CN107032390A - A kind of cube shaped frame SnS2The preparation method of anode material of lithium-ion battery - Google Patents
A kind of cube shaped frame SnS2The preparation method of anode material of lithium-ion battery Download PDFInfo
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- CN107032390A CN107032390A CN201610946170.8A CN201610946170A CN107032390A CN 107032390 A CN107032390 A CN 107032390A CN 201610946170 A CN201610946170 A CN 201610946170A CN 107032390 A CN107032390 A CN 107032390A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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 invention discloses a kind of cube shaped frame SnS2The preparation method of anode material of lithium-ion battery, 1) sodium thiosulfate is dissolved in deionized water, solution A is configured to, five water stannic chlorides are dissolved in aliquots of deionized water and are configured to solution B；2) solution B is added dropwise in solution A and obtains solution C, hexadecyltrimethylammonium chloride is added gradually in solution C to form solution D；3) solution D is put into sonic oscillation in supersonic generator；4) the pH formation solution Es of the mixed solution D after regulation is handled through ultrasonic vibration；5) solution E is subjected to hydro-thermal reaction；6) after question response terminates, presoma is taken out, centrifuge washing is distinguished through deionized water and absolute ethyl alcohol, then freeze-drying obtains cube shaped frame SnS2Anode material of lithium-ion battery.Present invention preparation cost is low, simple to operate, short preparation period, the cube shaped frame SnS of preparation2Anode material of lithium-ion battery has excellent charge-discharge magnification performance.
Description
Technical field
The present invention relates to a kind of preparation method of anode material of lithium-ion battery, and in particular to a kind of cube shaped frame SnS2
The preparation method of anode material of lithium-ion battery.
Background technology
As scarcity of resources, energy crisis and pollution pressure are increasingly sharpened, find a kind of efficient clean energy resource into
For the focus of various countries, and using and develop secondary rechargeable battery is most effective so far, can most solve the energy and environment danger
A kind of necessary mode of machine, wherein, sodium-ion battery is a kind of electrochemical energy storage power supply, with raw material resources are abundant, price is low
Honest and clean, specific energy is high, the advantages of have a safety feature.Compared to lithium ion battery, various excellent properties of sodium-ion battery and relatively steady
Fixed chemical property so that it is expected to replace lithium ion battery in energy storage field, will possess the city bigger than lithium ion battery
Field competitive advantage.Meanwhile, attention of the people to sodium-ion battery progress in recent years, not only widened positive and negative electrode material with
And the field of electrolyte, also achieve greater advance on the chemical property of experiment preparation method and battery.But sodium ion
Ionic radius (r=0.113nm) is about bigger by more than 30% than the ionic radius (r=0.076nm) of lithium ion, it is difficult to realize reversible
The embedding dealkylation reaction of electrochemistry, insertion-abjection process easily causes collapsing for host lattice structure, causes cycle performance, the multiplying power of material
Performance and electrochemical utilization rate poor-performing, therefore, finding suitable embedding sode cell material has certain difficulty.
SnS2It is to belong to IV:The binary compound of VI main groups, by hexagonal phase elementary cell CdI2Layered crystal structure (structure cell
Parameter：A=0.3648nm, c=0.5899nm) constitute, this construction unit adds in the middle of the sulphion of two layers of hexagonal closs packing
Enter sandwich structure (S-Sn-S) composition of tin ion.Every six sulphions insert a tin ion formation regular octahedron and matched somebody with somebody
Position, and there is weak Van der Waals force between layers and by Covalent bonding together.In addition, there are many crystalline substances in this layer structure
Body room, can as intercalation host lattice.This unique layer structure makes it have excellent photoelectric characteristic.At present, grind
The persons of studying carefully prepare different structure or the SnS of size by different methods2, main structure have stannic disulfide nano-particle,
The zero dimensions such as nanosphere, nanometer sheet, nanotube, nano-plates, one-dimensional and two-dimentional or 3-D nano, structure, or even also have more multiple
Miscellaneous multistage micro nano structure.Special performance that people possess using these different structures prepares semi-conducting material, light
Catalysis material, solar cell material, photo-translating system material and lithium ion battery material etc..Unique performance and extensively
Application cause SnS2Material, which turns into, most one of material of application prospect.
