CN104716311B - A kind of stannic disulphide nano slice composite and its preparation method and application - Google Patents
A kind of stannic disulphide nano slice composite and its preparation method and application Download PDFInfo
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- CN104716311B CN104716311B CN201510073828.4A CN201510073828A CN104716311B CN 104716311 B CN104716311 B CN 104716311B CN 201510073828 A CN201510073828 A CN 201510073828A CN 104716311 B CN104716311 B CN 104716311B
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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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- 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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- 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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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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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- 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
This application discloses a kind of stannic disulphide nano slice composite and its preparation method and application.The preparation method of the application includes, and Xi Yuan is mixed by (1) with L cysteine solution, reacting by heating 5 30 hours, natural cooling, is replaced with water and ethanol and washs, obtains flower-shaped stannic disulphide nano slice；(2) stannic disulfide and Oleic acid are according to weight 1:20‑1:60 mixing, soak 24 48 hours, and centrifugation removes unnecessary Oleic acid, heat 18 hours in 400 1000 DEG C of inert gas atmospheres, obtain agraphitic carbon cladding stannic disulphide nano slice composite.The present processes utilize Oleic acid adsorbing material flash annealing to form agraphitic carbon, flower-shaped stannic disulphide nano slice Surface coating amorphous carbon layer in hydro-thermal method preparation, method is simple, easy to operate, the agraphitic carbon cladding stannic disulphide nano slice composite of preparation, surface area is big, piece is thin, as battery cathode use with good cycling stability, rate capability high the features such as.
Description
Technical field
The application is related to lithium ion battery negative material field, more particularly to a kind of stannic disulphide nano slice composite
And its preparation method and application.
Background technology
The pressure of and ecological deterioration trend exhausted with fossil energy, Development of EV and hybrid-electric car gesture are must
OK.At present, the power supply as one of the core technology of electric automobile is the bottleneck quickly propelling Development of Electric Vehicles.Lithium-ion electric
Pond compared with other secondary power supplies, have the advantages that energy density is high, power density is big, environmental protection it is considered to be having most before
One of the power supply on way.However, its capacity low be still major issue, the graphite cathode capacity of especially its business application is about
370mAh/g.The emphasis of current lithium ion battery negative material research includes：Silicon substrate, tinbase, various material with carbon element.Material with carbon element capacity
Low, silicon substrate capacity is high but in charge and discharge process, change in volume is very big, causes capacity attenuation fast；It is compared to other negative materials,
Tin-based material is between.Stannic disulfide has layer structure, has higher lithium storage content and structural stability.However, two
Tin disulfide has relatively low electrical conductivity, restricts its charge/discharge capacity under high current density.
Content of the invention
The purpose of the application is to provide a kind of improved flower-shaped stannic disulphide nano slice composite of micro structure and its preparation
Methods and applications.
To achieve these goals, the application employs technical scheme below：
The one side of the application discloses a kind of preparation method of stannic disulphide nano slice composite, walks including following
Suddenly, (1) mixes stannum source solution and L-Cysteine solution as reactant liquor, reacting by heating 5-30 hour, reacts after terminating certainly
So cool down, replaced with water and ethanol and wash, obtain flower-shaped stannic disulphide nano slice；(2) stannic disulfide prepared by step (1) with
Oleic acid is according to weight 1:20-1:60 mixing, make stannic disulfide be fully immersed in Oleic acid, soak 24-48 hour, and centrifugation removes many
Remaining Oleic acid, at 400-1000 DEG C, heats 1-8 hour, obtains the stannic disulfide of agraphitic carbon cladding in inert gas atmosphere
Nanosheet composite material.
It should be noted that it is critical only that of the application will prepare hydro-thermal method and the Oleic acid annealing shape of stannic disulphide nano slice
Amorphous carbon is become to combine, the creative Surface coating at least one of which amorphous carbon in stannic disulphide nano slice, and single
Stannic disulfide is compared, the composite of the application, not only further increases specific capacity, and improves cycle life.This Shen
In implementation please, stannic disulfide and Oleic acid adopt ultrasonic mixing, to reach well-mixed purpose.
Also, it should be noted the concrete operations mode that water and ethanol replace washing produces two sulfur with reference to conventional hydro-thermal method
Change the mode of washing in stannum nanometer sheet, here is not specifically limited；Additionally, the key of the application is to form agraphitic carbon bag
The stannic disulphide nano slice composite covering, in follow-up application, for example prepare negative material when, its following process according to
Depending on specific working condition or production purpose, here is not specifically limited.
