CN104716311A - Tin bisulfide nanosheet composite material, as well as preparation method and application thereof - Google Patents
Tin bisulfide nanosheet composite material, as well as preparation method and application thereof Download PDFInfo
- Publication number
- CN104716311A CN104716311A CN201510073828.4A CN201510073828A CN104716311A CN 104716311 A CN104716311 A CN 104716311A CN 201510073828 A CN201510073828 A CN 201510073828A CN 104716311 A CN104716311 A CN 104716311A
- Authority
- CN
- China
- Prior art keywords
- composite material
- tin
- stannic
- preparation
- disulphide nano
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Composite Materials (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a tin bisulfide nanosheet composite material, as well as a preparation method and application thereof. The preparation method comprises the following steps: (1) uniformly mixing a tin source and an L-cysteine solution, performing heating reaction for 5 to 30 hours, naturally cooling the reaction product, and alternately washing the reaction product with water and ethanol to obtain a flower-like tin bisulfide nanosheet; (2) mixing tin bisulfide and oleic acid according to the weight ratio of (1 to 20) to (1 to 60), performing soaking for 24 to 48 hours, centrifugally removing redundant oleic acid, and performing heating for 1 to 8 hours in the inert gas atmosphere of 400 to 1,000 DEG C to obtain an amorphous carbon-coated tin bisulfide nanosheet composite material. According to the method, amorphous carbon is formed by oleic acid adsorption material surface annealing, and the surface of the flower-like tin bisulfide nanosheet prepared by a hydrothermal method is coated with an amorphous carbon layer, so that the method is simple and easy to operate; the prepared amorphous carbon-coated tin bisulfide nanosheet composite material is large in surface area and thin, and has the characteristics of high cycling stability, high rate capacity and the like when being used as a battery cathode.
Description
Technical field
The application relates to lithium ion battery negative material field, particularly relates to a kind of stannic disulphide nano slice composite material and its preparation method and application.
Background technology
Along with fossil energy is exhausted and the pressure of ecological deterioration trend, Development of EV and hybrid-electric car imperative.At present, the power supply as one of the core technology of electric automobile is the bottleneck advancing Development of Electric Vehicles fast.Lithium ion battery, compared with other secondary power supplies, has the advantages such as energy density is high, power density large, environmental protection, is considered to one of the most promising power supply.But its capacity is low is 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 comprises: silica-based, tinbase, various material with carbon element.Material with carbon element capacity is low, silica-based capacity high but in charge and discharge process change in volume very big, cause capacity attenuation fast; Be compared to other negative material, tin-based material is between wherein.Stannic disulfide has layer structure, has higher lithium storage content and structural stability.But stannic disulfide has lower conductivity, restrict its charge/discharge capacity under high current density.
Summary of the invention
The object of the application is to provide flower-shaped stannic disulphide nano slice composite material of a kind of micro-structural improvement and its preparation method and application.
To achieve these goals, the application have employed following technical scheme:
The one side of the application discloses a kind of preparation method of stannic disulphide nano slice composite material, comprise the following steps, (1) tin source solution and Cys solution are mixed as reactant liquor, add thermal response 5-30 hour, reaction terminates rear cooling naturally, with water and ethanol alternately washing, obtain flower-shaped stannic disulphide nano slice; (2) stannic disulfide prepared by step (1) is mixed according to weight 1:20-1:60 with oleic acid, stannic disulfide is made to be fully immersed in oleic acid, soak 24-48 hour, the oleic acid that centrifugal segregation is unnecessary, at 400-1000 DEG C, heat 1-8 hour in inert gas atmosphere, obtain the stannic disulphide nano slice composite material that agraphitic carbon is coated.
It should be noted that, the key of the application is the hydro thermal method preparing stannic disulphide nano slice and oleic acid to anneal and forms amorphous carbon and combine, the creationary Surface coating at stannic disulphide nano slice is one deck amorphous carbon at least, compared with independent stannic disulfide, the composite material of the application, not only further increase specific capacity, and improve cycle life.In the implementation of the application, stannic disulfide and oleic acid adopt ultrasonic mixing, to reach well-mixed object.