Composition, pattern, size due to material etc. be able to can affect to the chemical property of sample.Two dimension,
Three-dimensional and multidimensional or porous structure and morphology are conducive to the deintercalation of lithium ion, then the capacity of material can become big.And particle is got over
Small, specific surface area is bigger, then contact of the material with electrolyte is better, Li+Migration distance can also shorten, be more beneficial for lithium ion
The lifting of cell negative electrode material high rate performance.In addition, these special structure meetings such as two dimension, three-dimensional and multistage micro nano structure
Its chemical property is set to obtain very big breakthrough.
At present, nanometer SnS2The preparation method of material mainly have solid reaction process [Zhang, Y.C, Du, Z.N, Li, S.Y,
Zhang,M.Novel synthesis and high visible light photocatalytic activity of
SnS2nanoflakes from Sncl2·2H2O and S powders.Appl.Catal.B 2010,95,153-159.],
Mechanics stripping method [Song H S, Li S L, Gao L, et al.High-performance top-gated monolayer
SnS2field-effect transistors and their integrated logic circuits[J]
.Nanoscale,2013,5(20):9666-9670.], solvent thermal reaction method [T.-J.Kim, C.Kim, D.Son, M.Choi,
B.Park.Novel SnS2-nanosheet anodes for lithium-ion batteries[J].Journal of
Power Sources.2007,167(2):529-535.].Wherein solid reaction process, which has, is not required to play solvent, equipment simple and anti-
The advantages of condition is easily controlled is answered, but is carried out due to reacting in solid phase, generally reaction is not thorough, and yield is relatively low.Mechanics is peeled off
Method is usually used in obtaining highly crystalline ultra-thin SnS2Nanometer sheet, but the nanometer sheet yield very little that this method is obtained, and controllability is non-
Constant, may be only available for the scientific research on basis.And solvent thermal reaction method is a kind of improved hydro-thermal reaction method, organic solvent is used
Solvent is made instead of traditional water, but course of reaction needs the condition of strict control solvent heat.
The content of the invention
It is an object of the invention to provide a kind of cube shaped frame SnS2The preparation method of anode material of lithium-ion battery, with
The defect for overcoming above-mentioned prior art to exist, present invention preparation cost is low, simple to operate, short preparation period, the cube of preparation
Structure SnS2Anode material of lithium-ion battery has excellent charge-discharge magnification performance.
To reach above-mentioned purpose, the present invention is adopted the following technical scheme that：
A kind of cube shaped frame SnS2The preparation method of anode material of lithium-ion battery, comprises the following steps：
1) sodium thiosulfate is dissolved in deionized water, is configured to solution A, compare n according to the amount of elemental substanceSn:nS=
1.0:Five water stannic chlorides are dissolved in aliquots of deionized water by (2.0~4.2) is configured to solution B；
2) solution B is added dropwise in solution A under magnetic agitation effect and obtains mixed solution C, then in magnetic agitation
N in molar ratio under effectFive water stannic chlorides:nHexadecyltrimethylammonium chloride=1：The ratio of (0.00062~0.01187) is by cetyl trimethyl
Ammonium chloride is added gradually to form well mixed solution D in mixed solution C；
3) mixed solution D is put into sonic oscillation in supersonic generator；
4) pH=4~7 that the mixed solution D after being handled through ultrasonic vibration is adjusted under magnetic agitation effect form solution E；
5) solution E is put into hydrothermal reaction kettle sealing, packing ratio is controlled 40%~60%, is put into homogeneous hydrothermal reactor
Reacted；
6) after question response terminates, presoma is taken out, centrifuge washing is distinguished through deionized water and absolute ethyl alcohol, is then freezed dry
It is dry to obtain cube shaped frame SnS2Anode material of lithium-ion battery.
Further, step 1) in solution A concentration be 0.2~1.0mol/L.