Preferably, Xi Yuan is at least one in butter of tin, tin tetraiodide and tin tetrabromide.It should be noted that this
In a kind of implementation of application, it is preferred to use butter of tin.
Preferably, in reactant liquor, the mol ratio of Xi Yuan and L-Cysteine is 1:4-1:8.It should be noted that Xi Yuan and
The amount ratio of L-Cysteine, is defined that is to say, that participating in the chemical agent of reaction with it by generating stannic disulfide to greatest extent
Amount ratio is defined, the concrete working condition in conjunction with the application and purpose, and the application is preferred, using rubbing of Xi Yuan and L-Cysteine
That ratio is 1:4-1:8 amount is reacted；And, preferably adopt butter of tin to be Xi Yuan.
Preferably, in reactant liquor, the concentration of Xi Yuan is 0.02mol/L-0.1mol/L.It should be noted that stannum source concentration
Restriction, actually the restriction of reaction solution concentration it will be understood that need when Xi Yuan is reacted with L-Cysteine will both fully
Mix, concentration is too low, and yield is also low, affect production efficiency, and concentration is too high, is unfavorable for that reaction is carried out；Therefore, the application is excellent
The concentration using Xi Yuan of choosing is reacted for 0.02mol/L-0.1mol/L.
Preferably, in step (1), reaction temperature is 150-240 DEG C.It should be noted that reaction temperature refer to Xi Yuan with
The temperature of L-Cysteine hydro-thermal reaction, the application preferably adopts 150-240 DEG C that is to say, that reacting at 150-240 DEG C
5-30 hour.
The another side of the application also discloses the stannic disulphide nano slice composite of the preparation method preparation of the application, its
The surface of stannic disulphide nano slice is in flower-shaped, and its Surface coating has amorphous carbon layer.
Preferably, in the stannic disulphide nano slice composite of the application, amorphous carbon layer accounts for the 5%-15% of gross weight.
It should be noted that the Main Function of amorphous carbon is to play electric conductivity, to make up the defect of stannic disulfide conductivity difference, because
This, if can be complete by stannic disulfide wrap up wherein；In the application it is contemplated that specific capacity and electric conductivity etc. comprehensive because
Element is it is preferred that make the amorphous carbon of cladding stannic disulfide account for the 5%-15% of gross weight.
Additionally, the application is to use Shortcomings to enter for existing stannic disulfide as lithium ion battery negative material
Row research, therefore, lithium-ion electric prepared by the stannic disulphide nano slice composite that the application further provides the application
Application in the negative material of pond.It should be noted that in a kind of implementation of the application, stannic disulfide prepared by the application
Nanosheet composite material, together with conventional conductive agent and binding agent, is prepared into negative material for lithium ion battery.Wherein, lead
Electric agent is preferably acetylene black, the preferred Carboxymethyl cellulose sodium of binding agent (abbreviation CMC).
Therefore, the application simultaneously disclose a kind of negative material for lithium ion battery again, contain in this negative material
There is the stannic disulphide nano slice composite of the application.
Further, in a kind of implementation of the application, by the stannic disulphide nano slice composite containing the application
Negative material make lithium ion battery；Therefore, the application simultaneously disclose a kind of curing sijna containing the application again
The lithium ion battery made by negative material of rice piece composite.
Because using above technical scheme, the application has the beneficial effects that：
The preparation method of the application utilizes Oleic acid absorption crystal face annealing to form agraphitic carbon, flower-shaped the two of hydro-thermal method preparation
Tin disulfide nanometer sheet Surface coating amorphous carbon layer, preparation method is simple, easy to operate.And, the preparation method of the application is made
The stannic disulphide nano slice composite of standby agraphitic carbon cladding, surface area is big, piece is thin, uses to have as battery cathode and follows
The features such as ring good stability, rate capability are high.