Also it should be noted that, the concrete operations mode that water and ethanol alternately wash produces the mode of washing in stannic disulphide nano slice with reference to conventional hydro thermal method, be not specifically limited at this; In addition, the key of the application forms the coated stannic disulphide nano slice composite material of agraphitic carbon, in follow-up application, such as prepare negative material time, its following process is determined according to concrete working condition or production object, is not specifically limited at this.
Preferably, Xi Yuan is at least one in butter of tin, tin tetraiodide and tin tetrabromide.It should be noted that, in a kind of implementation of the application, preferably adopt butter of tin.
Preferably, in reactant liquor, the mol ratio of Xi Yuan and Cys is 1:4-1:8.It should be noted that, the amount ratio of Xi Yuan and Cys, be as the criterion to generate stannic disulfide to greatest extent, that is, be as the criterion with the chemical dosage ratio that it participates in reaction, in conjunction with concrete working condition and the object of the application, the application is preferred, adopts the mol ratio of Xi Yuan and Cys to be that the amount of 1:4-1:8 is reacted; Further, preferred employing butter of tin is Xi Yuan.
Preferably, in reactant liquor, the concentration of Xi Yuan is 0.02mol/L-0.1mol/L.It should be noted that, the restriction of tin source concentration, is actually the restriction of reaction solution concentration, be appreciated that Xi Yuan and Cys need both fully to mix when reacting, concentration is too low, output is also low, affects production efficiency, and concentration is too high, is unfavorable for that reaction is carried out; Therefore, the application preferably adopts the concentration of Xi Yuan to be that 0.02mol/L-0.1mol/L reacts.
Preferably, in step (1), reaction temperature is 150-240 DEG C.It should be noted that, reaction temperature refers to the temperature of Xi Yuan and Cys hydro-thermal reaction, and the application preferably adopts 150-240 DEG C, that is, at 150-240 DEG C, reacts 5-30 hour.
Stannic disulphide nano slice composite material prepared by the preparation method that the another side of the application also discloses the application, the surface of its stannic disulphide nano slice is flower-shaped, and its Surface coating has amorphous carbon layer.
Preferably, in the stannic disulphide nano slice composite material of the application, amorphous carbon layer accounts for the 5%-15% of total weight.It should be noted that, the Main Function of amorphous carbon plays conductivity, to make up the defect of stannic disulfide conduction rate variance, therefore, as long as can be complete by stannic disulfide parcel wherein; In the application, consider the composite factor such as specific capacity and conductivity, preferably, make the amorphous carbon of coated stannic disulfide account for the 5%-15% of total weight.
In addition, the application uses Shortcomings for existing stannic disulfide as lithium ion battery negative material and studies, therefore, the application in lithium ion battery negative material prepared by the stannic disulphide nano slice composite material that the application further provides the application.It should be noted that, in a kind of implementation of the application, stannic disulphide nano slice composite material the application prepared and conventional conductive agent, together with binding agent, are prepared into negative material for lithium ion battery.Wherein, conductive agent is preferably acetylene black, the preferred sodium cellulose glycolate of binding agent (abbreviation CMC).
Therefore, the one side again of the application discloses a kind of negative material for lithium ion battery, the stannic disulphide nano slice composite material containing the application in this negative material.
Further, in a kind of implementation of the application, the negative material of the stannic disulphide nano slice composite material containing the application is made lithium ion battery; Therefore, the one side again of the application discloses a kind of lithium ion battery made by negative material of the stannic disulphide nano slice composite material containing the application.