Further, step 3) in ultrasonic vibration processing time be 1~3h.
Further, step 4) the middle pH that the mixed solution D after being handled through ultrasonic vibration is adjusted using ammoniacal liquor.
Further, step 5) in reaction temperature control at 150~200 DEG C, the reaction time is controlled in 1~7h.
Further, step 6) in presoma distinguish centrifuge washing 3~5 times through deionized water and absolute ethyl alcohol.
Further, step 6) in freeze-drying temperature be -40~-60 DEG C, the time be 9~15h.
Compared with prior art, the present invention has following beneficial technique effect：
Prepared by the present invention have cube shaped frame SnS2Anode material of lithium-ion battery, first, ultrasonic wave are synthesized in solution
On play the role of uniqueness, the higher-order of oscillation signal that ultrasonic wave is sent is converted into high frequency machinery vibration by transducer and passed
It is multicast in reaction system, whole reaction uniformly can be quickly finished again.Ultrasonic assistant hydro-thermal method reaction rate is very fast, production
Thing crystallinity is strong, pattern is special, grain size distribution is uniform, and system is not in the phenomenon of reunion, and product also can be uniform
Spread out.Simultaneously in chemical reaction process, the energy that ultrasonic wave is sent can be as energy, reductionization needed for chemical reaction
Learn reaction energy.Cube shaped frame SnS prepared by the present invention2Anode material of lithium-ion battery size reach a few to tens of nanometers,
Crystallinity is strong, pattern is uniform, and being applied to negative electrode of lithium ion battery has excellent charge-discharge magnification performance.Experimental result table
It is bright, under 300mA/g current density, its first discharge capacity can reach 927mAh/g, after circulation 10 times, capacity is maintained at
397mAh/g, has compared with high circulation stability under high current density.
Further, by controlling response parameter, the stronger cube shaped frame of obtained crystallinity of the invention fills in battery
There is the charge-discharge performance under good stability, high current density to test the structure in discharge process to be not susceptible to collapse, and
Hole between cube shaped frame provides passage to ion so that migration rate and the ion populations increase of ion.
Brief description of the drawings
Fig. 1 is the cube shaped frame SnS prepared by the embodiment of the present invention 22The SEM figures of anode material of lithium-ion battery；
Fig. 2 is the cube shaped frame SnS prepared by the embodiment of the present invention 22The cycle performance of anode material of lithium-ion battery
Figure.
Embodiment
Embodiments of the present invention are described in further detail below：
A kind of cube shaped frame SnS2The preparation method of anode material of lithium-ion battery, comprises the following steps：
1) by sodium thiosulfate (Na2S2O2) be dissolved in deionized water, it is configured to the solution that concentration is 0.2~1.0mol/L
A, compares n according to the amount of elemental substanceSn:nS=1.0:(2.0~4.2) are by five water stannic chloride (SnCl4·5H2O) be dissolved in equivalent go from
Solution B is configured in sub- water (the deionized water equivalent i.e. with dissolving sodium thiosulfate)；
2) solution B is added dropwise in solution A under magnetic agitation effect and obtains mixed solution C, then in magnetic agitation
Effect is lower to press nFive water stannic chlorides:nHexadecyltrimethylammonium chloride=1：The ratio of (0.00062~0.01187) is by hexadecyltrimethylammonium chloride
(CTAC) it is added gradually in mixed solution C form well mixed solution D；
3) mixed solution D is put into 1~3h of sonic oscillation in supersonic generator.
4) ammoniacal liquor is added dropwise in the mixed solution D after being handled under magnetic agitation effect to ultrasonic vibration, solution is adjusted
PH=4~7 form solution E；
5) solution E is put into hydrothermal reaction kettle sealing, packing ratio is controlled 40%~60%, is put into homogeneous hydro-thermal reaction
Device, reaction temperature control is at 150~200 DEG C, and the reaction time is controlled in 1~7h；
6) after question response terminates, presoma is taken out, centrifuge washing is distinguished 3~5 times through deionized water and absolute ethyl alcohol, -40
~-60 DEG C of 9~15h of freeze-drying are to obtain SnS2Product.