Brief description
Fig. 1 is the scanning electron microscope (SEM) photograph of the stannic disulphide nano slice composite of agraphitic carbon cladding in the embodiment of the present application；
Fig. 2 is the transmission electron microscope picture of the stannic disulphide nano slice composite of agraphitic carbon cladding in the embodiment of the present application；
Fig. 3 is the button as negative material for the stannic disulphide nano slice composite adopting the application in the embodiment of the present application
The capacity curve figure of charged/discharged first of formula battery；
Fig. 4 is the button as negative material for the stannic disulphide nano slice composite adopting the application in the embodiment of the present application
The charging cycle performance chart of formula battery；
Fig. 5 is the button as negative material for the stannic disulphide nano slice composite adopting the application in the embodiment of the present application
The multiplying power charging performance curve chart of formula battery.
Specific embodiment
Amorphous carbon, as a kind of special defect grapheme material, is rarely used in composite, and the application is creative
Utilization Oleic acid annealing formed amorphous carbon feature, in advance Oleic acid mix with stannic disulfide, then is annealed, formed nothing determine
The stannic disulphide nano slice composite of shape carbon coating.The composite of the application preparation has good specific capacity stable circulation
The features such as property is good, rate capability is high.
It should be noted that the flower-shaped stannic disulphide nano slice of the application preparation, its surface is in flower-like structure；As Fig. 1 institute
Show, whole stannic disulfide is in flaky nanometer structure, the stannic disulphide nano slice of flower-shaped surface texture is absorption Oleic acid, it is no fixed to be formed
Shape carbon coating layer is provided convenience.
Below by specific embodiments and the drawings, the application is described in further detail.Following examples are only to the application
It is further described, should not be construed as the restriction to the application.
Embodiment one
The stannic disulphide nano slice composite material and preparation method thereof of this example is as follows：
(1) respectively the L-Cysteine of the butter of tin aqueous solution of 20ml 0.04mol/L and 20ml 0.16mol/L is mixed
It is combined and makes reactant liquor, reactant liquor is transferred in 50 milliliters of polytetrafluoro container, and polytetrafluoro container is fixed on not
In the reactor of rust steel, then with baking oven directly at 200 DEG C, heat 20 hours, the temperature of question response kettle is reduced to room temperature naturally
When, obtained reactant is washed 3 times successively with water and ethanol respectively, the sample after washing is dried 12 in 50 DEG C of baking ovens little
When, obtaining surface is in flower-shaped stannic disulphide nano slice；Wherein, in reactant liquor, the concentration of butter of tin is 0.02mol/L.
(2) stannic disulfide and then by step (1) prepared compares 1 with Oleic acid according to weight：40 ultrasonic 1 hour of mixing, soak
24 hours, unnecessary Oleic acid was removed in centrifugation, is mixed thing and heats the agraphitic carbon obtaining this example for 3 hours for 800 DEG C in argon
The flower-shaped stannic disulphide nano slice composite of cladding.
Through measurement, in the composite of this example, the stannic disulphide nano slice that agraphitic carbon content accounts for agraphitic carbon cladding is multiple
The 13.9% of condensation material gross weight.
Observed using the composite that scanning electron microscope and transmission electron microscope are prepared to this example, result such as Fig. 1 and Fig. 2 institute
Show, Fig. 1 coats the scanning electron microscope (SEM) photograph of flower-shaped stannic disulphide nano slice, as shown in Figure 1, this example for agraphitic carbon prepared by this example
Agraphitic carbon cladding stannic disulphide nano slice size is about 2 microns, and its thickness is about 10 nanometers.Fig. 2 is prepared for this example
Agraphitic carbon coats the transmission electron microscope picture of flower-shaped stannic disulphide nano slice, as shown in Figure 2, the agraphitic carbon cladding curing of this example
The thickness of the clad of stannum is 3.5nm.
Agraphitic carbon prepared by this example coats flower-shaped stannic disulphide nano slice composite and makes lithium ion battery negative
Material, and its chemical property is tested using button cell.In the lithium ion battery negative material of this example, conductive agent adopts acetylene
Black, binding agent adopts CMC, stannic disulphide nano slice composite：Acetylene black：CMC is according to weight than 80wt.%: 10wt.%:
The ratio mix homogeneously of 10wt.%, coats on Copper Foil.In button cell, electrolyte adopts the LiPF of 1mol/L6/EC-DEC-
DMC (1: 1: 1, w/w).Respectively charged/discharged is carried out with 100mA/g, potential range is 0.01～2.5V.After tested, when with
During the electric current charging and discharging of 100mA/g, charge specific capacity can reach 1580mAh/g within the 1st week, and after 140 circulations, discharge capacity is
990mAh/g.Fig. 3, Fig. 4, Fig. 5 are respectively the charge and discharge that agraphitic carbon coats the different circulations of flower-shaped stannic disulfide piece composite
Electric curve, cycle characteristics curve and multiplying power property curve.
