novel two-dimentional carbon nanomaterial, has fabulous conductance property and electrochemical stability, will
Graphene coated not only increases the electric conductivity of composite material, is conducive to lithium ion on the surface of tin oxide nano particles
Rapidly intercalation/deintercalation, and the cyclical stability of battery is also improved, extend the service life of road battery.
There are many method for preparing graphene/tin dioxide quantal-point at present, mostly use first synthesis graphene oxide (GO),
In solution after dioxide composite tin, annealing reduction is being carried out, is finally obtaining redox graphene (RGO)/stannic oxide nanometer
Composite material, these method and processes are excessively cumbersome, and yield is not high, it is difficult to realize real large-scale application.
Therefore, in order to solve the above technical problems, preparing graphene/stannic oxide quantum it is necessory to provide a kind of innovation
The method of point lithium ion battery negative material, to overcome the defect in the prior art.
Invention content
To solve the above problems, the purpose of the present invention is to provide a kind of extensive, low costs to prepare graphene/titanium dioxide
The method of tin quantum dot lithium ion battery negative material.
To achieve the above object, the technical solution that the present invention takes is：Prepare graphene/tin dioxide quantal-point lithium ion
The method of cell negative electrode material, uses one-step synthesis, comprises the technical steps that：
1), glucose and stannous chloride are mixed, ground in the agate mortar；
2), sodium chloride and potassium chloride are mixed, through ball mill ball milling；
3), by step 1) and 2) in obtained material be uniformly mixed, and the pre-heat treatment；
4), the mixing material after the pre-heat treatment is placed in rectangular porcelain boat, porcelain boat is positioned over to the centre position of tube furnace,
It is passed through inert gas shielding, is calcined under certain heating rate；
5) isothermal holding, is carried out after calcining；
6) it, under inert gas protection, is naturally cooling to room temperature, takes out sample；
7), gained sample is cleaned with dilute hydrochloric acid, and by vacuum filtration obtain graphene/tin dioxide quantal-point lithium from
Sub- cell negative electrode material.
The present invention the method for preparing graphene/tin dioxide quantal-point lithium ion battery negative material be further：Step
It is rapid 1) in, the mass ratio of the glucose and stannous chloride is (1-16):1.
The present invention the method for preparing graphene/tin dioxide quantal-point lithium ion battery negative material be further：Step
It is rapid 2) in, the mass ratio of the sodium chloride and potassium chloride is (1-3):1.
The present invention the method for preparing graphene/tin dioxide quantal-point lithium ion battery negative material be further：Step
It is rapid 3) in, the temperature of the pre-heat treatment is 80 DEG C -200 DEG C.
The present invention the method for preparing graphene/tin dioxide quantal-point lithium ion battery negative material be further：Step
It is rapid 4) in, heating rate be 5 DEG C -30 DEG C/min；Calcination temperature is 950 DEG C -1300 DEG C；The inert gas is nitrogen.
The present invention the method for preparing graphene/tin dioxide quantal-point lithium ion battery negative material be further：Step
It is rapid 5) in, the soaking time be 30min-60min.
The present invention the method for preparing graphene/tin dioxide quantal-point lithium ion battery negative material be further：Step
It is rapid 6) in, mixture is placed in beaker, is added 0.5% dilute hydrochloric acid, and 30min is stirred by ultrasonic, and is carried out using the filter membrane of 0.5 mesh true
Sky filters, and 0.5% dilute hydrochloric acid is added again, washes repeatedly 3-5 times；Products therefrom is placed in air dry oven and dries for 24 hours.
The present invention the method for preparing graphene/tin dioxide quantal-point lithium ion battery negative material be further：Step
It is rapid 1) in, need that ammonium chloride is added in the mixture of glucose and stannous chloride, the mass ratio of the glucose and ammonium chloride is 4:
5。
The present invention the method for preparing graphene/tin dioxide quantal-point lithium ion battery negative material be also：Step 1)
In, glucose 0.1g, stannous chloride 0.1g grind 50min；In step 2), sodium chloride 11.4g and potassium chloride 2.8g, ball milling
50min；In step 3), in 150 DEG C of the pre-heat treatment 20h；In step 4), 1000 DEG C are warming up to, heating rate is 20 DEG C/min；
In step 5), 40min is kept the temperature.
Compared with prior art, the present invention has the advantages that：The present invention uses a single-step solid phase reaction synthetic method,
Using cheap glucose as carbon source, extensive synthesizing graphite alkene/tin dioxide quantal-point negative electrode of lithium ion battery is realized
Material is widely used in as negative material in current lithium ion battery.
Description of the drawings
Fig. 1 is the X ray diffracting spectrum (XRD) of sample obtained by the present invention.
Fig. 2 a and Fig. 2 b are field emission scanning electron microscope (SEM) figure of present invention gained sample.
Fig. 3 is transmission electron microscope (TEM) figure of present invention gained sample.