The present invention is described in further detail with reference to embodiment：
Embodiment 1
1) by sodium thiosulfate (Na2S2O2) be dissolved in deionized water, the solution A that concentration is 0.2mol/L is configured to, according to
The amount of elemental substance compares nSn:nS=1.0:2.0 by five water stannic chloride (SnCl4·5H2O) it is dissolved in aliquots of deionized water and is configured to
Solution B；
2) solution B is added dropwise in solution A under magnetic agitation effect and obtains mixed solution C, then magnetic agitation is made
N is pressed with lowerFive water stannic chlorides:nHexadecyltrimethylammonium chloride=1：Hexadecyltrimethylammonium chloride (CTAC) is gradually added into by 0.00062 ratio
Well mixed solution D is formed into mixed solution C；
3) mixed solution D is put into sonic oscillation 1h in supersonic generator.
4) ammoniacal liquor is added dropwise into mixed solution D under magnetic agitation effect, regulation pH value of solution=4 form solution E；
5) E solution is put into hydrothermal reaction kettle sealing, packing ratio is controlled 40%, is put into homogeneous hydrothermal reactor, is reacted
Temperature control is at 200 DEG C, and the reaction time is controlled in 1h；
6) after question response terminates, presoma is taken out, centrifuge washing is distinguished 3 times through deionized water and absolute ethyl alcohol, -60 DEG C cold
It is to obtain SnS to freeze dry 9h2Product.
Embodiment 2
1) by sodium thiosulfate (Na2S2O2) be dissolved in deionized water, the solution A that concentration is 0.7mol/L is configured to, according to
The amount of elemental substance compares nSn:nS=1.0:3.0 by five water stannic chloride (SnCl4·5H2O) it is dissolved in aliquots of deionized water and is configured to
Solution B；
2) solution B is added dropwise in solution A under magnetic agitation effect and obtains mixed solution C, then magnetic agitation is made
N is pressed with lowerFive water stannic chlorides:nHexadecyltrimethylammonium chloride=1：Hexadecyltrimethylammonium chloride (CTAC) is gradually added into by 0.0086 ratio
Well mixed solution D is formed into mixed solution C；
3) mixed solution D is put into sonic oscillation 2h in supersonic generator.
4) ammoniacal liquor is added dropwise into mixed solution D under magnetic agitation effect, regulation pH value of solution=5 form solution E；
5) E solution is put into hydrothermal reaction kettle sealing, packing ratio is controlled 50%, is put into homogeneous hydrothermal reactor, is reacted
Temperature control is at 180 DEG C, and the reaction time is controlled in 5h；
6) after question response terminates, presoma is taken out, centrifuge washing is distinguished 4 times through deionized water and absolute ethyl alcohol, -50 DEG C cold
It is to obtain SnS to freeze dry 13h2Product.
As can be seen from Figure 1 sample prepared by the present embodiment has stronger crystallinity, as can be seen from Figure 2 this reality
Sample prepared by example is applied under 300mA/g current density, its first discharge capacity can reach 927mAh/g, after circulation 10 times,
Capacity is maintained at 397mAh/g, has under high current density compared with high circulation stability.
Embodiment 3
1) by sodium thiosulfate (Na2S2O2) be dissolved in deionized water, the solution A that concentration is 1.0mol/L is configured to, according to
The amount of elemental substance compares nSn:nS=1.0:4.2 by five water stannic chloride (SnCl4·5H2O) it is dissolved in aliquots of deionized water and is configured to
Solution B；
2) solution B is added dropwise in solution A under magnetic agitation effect and obtains mixed solution C, then magnetic agitation is made
N is pressed with lowerFive water stannic chlorides:nHexadecyltrimethylammonium chloride=1：Hexadecyltrimethylammonium chloride (CTAC) is gradually added into by 0.01187 ratio
Well mixed solution D is formed into mixed solution C；
3) mixed solution D is put into sonic oscillation 3h in supersonic generator.