Owing to adopting above technical scheme, the beneficial effect of the application is:
The preparation method of the application utilizes oleic acid to adsorb crystal face annealing and forms agraphitic carbon, and at flower-shaped stannic disulphide nano slice Surface coating amorphous carbon layer prepared by hydro thermal method, preparation method is simple, easy to operate.Further, the stannic disulphide nano slice composite material that the agraphitic carbon prepared by the preparation method of the application is coated, surface area is large, sheet is thin, uses have good cycling stability, rate capability high as battery cathode.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the stannic disulphide nano slice composite material that in the embodiment of the present application, agraphitic carbon is coated;
Fig. 2 is the transmission electron microscope picture of the stannic disulphide nano slice composite material that in the embodiment of the present application, agraphitic carbon is coated;
Fig. 3 adopts the stannic disulphide nano slice composite material of the application as the capacity curve of the charged/discharged first figure of the button cell of negative material in the embodiment of the present application;
Fig. 4 adopts the stannic disulphide nano slice composite material of the application as the charging cycle performance chart of the button cell of negative material in the embodiment of the present application;
Fig. 5 adopts the stannic disulphide nano slice composite material of the application as the multiplying power charging performance curve chart of the button cell of negative material in the embodiment of the present application.
Embodiment
Amorphous carbon is as a kind of special defect grapheme material, be rarely used in composite material, the creationary feature utilizing oleic acid annealing to form amorphous carbon of the application, mixes oleic acid with stannic disulfide in advance, anneal again, form the stannic disulphide nano slice composite material that amorphous carbon is coated.Composite material prepared by the application has good specific capacity good cycling stability, rate capability high.
It should be noted that, flower-shaped stannic disulphide nano slice prepared by the application, its surface is in flower-like structure; As shown in Figure 1, whole stannic disulfide is flaky nanometer structure, and the stannic disulphide nano slice of flower-shaped surface texture is absorption oleic acid, forms amorphous carbon coating layer and provides convenience.
Below by specific embodiments and the drawings, the application is described in further detail.Following examples are only further described the application, 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) the butter of tin aqueous solution of 20ml 0.04mol/L and the Cys of 20ml 0.16mol/L are mixed make reactant liquor respectively, reactant liquor is transferred in the polytetrafluoro container of 50 milliliters, and polytetrafluoro container is fixed in stainless reactor, then with baking oven directly at 200 DEG C, heat 20 hours, when the temperature of question response still is reduced to room temperature naturally, obtained reactant is washed 3 times successively with water and ethanol respectively, by the sample after washing in 50 DEG C of baking ovens dry 12 hours, obtain surface in flower-shaped stannic disulphide nano slice; Wherein, in reactant liquor, the concentration of butter of tin is 0.02mol/L.
(2) then stannic disulfide prepared by step (1) is mixed ultrasonic 1 hour with oleic acid according to weight ratio 1:40, soak 24 hours, centrifugally remove unnecessary oleic acid, the flower-shaped stannic disulphide nano slice composite material that the agraphitic carbon that namely the 800 DEG C of heating in argon gas of its mixture are obtained this example for 3 hours is coated.
Through measuring, in the composite material of this example, agraphitic carbon content accounts for 13.9% of the coated stannic disulphide nano slice composite material total weight of agraphitic carbon.
ESEM and transmission electron microscope is adopted to observe composite material prepared by this example, result as depicted in figs. 1 and 2, Fig. 1 is the scanning electron microscope (SEM) photograph of the coated flower-shaped stannic disulphide nano slice of agraphitic carbon of this example preparation, as shown in Figure 1, the coated stannic disulphide nano slice size of agraphitic carbon of this example is about 2 microns, and its thickness is about 10 nanometers.Fig. 2 is the transmission electron microscope picture of the coated flower-shaped stannic disulphide nano slice of agraphitic carbon of this example preparation, and as shown in Figure 2, the thickness of the coating layer of the coated stannic disulfide of agraphitic carbon of this example is about 3.5nm.
The coated flower-shaped stannic disulphide nano slice composite material of agraphitic carbon prepared by this example is made lithium ion battery negative material, and adopts button cell to test its chemical property.In the lithium ion battery negative material of this example, conductive agent adopts acetylene black, and binding agent adopts CMC, and stannic disulphide nano slice composite material: acetylene black: CMC mixes according to the ratio of weight ratio 80wt.%: 10wt.%: 10wt.%, coats on Copper Foil.In button cell, electrolyte adopts the LiPF of 1mol/L
6/ EC-DEC-DMC (1: 1: 1, w/w).Carry out charged/discharged with 100mA/g respectively, potential range is 0.01 ~ 2.5V.After tested, when discharging with the current charges of 100mA/g, within the 1st week, charge specific capacity can reach 1580mAh/g, and after 140 circulations, discharge capacity is 990mAh/g.Charging and discharging curve, cycle characteristics curve and multiplying power property curve that the difference that Fig. 3, Fig. 4, Fig. 5 are respectively the coated flower-shaped stannic disulfide sheet composite material of agraphitic carbon circulates.
