CN106564934A - Method for preparing granular assembly spherical SnS<2> sodium ion battery anode material - Google Patents
Method for preparing granular assembly spherical SnS<2> sodium ion battery anode material Download PDFInfo
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- CN106564934A CN106564934A CN201610945677.1A CN201610945677A CN106564934A CN 106564934 A CN106564934 A CN 106564934A CN 201610945677 A CN201610945677 A CN 201610945677A CN 106564934 A CN106564934 A CN 106564934A
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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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- 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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- 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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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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
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Abstract
The invention discloses a method for preparing a granular assembly spherical SnS<2> sodium ion battery anode material. The method is characterized by comprising the following steps of: (1), dissolving SnCl<4>5H<2>O in deionized water to prepare solution A, and dissolving thioacetamide in the same amount of deionized water to prepare solution B; (2), dropwise adding the solution B into the solution A under the magnetic stirring action, continuously stirring to obtain uniformly mixed solution C, and continuously stirring after dropwise adding NaOH solution to form solution D; (3), putting the solution D in a microwave hydrothermal reaction instrument, and reacting in a homogeneous-phase hydrothermal reactor; and (4), after reaction is ended, taking out a precursor, respectively performing centrifugal washing through deionized water and absolute ethyl alcohol, and freezing and drying so as to obtain the granular assembly spherical SnS<2> sodium ion battery anode material. The method disclosed by the invention is low in preparation cost and short in preparation period; furthermore, the prepared granular assembly spherical SnS<2> sodium ion battery anode material has excellent electrochemical 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 granule assembling is spherical
SnS2The 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 use and develop secondary rechargeable battery and be 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.Compare 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, embedded-abjection process easily causes subsiding for host lattice structure, causes cycle performance, the multiplying power of material
Performance and electrochemical utilization rate poor-performing, therefore, find suitable embedding sode cell material and there is certain difficulty.
SnS2It is belonging 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 is added by the sulphion centre of two-layer hexagonal closs packing
Enter sandwich structure (S-Sn-S) composition of tin ion.Insert a tin ion formation regular octahedron per six sulphions to match 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 be used as the host lattice of intercalation.This unique layer structure makes it have excellent photoelectric characteristic.At present, grind
The persons of studying carefully prepare the SnS of different structure or size by different methods2, main structure have stannic disulfide nanoparticle,
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
Complicated multistage micro nano structure.The special performance that people possess using these different structures prepare semi-conducting material,
Catalysis material, solar cell material, photo-translating system material and lithium ion battery material etc..Unique performance and wide
General application causes SnS2Material becomes most have 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,
The structure and morphology of three-dimensional and multidimensional or porous is conducive to the deintercalation of sodium ion, then the capacity of material can become big.And granule is got over
Little, specific surface area is bigger, then contact of the material with electrolyte is better, Na+Migration distance also can shorten, be more beneficial for sodium ion
The lifting of cell negative electrode material high rate performance.In addition, these special structure meetings such as two-dimentional, 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 has and is not required to play solvent, equipment simple and anti-
The advantages of answering condition to be easily controlled, but because reaction is carried out in solid phase, generally not thoroughly, yield is relatively low for reaction.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
Traditional water is replaced to make solvent, but course of reaction needs the condition of strict control solvent thermal.
The content of the invention
It is an object of the invention to provide a kind of granule assembles spherical SnS2The preparation side of anode material of lithium-ion battery
Method, with the defect for overcoming above-mentioned prior art to exist, preparation cost of the present invention is low, short preparation period, and the particle group prepared
Fill spherical SnS2Anode material of lithium-ion battery electrochemical performance.