4) ammoniacal liquor is added dropwise into mixed solution D under magnetic agitation effect, regulation pH value of solution=7 form solution E；
5) E solution is put into hydrothermal reaction kettle sealing, packing ratio is controlled 60%, is put into homogeneous hydrothermal reactor, is reacted
Temperature control is at 150 DEG C, and the reaction time is controlled in 7h；
6) after question response terminates, presoma is taken out, centrifuge washing is distinguished 5 times through deionized water and absolute ethyl alcohol, -40 DEG C cold
It is to obtain SnS to freeze dry 15h2Product.
Claims (7)
1. a kind of cube shaped frame SnS2The preparation method of anode material of lithium-ion battery, it is characterised in that comprise the following steps：
1) sodium thiosulfate is dissolved in deionized water, is configured to solution A, compare n according to the amount of elemental substanceSn:nS=1.0:
Five water stannic chlorides are dissolved in aliquots of deionized water by (2.0~4.2) is configured to solution B；
2) solution B is added dropwise in solution A under magnetic agitation effect and obtains mixed solution C, then acted in magnetic agitation
Under n in molar ratioFive water stannic chlorides:nHexadecyltrimethylammonium chloride=1：The ratio of (0.00062~0.01187) is by cetyl trimethyl chlorination
Ammonium is added gradually to form well mixed solution D in mixed solution C；
3) mixed solution D is put into sonic oscillation in supersonic generator；
4) pH=4~7 that the mixed solution D after being handled through ultrasonic vibration is adjusted under magnetic agitation effect form solution E；
5) solution E is put into hydrothermal reaction kettle sealing, packing ratio is controlled 40%~60%, is put into homogeneous hydrothermal reactor and carries out
Reaction；
6) after question response terminates, presoma is taken out, centrifuge washing is distinguished through deionized water and absolute ethyl alcohol, then freeze-drying is
Obtain cube shaped frame SnS2Anode material of lithium-ion battery.
2. a kind of cube shaped frame SnS according to claim 12The preparation method of anode material of lithium-ion battery, its feature
Be, step 1) in solution A concentration be 0.2~1.0mol/L.
3. a kind of cube shaped frame SnS according to claim 12The preparation method of anode material of lithium-ion battery, its feature
Be, step 3) in ultrasonic vibration processing time be 1~3h.
4. a kind of cube shaped frame SnS according to claim 12The preparation method of anode material of lithium-ion battery, its feature
It is, step 4) the middle pH that the mixed solution D after being handled through ultrasonic vibration is adjusted using ammoniacal liquor.
5. a kind of cube shaped frame SnS according to claim 12The preparation method of anode material of lithium-ion battery, its feature
Be, step 5) in reaction temperature control at 150~200 DEG C, the reaction time is controlled in 1~7h.
6. a kind of cube shaped frame SnS according to claim 12The preparation method of anode material of lithium-ion battery, its feature
Be, step 6) in presoma distinguish centrifuge washing 3~5 times through deionized water and absolute ethyl alcohol.
7. a kind of cube shaped frame SnS according to claim 12The preparation method of anode material of lithium-ion battery, its feature
Be, step 6) in freeze-drying temperature be -40~-60 DEG C, the time be 9~15h.
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Cited By (1)
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| 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 |
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| CN101950804A (en) * | 2010-07-14 | 2011-01-19 | 北京理工大学 | Method for preparing spherical SnS2 anode material of lithium ion battery |
| CN102502791A (en) * | 2011-11-23 | 2012-06-20 | 陕西科技大学 | Method for preparing flower-cluster-shaped tin sulfide (SnS) nanometer particles by microwave hydrothermal method |
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| CN101950804A (en) * | 2010-07-14 | 2011-01-19 | 北京理工大学 | Method for preparing spherical SnS2 anode material of lithium ion battery |
| CN102502791A (en) * | 2011-11-23 | 2012-06-20 | 陕西科技大学 | Method for preparing flower-cluster-shaped tin sulfide (SnS) nanometer particles by microwave hydrothermal method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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