Embodiment two
This example mixes with the Cys of the 0.8mol/L of the butter of tin aqueous solution of the 0.2mol/L of 20ml and 20ml prepares stannic disulfide, and baking oven is directly at 240 DEG C, heat 20 hours, that is, hydrothermal temperature is 240 DEG C, and in step (2), stannic disulfide mixes ultrasonic 1 hour with oleic acid according to weight ratio 1:60, soak 48 hours, centrifugally remove unnecessary oleic acid.All the other steps and condition are all identical with embodiment one.
Adopt ESEM to observe composite material prepared by this example, result shows, and the coated stannic disulphide nano slice of agraphitic carbon of this example is of a size of 3 microns, and its nanometer sheet thickness is about 10 nanometers.Through measuring, in the composite material of this example, agraphitic carbon content accounts for 13.7% of the coated stannic disulphide nano slice composite material total weight of agraphitic carbon.
This example adopts the identical method of embodiment one to prepare negative material, and its chemical property tested by the same button cell that adopts, and the preparation method of button cell is all identical with embodiment one with method of testing.Test result shows, and when discharging with the current charges of 100mA/g, within the 1st week, charge specific capacity can reach 1220mAh/g, and after 140 circulations, discharge capacity is 971mAh/g.
Embodiment three
This example mixes with the Cys of the 0.4mol/L of the butter of tin aqueous solution of the 0.1mol/L of 20ml and 20ml prepares stannic disulfide, and baking oven is directly at 180 DEG C, heat 20 hours, that is, hydrothermal temperature is 180 DEG C, and in step (2), stannic disulfide mixes ultrasonic 1 hour with oleic acid according to weight ratio 1:50, soak 36 hours, centrifugally remove unnecessary oleic acid.All the other steps and condition are all identical with embodiment one.
Adopt ESEM to observe composite material prepared by this example, result shows, and the coated stannic disulphide nano slice of agraphitic carbon of this example is of a size of 3.5 microns, and its nanometer sheet thickness is about 10 nanometers.Through measuring, in the composite material of this example, agraphitic carbon content accounts for 14% of the coated stannic disulphide nano slice composite material total weight of agraphitic carbon.
This example adopts the identical method of embodiment one to prepare negative material, and its chemical property tested by the same button cell that adopts, and the preparation method of button cell is all identical with embodiment one with method of testing.Test result shows, and when discharging with the current charges of 100mA/g, within the 1st week, specific discharge capacity can reach 1250mAh/g, and 140 discharge capacities are 950mAh/g.
Embodiment four
This example adopts the condition identical with embodiment one and method to prepare stannic disulphide nano slice composite material, uniquely unlike, in step (2), in argon gas, 1000 DEG C are heated 3 hours, and all the other are all identical with embodiment one.
Adopt ESEM to observe composite material prepared by this example, result shows, and the coated stannic disulphide nano slice of agraphitic carbon of this example is of a size of 2.5 microns, and its nanometer sheet thickness is about 10 nanometers.Through measuring, in the composite material of this example, agraphitic carbon content accounts for 14.1% of the coated stannic disulphide nano slice composite material total weight of agraphitic carbon.
This example adopts the identical method of embodiment one to prepare negative material, and its chemical property tested by the same button cell that adopts, and the preparation method of button cell is all identical with embodiment one with method of testing.Test result shows, and when discharging with the current charges of 100mA/g, within the 1st week, charge specific capacity can reach 1322mAh/g, and after 140 circulations, discharge capacity is 1020mAh/g.