To reach above-mentioned purpose, the present invention is adopted the following technical scheme that：
A kind of granule assembles spherical SnS2The preparation method of anode material of lithium-ion battery, comprises the following steps：
1) by SnCl4·5H2O is dissolved in deionized water, is configured to solution A, according to element mass ratio mSn:mS=(1.85～
2.8):Thioacetamide is dissolved in aliquots of deionized water and is configured to solution B by (1.0～1.53)；
2) solution B is added dropwise in solution A under magnetic agitation effect, persistently stirs the C that gets a uniform mixture, adjusted
Section pH value is 4～8, obtains solution D；
3) solution D is placed in microwave hydrothermal reaction, packing ratio is controlled 15%～30%, is put into homogeneous hydro-thermal reaction
Device is reacted；
4) after question response terminates, presoma, Jing deionized waters and dehydrated alcohol difference centrifuge washing are taken out, is then freezed dry
The dry particle group that obtains fills spherical SnS2Anode material of lithium-ion battery.
Further, step 1) in solution A concentration be 0.6～1.3mol/L.
Further, step 2) in using NaOH solution solution adjust pH value, and the concentration of NaOH solution be 0.5mol/L.
Further, step 2) in add NaOH solution after persistently stir 0.5～2h.
Further, step 3) in reaction temperature control at 150～230 DEG C, the response time is controlled in 8～13h.
Further, step 4) in by presoma Jing deionized waters and dehydrated alcohol difference centrifuge washing 3～5 times.
Further, step 4) in cryodesiccated temperature be -40～-60 DEG C, the time be 10～12h.
Compared with prior art, the present invention has following beneficial technique effect：
Granule prepared by the present invention assembles spherical SnS2Anode material of lithium-ion battery, in preparation method, microwave hydrothermal
Method due to the auxiliary of microwave and the full and uniform mixing of hydro-thermal method, with reaction rate is very fast, reaction fully thoroughly, grain growth
The advantages such as controllable and even size distribution, it avoids the high energy consumption of traditional method, reacts the shortcomings of hardly possible is controlled, product is impure.
Material prepared by the present invention has cheap, preparation method simple and short preparation period, electrochemical performance it is excellent
Gesture, in addition, material purity is high, crystallinity is strong, pattern is uniform, be applied to sodium-ion battery negative pole have it is excellent forthright again
Can, test result indicate that, under the electric current density of 50mA/g, its first discharge capacity can reach 731mAh/g, after circulation 10 times,
Capacity is maintained at 417mAh/g, has higher cycle performance under high current density.
Further, by controlling response parameter, granule assembling chondritic SnS prepared2Sodium-ion battery negative pole
Material, because short grained specific surface area is larger, it can increase with the contact area of electrolyte, and ion migration is more, and granule
The hole that formation is piled up between granule provides passage to ion, and ion migration path is shorter, and migration velocity also can be accelerated, and this
Plant hole and provide relief area to the volumetric expansion produced in charge and discharge process, the structure of material just becomes more stable, and this is just
The chemical property of material can be improved.
Description of the drawings
Fig. 1 is to assemble spherical SnS with granule prepared by the embodiment of the present invention 22The SEM of anode material of lithium-ion battery
Figure；
Fig. 2 is that the granule prepared by the embodiment of the present invention 2 assembles spherical SnS2Anode material of lithium-ion battery it is forthright again
Can figure.
Specific embodiment
Embodiments of the present invention are described in further detail below：
A kind of granule assembles spherical SnS2The preparation method of anode material of lithium-ion battery, comprises the following steps：
1) by SnCl4·5H2O is dissolved in deionized water, the solution A that concentration is 0.6～1.3mol/L is configured to, according to unit
Plain mass ratio mSn:mS=(1.85～2.8):Thioacetamide is dissolved in aliquots of deionized water (i.e. with dissolving by (1.0～1.53)
SnCl4·5H2The deionized water consumption of O is equal) in be configured to solution B；
2) B solution is added dropwise in solution A under magnetic agitation effect, persistently stirs the C that gets a uniform mixture, by
Be added dropwise to 0.5mol/L NaOH solutions adjust pH value be 4～8, obtain solution D, after persistently stir 0.5～2h；
3) mixed solution D is placed in microwave hydrothermal reaction, packing ratio is controlled 15%～30%, is put into homogeneous water
Thermal reactor, at 150～230 DEG C, the response time is controlled in 8～13h for reaction temperature control；
4) presoma, Jing deionized waters and dehydrated alcohol difference centrifuge washing 3～5 times are taken out after question response terminates, -40
～-60 DEG C of 10～12h of lyophilization obtain SnS2Product.