Embodiment two
This example is mixed with the L-Cysteine of the butter of tin aqueous solution of the 0.2mol/L of 20ml and the 0.8mol/L of 20ml
Prepare stannic disulfide together, and baking oven, directly at 240 DEG C, heats 20 hours that is to say, that hydrothermal temperature is 240
DEG C, in step (2), stannic disulfide compares 1 with Oleic acid according to weight：60 ultrasonic 1 hour of mixing, soak 48 hours, centrifugation is removed many
Excess oil acid.Remaining step is all identical with embodiment one with condition.
Observed using the composite that scanning electron microscope is prepared to this example, result shows, the agraphitic carbon cladding of this example
Stannic disulphide nano slice a size of 3 microns, its nanometer sheet thickness is about 10 nanometers.Through measurement, in the composite of this example,
Agraphitic carbon content accounts for the 13.7% of the stannic disulphide nano slice composite gross weight of agraphitic carbon cladding.
This example prepares negative material using embodiment one identical method, equally tests its electrochemistry using button cell
Can, the preparation method of button cell is all identical with embodiment one with method of testing.Test result shows, when with the electricity of 100mA/g
During current charge electric discharge, charge specific capacity can reach 1220mAh/g within the 1st week, and after 140 circulations, discharge capacity is 971mAh/g.
Embodiment three
This example is mixed with the L-Cysteine of the butter of tin aqueous solution of the 0.1mol/L of 20ml and the 0.4mol/L of 20ml
Prepare stannic disulfide together, and baking oven, directly at 180 DEG C, heats 20 hours that is to say, that hydrothermal temperature is 180
DEG C, in step (2), stannic disulfide compares 1 with Oleic acid according to weight：50 ultrasonic 1 hour of mixing, soak 36 hours, centrifugation is removed many
Excess oil acid.Remaining step is all identical with embodiment one with condition.
Observed using the composite that scanning electron microscope is prepared to this example, result shows, the agraphitic carbon cladding of this example
Stannic disulphide nano slice a size of 3.5 microns, its nanometer sheet thickness is about 10 nanometers.Through measurement, the composite of this example
In, agraphitic carbon content accounts for the 14% of the stannic disulphide nano slice composite gross weight of agraphitic carbon cladding.
This example prepares negative material using embodiment one identical method, equally tests its electrochemistry using button cell
Can, the preparation method of button cell is all identical with embodiment one with method of testing.Test result shows, when with the electricity of 100mA/g
During current charge electric discharge, specific discharge capacity can reach 1250mAh/g within the 1st week, and 140 discharge capacities are 950mAh/g.
Example IV
This example prepares stannic disulphide nano slice composite using with embodiment one identical condition and method, uniquely different
, in step (2), in argon, 1000 DEG C are heated 3 hours, and remaining is all identical with embodiment one.
Observed using the composite that scanning electron microscope is prepared to this example, result shows, the agraphitic carbon cladding of this example
Stannic disulphide nano slice a size of 2.5 microns, its nanometer sheet thickness is about 10 nanometers.Through measurement, the composite of this example
In, agraphitic carbon content accounts for the 14.1% of the stannic disulphide nano slice composite gross weight of agraphitic carbon cladding.
This example prepares negative material using embodiment one identical method, equally tests its electrochemistry using button cell
Can, the preparation method of button cell is all identical with embodiment one with method of testing.Test result shows, when with the electricity of 100mA/g
During current charge electric discharge, charge specific capacity can reach 1322mAh/g within the 1st week, and after 140 circulations, discharge capacity is 1020mAh/g.
Embodiment five
This example is mixed with the L-Cysteine of the butter of tin aqueous solution of the 0.04mol/L of 20ml and the 0.32mol/L of 20ml
It is combined and prepares stannic disulfide, and baking oven, directly at 240 DEG C, heats 20 hours that is to say, that hydrothermal temperature is
240 DEG C, in step (2), in argon, 400 DEG C are heated 3 hours, and remaining step is all identical with embodiment one with condition.
Observed using the composite that scanning electron microscope is prepared to this example, result shows, the agraphitic carbon cladding of this example
Stannic disulphide nano slice a size of 4 microns, its nanometer sheet thickness is about 10 nanometers.Through measurement, in the composite of this example,
Agraphitic carbon content accounts for the 15.2% of the stannic disulphide nano slice composite gross weight of agraphitic carbon cladding.