Embodiment five
This example mixes with the Cys of the 0.32mol/L of the butter of tin aqueous solution of the 0.04mol/L of 20ml and 20ml prepares stannic disulfide, and baking oven is directly at 240 DEG C, heat 20 hours, that is, hydrothermal temperature is 240 DEG C, in step (2), in argon gas, 400 DEG C are heated 3 hours, and all the other steps and condition are all identical with embodiment one.
Adopt ESEM to observe composite material prepared by this example, result shows, and the coated stannic disulphide nano slice of agraphitic carbon of this example is of a size of 4 microns, and its nanometer sheet thickness is about 10 nanometers.Through measuring, in the composite material of this example, agraphitic carbon content accounts for 15.2% of the coated stannic disulphide nano slice composite material total weight of agraphitic carbon.
This example adopts the identical method of embodiment one to prepare negative material, and its chemical property tested by the same button cell that adopts, and the preparation method of button cell is all identical with embodiment one with method of testing.Test result shows, and when discharging with the current charges of 100mA/g, within the 1st week, charge specific capacity can reach 1158mAh/g, and after 140 circulations, discharge capacity is 1911mAh/g.
Embodiment six
This example adopts the condition identical with embodiment one and method to prepare stannic disulphide nano slice composite material, difference is, in step (1), baking oven, directly at 240 DEG C, heats 20 hours, that is, hydrothermal temperature is 240 DEG C, in step (2), in argon gas, 400 DEG C are heated 3 hours, and all the other are all identical with embodiment one.
Adopt ESEM to observe composite material prepared by this example, result shows, and the coated stannic disulphide nano slice of agraphitic carbon of this example is of a size of 2.5 microns, and its nanometer sheet thickness is about 10 nanometers.Through measuring, in the composite material of this example, agraphitic carbon content accounts for 13.9% of the coated stannic disulphide nano slice composite material total weight of agraphitic carbon.
This example adopts the identical method of embodiment one to prepare negative material, and its chemical property tested by the same button cell that adopts, and the preparation method of button cell is all identical with embodiment one with method of testing.Test result shows, and when discharging with the current charges of 100mA/g, within the 1st week, charge specific capacity can reach 906mAh/g, and after 140 times circulations, discharge capacity is 1034mAh/g.
Embodiment seven
This example adopts the condition identical with embodiment one and method to prepare stannic disulphide nano slice composite material, difference is, in step (1), baking oven, directly at 150 DEG C, heats 20 hours, that is, hydrothermal temperature is 150 DEG C, in step (2), in argon gas, 1000 DEG C are heated 3 hours, and all the other are all identical with embodiment one.
Adopt ESEM to observe composite material prepared by this example, result shows, and the coated stannic disulphide nano slice of agraphitic carbon of this example is of a size of 5 microns, and its nanometer sheet thickness is about 10 nanometers.Through measuring, in the composite material of this example, agraphitic carbon content accounts for 12.3% of the coated stannic disulphide nano slice composite material total weight of agraphitic carbon.
This example adopts the identical method of embodiment one to prepare negative material, and its chemical property tested by the same button cell that adopts, and the preparation method of button cell is all identical with embodiment one with method of testing.Test result shows, and when discharging with the current charges of 100mA/g, within the 1st week, charge specific capacity can reach 1223mAh/g, and after 140 circulations, discharge capacity is 1162mAh/g.
Visible according to above embodiment, the flower-shaped stannic disulphide nano slice composite material that the agraphitic carbon of the application is coated, uses as lithium ion battery negative material and has good cycling stability, rate capability high.On the basis of above embodiment, the application also tests the atmosphere of oleic acid annealing, and found that, except adopting except argon gas, other inert gas, such as nitrogen also may be used for the application.In addition, in inert atmosphere, calcining is to make oleic acid carbonization form amorphous carbon, its temperature is at 400-1000 DEG C, the composite material that agraphitic carbon content accounts for the 5%-15% of the coated stannic disulphide nano slice composite material total weight of agraphitic carbon can be obtained 1-8 hour heating time, further, the amorphous carbon of the lower conversion of temperature is more.