Specific implementation mode
Embodiment 1：
One, raw material are prefabricated
0.8g glucose is weighed, 0.05g stannous chlorides after being sufficiently mixed in glove box, are placed in agate mortar and grind
30min obtains mixture A；11.5g sodium chloride and 11.5g potassium chloride are weighed, to be placed in ball milling in ball mill after being sufficiently mixed
30min obtains mixture B；Mixture A and B are mixed, are placed in rectangular porcelain boat, total mixture amount is no more than porcelain boat total amount
2/3rds.
Two, pretreatment
The mixture of gained in step 1 is placed in vacuum drying chamber, 10h is heat-treated at 80 DEG C；
Three, solid phase reaction
Gained mixture in step 2 is placed among tube furnace boiler tube, nitrogen protection is passed through, is warming up to 950 DEG C, heating
Rate is 5 DEG C/min, after reaching target temperature, keeps the temperature 30min, cooled to room temperature is taken out.
Four, product washs
Porcelain boat product in step 3 is taken out, is placed in 500ml beakers, 0.5% dilute hydrochloric acid is added, is stirred by ultrasonic
30min is filtered by vacuum using the filter membrane of 0.5 mesh, and 0.5% dilute hydrochloric acid is added again, washes repeatedly step, washs 3- altogether
5 times.Products therefrom is placed in air dry oven and dries for 24 hours.
Embodiment 2：
One, raw material are prefabricated
0.1g glucose is weighed, 0.1g stannous chlorides after being sufficiently mixed in glove box, are placed in agate mortar and grind
50min obtains mixture A；11.4g sodium chloride and 2.8g potassium chloride are weighed, to be placed in ball milling in ball mill after being sufficiently mixed
50min obtains mixture B；Mixture A and B are mixed, are placed in rectangular porcelain boat, total mixture amount is no more than porcelain boat total amount
2/3rds.
Two, pretreatment
The mixture of gained in step 1 is placed in vacuum drying chamber, 20h is heat-treated at 150 DEG C；
Three, solid phase reaction
Gained mixture in step 2 is placed among tube furnace boiler tube, nitrogen protection is passed through, is warming up to 1000 DEG C, heating
Rate is 20 DEG C/min, after reaching target temperature, keeps the temperature 40min, cooled to room temperature is taken out.
Four, product washs
Porcelain boat product in step 3 is taken out, is placed in 500ml beakers, 0.5% dilute hydrochloric acid is added, is stirred by ultrasonic
30min is filtered by vacuum using the filter membrane of 0.5 mesh, and 0.5% dilute hydrochloric acid is added again, washes repeatedly step, washs 3- altogether
5 times.Products therefrom is placed in air dry oven and dries for 24 hours.
Embodiment 3：
One, raw material are prefabricated
0.4g glucose, the ammonium chloride of 0.5g are weighed, 0.05g stannous chlorides after being sufficiently mixed in glove box, are placed in agate
60min is ground in Nao mortars, obtains mixture A；13.5g sodium chloride and 11.5g potassium chloride are weighed, to be placed in ball after being sufficiently mixed
Ball milling 60min in grinding machine obtains mixture B；Mixture A and B are mixed, are placed in rectangular porcelain boat, total mixture amount is no more than
2/3rds of porcelain boat total amount.
Two, pretreatment
The mixture of gained in step 1 is placed in vacuum drying chamber, 30h is heat-treated at 200 DEG C；
Three, solid phase reaction
Gained mixture in step 2 is placed among tube furnace boiler tube, nitrogen protection is passed through, is warming up to 1300 DEG C, heating
Rate is 30 DEG C/min, after reaching target temperature, keeps the temperature 60min, cooled to room temperature is taken out.
Four, product washs
Porcelain boat product in step 3 is taken out, is placed in 500ml beakers, 0.5% dilute hydrochloric acid is added, is stirred by ultrasonic
30min is filtered by vacuum using the filter membrane of 0.5 mesh, and 0.5% dilute hydrochloric acid is added again, washes repeatedly step, washs 3- altogether
5 times.Products therefrom is placed in air dry oven and dries for 24 hours.
Sample obtained by technique using the present invention has following characteristics：
1. as shown in Figure 1, being X-ray diffraction (XRD) figure of graphene/tin dioxide quantal-point composite material, XRD spectrum
Show：The main indices of crystallographic plane of compound and the standard X-ray diffraction (pdf document number of tetragonal phase stannic oxide：77-0447) base
This is consistent, such as tetragonal phase stannic oxide (110), (101), (211), (301), (202) face, without other impurity peaks or oxidation
Xi Feng illustrates that the sample being prepared includes tetragonal phase stannic oxide particle.
2. as shown in Fig. 2, for the field emission scanning electron microscope figure of graphene/tin dioxide quantal-point composite material.From figure a
It can be seen that successfully having prepared graphene；It can be seen that the tin dioxide quantal-point of graphene coated, stannic oxide from figure b
Quantum dot is evenly distributed in graphene surface.
3. as shown in figure 3, for the transmission electron microscope figure of graphene/tin dioxide quantal-point composite material.From figure
As can be seen that tin dioxide quantal-point is evenly distributed in graphene surface, grain size is about 3 nanometers, and tin dioxide quantal-point is brilliant
Change perfect, about 0.33 nanometer of spacing of lattice, corresponding (110) crystal face.