This example prepares negative material using embodiment one identical method, equally tests its electrochemistry using button cell
Can, the preparation method of button cell is all identical with embodiment one with method of testing.Test result shows, when with the electricity of 100mA/g
During current charge electric discharge, charge specific capacity can reach 1158mAh/g within the 1st week, and after 140 circulations, discharge capacity is 1911mAh/g.
Embodiment six
This example prepares stannic disulphide nano slice composite using with embodiment one identical condition and method, different
It is that, in step (1), baking oven, directly at 240 DEG C, heats 20 hours that is to say, that hydrothermal temperature is 240 DEG C, step (2)
In, in argon, 400 DEG C are heated 3 hours, and remaining is all identical with embodiment one.
Observed using the composite that scanning electron microscope is prepared to this example, result shows, the agraphitic carbon cladding of this example
Stannic disulphide nano slice a size of 2.5 microns, its nanometer sheet thickness is about 10 nanometers.Through measurement, the composite of this example
In, agraphitic carbon content accounts for the 13.9% of the stannic disulphide nano slice composite gross weight of agraphitic carbon cladding.
This example prepares negative material using embodiment one identical method, equally tests its electrochemistry using button cell
Can, the preparation method of button cell is all identical with embodiment one with method of testing.Test result shows, when with the electricity of 100mA/g
During current charge electric discharge, charge specific capacity can reach 906mAh/g within the 1st week, and after 140 times circulations, discharge capacity is 1034mAh/g.
Embodiment seven
This example prepares stannic disulphide nano slice composite using with embodiment one identical condition and method, different
It is that, in step (1), baking oven, directly at 150 DEG C, heats 20 hours that is to say, that hydrothermal temperature is 150 DEG C, step (2)
In, in argon, 1000 DEG C are heated 3 hours, and remaining is all identical with embodiment one.
Observed using the composite that scanning electron microscope is prepared to this example, result shows, the agraphitic carbon cladding of this example
Stannic disulphide nano slice a size of 5 microns, its nanometer sheet thickness is about 10 nanometers.Through measurement, in the composite of this example,
Agraphitic carbon content accounts for the 12.3% of the stannic disulphide nano slice composite gross weight of agraphitic carbon cladding.
This example prepares negative material using embodiment one identical method, equally tests its electrochemistry using button cell
Can, the preparation method of button cell is all identical with embodiment one with method of testing.Test result shows, when with the electricity of 100mA/g
During current charge electric discharge, charge specific capacity can reach 1223mAh/g within the 1st week, and after 140 circulations, discharge capacity is 1162mAh/g.
Visible according to above example, the flower-shaped stannic disulphide nano slice composite of the agraphitic carbon cladding of the application,
As lithium ion battery negative material use with good cycling stability, rate capability high the features such as.Base in above example
On plinth, the application is also tested to the atmosphere of Oleic acid annealing, it was found that in addition to can be using argon, other lazy
Property gas, such as nitrogen can be used for the application.In addition, in inert atmosphere calcining be in order that Oleic acid carbonization formed amorphous
Carbon, at 400-1000 DEG C, heat time heating time, 1-8 hour can obtain two sulfur that agraphitic carbon content accounts for agraphitic carbon cladding to its temperature
Change the composite of the 5%-15% of stannum nanosheet composite material gross weight, and, the amorphous carbon of the lower conversion of temperature is more.
Above content is further description the application made with reference to specific embodiment it is impossible to assert this Shen
Being embodied as please is confined to these explanations.For the application person of an ordinary skill in the technical field, do not taking off
On the premise of the application design, some simple deduction or replace can also be made, all should be considered as belonging to the protection of the application
Scope.
Claims (10)
1. a kind of preparation method of stannic disulphide nano slice composite it is characterised in that：Described preparation method includes following step
Suddenly,
(1) stannum source solution and L-Cysteine solution are mixed as reactant liquor, reacting by heating 5-30 hour, react after terminating certainly
So cool down, replaced with water and ethanol and wash, obtain flower-shaped stannic disulphide nano slice；
(2) stannic disulfide preparing step (1) and Oleic acid are according to weight 1:20-1:60 mixing, make stannic disulfide be completely soaked
In Oleic acid, soak 24-48 hour, centrifugation removes unnecessary Oleic acid, at 400-1000 DEG C, in inert gas atmosphere, heat 1-
8 hours, obtain the stannic disulphide nano slice composite of agraphitic carbon cladding.