Above content is the further description done the application in conjunction with concrete execution mode, can not assert that the concrete enforcement of the application is confined to these explanations.For the application person of an ordinary skill in the technical field, under the prerequisite not departing from the application's design, some simple deduction or replace can also be made, all should be considered as the protection range belonging to the application.
Claims (10)
1. a preparation method for stannic disulphide nano slice composite material, is characterized in that: described preparation method comprises the following steps,
(1) mix tin source solution and Cys solution as reactant liquor, add thermal response 5-30 hour, reaction terminates rear cooling naturally, with water and ethanol alternately washing, obtains flower-shaped stannic disulphide nano slice;
(2) stannic disulfide prepared by step (1) is mixed according to weight 1:20-1:60 with oleic acid, stannic disulfide is made to be fully immersed in oleic acid, soak 24-48 hour, the oleic acid that centrifugal segregation is unnecessary, at 400-1000 DEG C, heat 1-8 hour in inert gas atmosphere, obtain the stannic disulphide nano slice composite material that agraphitic carbon is coated.
2. preparation method according to claim 1, is characterized in that: described Xi Yuan is at least one in butter of tin, tin tetraiodide and tin tetrabromide.
3. preparation method according to claim 1, is characterized in that: in described reactant liquor, and the mol ratio of Xi Yuan and Cys is 1:4-1:8.
4. preparation method according to claim 1, is characterized in that: in described reactant liquor, and the concentration of tin source solution is 0.02mol/L-0.1mol/L.
5. preparation method according to claim 1, is characterized in that: in described step (1), and reaction temperature is 150-240 DEG C.
6. stannic disulphide nano slice composite material prepared by the preparation method according to any one of claim 1-5, is characterized in that: the surface of stannic disulphide nano slice is flower-shaped, and its Surface coating has amorphous carbon layer.
7. stannic disulphide nano slice composite material according to claim 6, is characterized in that: described amorphous carbon layer accounts for the 5%-15% of total weight.
8. the application in lithium ion battery negative material prepared by the stannic disulphide nano slice composite material according to claim 6 or 7.
9. for a negative material for lithium ion battery, it is characterized in that: containing the stannic disulphide nano slice composite material described in claim 6 or 7 in described negative material.
10. one kind adopts the lithium ion battery of negative material according to claim 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510073828.4A CN104716311B (en) | 2015-02-11 | 2015-02-11 | A kind of stannic disulphide nano slice composite and its preparation method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510073828.4A CN104716311B (en) | 2015-02-11 | 2015-02-11 | A kind of stannic disulphide nano slice composite and its preparation method and application |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104716311A true CN104716311A (en) | 2015-06-17 |
| CN104716311B CN104716311B (en) | 2017-03-01 |
Family
ID=53415432
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510073828.4A Active CN104716311B (en) | 2015-02-11 | 2015-02-11 | A kind of stannic disulphide nano slice composite and its preparation method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104716311B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105118976A (en) * | 2015-07-29 | 2015-12-02 | 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 |
| CN107931600A (en) * | 2017-11-29 | 2018-04-20 | 广东聚航新材料研究院有限公司 | A kind of method of cysteine-modifying copper nano-particle |
| CN108786849A (en) * | 2018-06-08 | 2018-11-13 | 西北师范大学 | A kind of preparation and application of artificial gold/composite titania material |
| CN109956495A (en) * | 2017-12-25 | 2019-07-02 | 中国科学院物理研究所 | Upright alternating expression petal-shaped stannic disulphide nano slice and preparation method thereof |
| CN111268720A (en) * | 2020-01-13 | 2020-06-12 | 信阳师范学院 | Preparation method of large interlayer spacing tin disulfide nanoflower sodium ion battery negative electrode material |
| CN111584845A (en) * | 2020-05-20 | 2020-08-25 | 信阳师范学院 | Preparation method and application of N, S co-doped carbon/tin disulfide composite material |
| CN113851620A (en) * | 2021-08-30 | 2021-12-28 | 北京理工大学 | Potassium ion battery cathode composite material with multi-stage heterostructure and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2015
- 2015-02-11 CN CN201510073828.4A patent/CN104716311B/en active Active