Above specific implementation mode is only the preferred embodiment of this creation, all in this wound not to limit this creation
Any modification, equivalent substitution, improvement and etc. done within the spirit and principle of work, should be included in this creation protection domain it
It is interior.
Claims (9)
1. the method for preparing graphene/tin dioxide quantal-point lithium ion battery negative material, it is characterised in that：It uses a step
Synthetic method comprises the technical steps that：
1）, glucose and stannous chloride are mixed, ground in the agate mortar；
2）, sodium chloride and potassium chloride are mixed, through ball mill ball milling；
3）, by step 1）With 2）In obtained material be uniformly mixed, and the pre-heat treatment；
4）, the mixing material after the pre-heat treatment is placed in rectangular porcelain boat, porcelain boat is positioned over to the centre position of tube furnace, is passed through
Inert gas shielding is calcined under certain heating rate；
5）, isothermal holding is carried out after calcining；
6）, under inert gas protection, it is naturally cooling to room temperature, takes out sample；
7）, gained sample is cleaned with dilute hydrochloric acid, and graphene/tin dioxide quantal-point lithium-ion electric is obtained by vacuum filtration
Pond negative material.
2. the method as described in claim 1 for preparing graphene/tin dioxide quantal-point lithium ion battery negative material, special
Sign is：Step 1）In, the mass ratio of the glucose and stannous chloride is（1-16）:1.
3. the method as described in claim 1 for preparing graphene/tin dioxide quantal-point lithium ion battery negative material, special
Sign is：Step 2）In, the mass ratio of the sodium chloride and potassium chloride is（1-3）:1.
4. the method as described in claim 1 for preparing graphene/tin dioxide quantal-point lithium ion battery negative material, special
Sign is：Step 3）In, the temperature of the pre-heat treatment is 80 DEG C -200 DEG C.
5. the method as described in claim 1 for preparing graphene/tin dioxide quantal-point lithium ion battery negative material, special
Sign is：Step 4）In, heating rate is 5 DEG C -30 DEG C/min；Calcination temperature is 950 DEG C -1300 DEG C；The inert gas is
Nitrogen.
6. the method as described in claim 1 for preparing graphene/tin dioxide quantal-point lithium ion battery negative material, special
Sign is：Step 5）In, the soaking time is 30min-60min.
7. the method as described in claim 1 for preparing graphene/tin dioxide quantal-point lithium ion battery negative material, special
Sign is：Step 7）In, mixture is placed in beaker, and 0.5% dilute hydrochloric acid is added, and 30min is stirred by ultrasonic, using 0.5 purpose
Filter membrane is filtered by vacuum, and 0.5% dilute hydrochloric acid is added again, washes repeatedly 3-5 times；Products therefrom is placed in air dry oven
Drying is for 24 hours.
8. the method as described in claim 1 for preparing graphene/tin dioxide quantal-point lithium ion battery negative material, special
Sign is：Step 1）In, it needs that ammonium chloride, the matter of the glucose and ammonium chloride is added in the mixture of glucose and stannous chloride
Amount is than being 4:5.
9. the method for preparing graphene/tin dioxide quantal-point lithium ion battery negative material as described in claim 1, special
Sign is：Step 1）In, glucose 0.1g, stannous chloride 0.1g grind 50min；Step 2）In, sodium chloride 11.4g and chlorination
Potassium 2.8g, ball milling 50min；Step 3）In, in 150 DEG C of the pre-heat treatment 20h；Step 4）In, 1000 DEG C are warming up to, heating rate is
20 DEG C/min；Step 5）In, keep the temperature 40min.
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| CN106803577B (en) * | 2016-12-31 | 2019-06-14 | 浙江工业大学 | A kind of hollow copper quantum dot/mesoporous carbon composite material and its preparation method and application |
| CN108264099B (en) * | 2018-01-03 | 2019-11-26 | 桂林理工大学 | A kind of preparation method of lithium ion battery high-performance two-dimensional sheet nickel oxide negative electrode material |
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| CN101478043A (en) * | 2009-01-08 | 2009-07-08 | 上海交通大学 | Negative pole material for lithium ionic cell and preparation process thereof |
| CN102208639A (en) * | 2011-05-09 | 2011-10-05 | 北京化工大学 | Graphene/transition metal oxide composite cathode material and preparation method thereof |
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| US9017867B2 (en) * | 2009-08-10 | 2015-04-28 | Battelle Memorial Institute | Self assembled multi-layer nanocomposite of graphene and metal oxide materials |
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| CN101478043A (en) * | 2009-01-08 | 2009-07-08 | 上海交通大学 | Negative pole material for lithium ionic cell and preparation process thereof |
| CN102208639A (en) * | 2011-05-09 | 2011-10-05 | 北京化工大学 | Graphene/transition metal oxide composite cathode material and preparation method thereof |
| CN103441254A (en) * | 2013-09-03 | 2013-12-11 | 青岛科技大学 | Preparation method of graphene-supported stannic oxide quantum dot negative electrode material for lithium ion battery |
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