2. preparation method according to claim 1 it is characterised in that：Described Xi Yuan is butter of tin, tin tetraiodide and four
At least one in Tin tetrabromide..
3. preparation method according to claim 1 it is characterised in that：In described reactant liquor, Xi Yuan and L-Cysteine
Mol ratio is 1:4-1:8.
4. preparation method according to claim 1 it is characterised in that：In described reactant liquor, the concentration of stannum source solution is
0.02mol/L-0.1mol/L.
5. preparation method according to claim 1 it is characterised in that：In described step (1), reaction temperature is 150-240
℃.
6. the stannic disulphide nano slice composite of the preparation method preparation according to any one of claim 1-5, its feature
It is：The surface of stannic disulphide nano slice is in flower-shaped, and its Surface coating has amorphous carbon layer.
7. stannic disulphide nano slice composite according to claim 6 it is characterised in that：Described amorphous carbon layer accounts for always
The 5%-15% of weight.
8. the stannic disulphide nano slice composite according to claim 6 or 7 is in preparing lithium ion battery negative material
Application.
9. a kind of negative material for lithium ion battery it is characterised in that：Claim 6 or 7 is contained in described negative material
Described stannic disulphide nano slice composite.
10. the lithium ion battery of the negative material described in a kind of employing claim 9.
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| CN105118976B (en) * | 2015-07-29 | 2017-05-17 | 深圳新宙邦科技股份有限公司 | Mesoporous material of molybdenum dioxide cladded with carbon, preparation method thereof and application |
| CN107931600B (en) * | 2017-11-29 | 2019-08-09 | 广东聚航新材料研究院有限公司 | A kind of method of cysteine-modifying copper nano-particle |
| CN109956495B (en) * | 2017-12-25 | 2020-12-22 | 中国科学院物理研究所 | Vertical staggered petal-shaped tin disulfide nanosheet and preparation method thereof |
| CN108786849B (en) * | 2018-06-08 | 2021-08-17 | 西北师范大学 | Preparation and application of tin sulfide/titanium dioxide composite material |
| CN111268720B (en) * | 2020-01-13 | 2022-07-01 | 信阳师范学院 | Preparation method of large interlayer spacing tin disulfide nanoflower sodium ion battery negative electrode material |
| CN111584845B (en) * | 2020-05-20 | 2022-04-29 | 信阳师范学院 | Preparation method and application of N, S co-doped carbon/tin disulfide composite material |
| CN113851620B (en) * | 2021-08-30 | 2023-01-20 | 北京理工大学 | Potassium ion battery cathode composite material with multi-stage heterostructure and preparation method thereof |
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| CN101609885A (en) * | 2009-07-20 | 2009-12-23 | 北京理工大学 | A kind of raising lithium ion battery negative material SnS 2The method of chemical property |
| CN101609887A (en) * | 2009-07-16 | 2009-12-23 | 浙江大学 | A kind of lithium ion battery SnS 2The preparation method of nanometer sheet negative material |
| CN103531747A (en) * | 2013-10-17 | 2014-01-22 | 合肥工业大学 | Preparation method of carbon-coated tin dioxide superfine powder lithium ion battery negative electrode material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101609887A (en) * | 2009-07-16 | 2009-12-23 | 浙江大学 | A kind of lithium ion battery SnS 2The preparation method of nanometer sheet negative material |
| CN101609885A (en) * | 2009-07-20 | 2009-12-23 | 北京理工大学 | A kind of raising lithium ion battery negative material SnS 2The method of chemical property |
| CN103531747A (en) * | 2013-10-17 | 2014-01-22 | 合肥工业大学 | Preparation method of carbon-coated tin dioxide superfine powder lithium ion battery negative electrode material |
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Effective date of registration: 20191211 Address after: Taihu County, Anhui city of Anqing Province Jin Xi Zhen 246400 Patentee after: Taihu County market supervision and Inspection Institute (Taihu County functional membrane Testing Institute) Address before: 518118 Guangdong province Shenzhen City Pingshan sand Tang with rich industrial area Patentee before: Shenzhen Xinyubang Science and Technology Co., Ltd. |