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 |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105118976A (en) * | 2015-07-29 | 2015-12-02 | 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 |
| 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 |
| CN107931600A (en) * | 2017-11-29 | 2018-04-20 | 广东聚航新材料研究院有限公司 | A kind of method of cysteine-modifying copper nano-particle |
| 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 |
| CN109956495A (en) * | 2017-12-25 | 2019-07-02 | 中国科学院物理研究所 | Upright alternating expression petal-shaped stannic disulphide nano slice and preparation method thereof |
| CN108786849A (en) * | 2018-06-08 | 2018-11-13 | 西北师范大学 | A kind of preparation and application of artificial gold/composite titania material |
| CN111268720A (en) * | 2020-01-13 | 2020-06-12 | 信阳师范学院 | Preparation method of large interlayer spacing tin disulfide nanoflower sodium ion battery negative electrode 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 |
| CN111584845A (en) * | 2020-05-20 | 2020-08-25 | 信阳师范学院 | Preparation method and application of N, S co-doped carbon/tin disulfide composite 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 |
| CN113851620A (en) * | 2021-08-30 | 2021-12-28 | 北京理工大学 | Potassium ion battery cathode composite material with multi-stage heterostructure and preparation method thereof |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104716311B (en) | 2017-03-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106935860B (en) | A kind of carbon intercalation V2O3Nano material, preparation method and application | |
| CN104681815B (en) | Spherical molybdenum disulfide composite material and preparation method and application thereof | |
| CN104716311B (en) | A kind of stannic disulphide nano slice composite and its preparation method and application | |
| CN106450265B (en) | A kind of situ Nitrogen Doping carbon coating lithium titanate combination electrode material and preparation method thereof | |
| CN104124431B (en) | A kind of lithium ion battery graphite cathode material and preparation method thereof | |
| CN102569769B (en) | Preparation method for lithium titanate and graphene composite electrode materials | |
| CN103682296B (en) | A kind of preparation method of nanoscale lithium titanate material with high specific capacity | |
| CN103682327B (en) | Based on the lithium ion battery and preparation method thereof of the hollow porous nickel oxide composite material of N doping carbon-coating parcel | |
| CN105938899A (en) | Preparation method and application of cathode material of fast ion conductor coated modified lithium ion battery | |
| CN107293710A (en) | The preparation method of transition metal oxide/graphene composite material, negative electrode of lithium ion battery, lithium ion battery | |
| CN108899530B (en) | Silicon-carbon composite material and preparation method and application thereof | |
| CN108878826B (en) | Sodium manganate/graphene composite electrode material and preparation method and application thereof | |
| CN107681147A (en) | A kind of preparation method of solid electrolyte coating modification anode material for lithium-ion batteries and application | |
| CN105789615A (en) | Modified lithium nickel cobalt manganese cathode material and preparation method thereof | |
| CN106410153A (en) | Titanium nitride-cladded nickel titanate composite material as well as preparation method and application thereof | |
| CN103078095A (en) | Method for preparing tin dioxide/graphene-compounded anode material of lithium ion battery | |
| CN105810456A (en) | Activated graphene/needle-shaped nickel hydroxide nanocomposite material and preparation method thereof | |
| CN104852015A (en) | Niobium pentoxide nanosheet composite material, preparation method and application thereof | |
| CN101894943A (en) | Method for coating lithium ion battery anode material with carbon | |
| CN104638248B (en) | A kind of preparation method of graphene/lead compound composite | |
| CN114057488B (en) | Preparation method of porous SiOC ceramic and application of porous SiOC ceramic in negative electrode material of lithium ion battery | |
| CN114975964A (en) | Polypyrrole-coated tin dioxide/nano carbon sphere negative electrode material, preparation method thereof and sodium ion battery | |
| CN103682278B (en) | The preparation method of the coated lithium titanate anode material of a kind of nanometer carbon | |
| CN109360961B (en) | Hollow composite microsphere for lithium-sulfur battery positive electrode material and preparation method thereof | |
| CN105428613B (en) | A kind of preparation method and lead-acid battery of lead-acid battery |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
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. |