The present invention is described in further detail with reference to embodiment：
Embodiment 1
1) by SnCl4·5H2O is dissolved in deionized water, the solution A that concentration is 0.6mol/L is configured to, according to element quality
Compare mSn:mS=1.85:Thioacetamide is dissolved in aliquots of deionized water and is configured to solution B by 1.0；
2) B solution is added dropwise in solution A under magnetic agitation effect, persistently stirs the C that gets a uniform mixture, by
Be added dropwise to 0.5mol/L NaOH solutions adjust pH value be 4, obtain solution D, after persistently stir 0.5h；
3) mixed solution D is placed in microwave hydrothermal reaction, packing ratio is controlled 15%, is put into homogeneous hydro-thermal reaction
Device, at 230 DEG C, the response time is controlled in 8h for reaction temperature control；
4) after question response terminates, presoma, Jing deionized waters and dehydrated alcohol difference centrifuge washing 3 times are taken out, -60 DEG C cold
The dry 10h of lyophilizing obtains SnS2Product.
Embodiment 2
1) by SnCl4·5H2O is dissolved in deionized water, the solution A that concentration is 0.8mol/L is configured to, according to element quality
Compare mSn:mS=2.0:Thioacetamide is dissolved in aliquots of deionized water and is configured to solution B by 1.4；
2) B solution is added dropwise in solution A under magnetic agitation effect, persistently stirs the C that gets a uniform mixture, by
Be added dropwise to 0.5mol/L NaOH solutions adjust pH value be 6, obtain solution D, after persistently stir 1.5h；
3) mixed solution D is placed in microwave hydrothermal reaction, packing ratio is controlled 25%, is put into homogeneous hydro-thermal reaction
Device, at 190 DEG C, the response time is controlled in 10h for reaction temperature control；
4) after question response terminates, presoma, Jing deionized waters and dehydrated alcohol difference centrifuge washing 4 times, -50 DEG C are taken out
Lyophilization 11h obtains SnS2Product.
As can be seen from Figure 1 sample structure prepared by the present embodiment is assembled by many spherical granules,
Particle size is about tens between hundreds of nanometer.The analysis from Fig. 2 understands that granule manufactured in the present embodiment assembles spherical SnS2
Anode material of lithium-ion battery has preferable capability retention in high current.
Embodiment 3
1) by SnCl4·5H2O is dissolved in deionized water, the solution A that concentration is 1.3mol/L is configured to, according to element quality
Compare mSn:mS=2.8:Thioacetamide is dissolved in aliquots of deionized water and is configured to solution B by 1.53；
2) B solution is added dropwise in solution A under magnetic agitation effect, persistently stirs the C that gets a uniform mixture, by
Be added dropwise to 0.5mol/L NaOH solutions adjust pH value be 8, obtain solution D, after persistently stir 2h；
3) mixed solution D is placed in microwave hydrothermal reaction, packing ratio is controlled 30%, is put into homogeneous hydro-thermal reaction
Device, at 150 DEG C, the response time is controlled in 13h for reaction temperature control；
4) after question response terminates, presoma, Jing deionized waters and dehydrated alcohol difference centrifuge washing 5 times are taken out, -40 DEG C cold
The dry 12h of lyophilizing obtains SnS2Product.
Claims (7)
1. a kind of granule assembles spherical SnS2The preparation method of anode material of lithium-ion battery, it is characterised in that including following step
Suddenly：
1) by SnCl4·5H2O is dissolved in deionized water, is configured to solution A, according to element mass ratio mSn:mS=(1.85～
2.8):Thioacetamide is dissolved in aliquots of deionized water and is configured to solution B by (1.0～1.53)；
2) solution B is added dropwise in solution A under magnetic agitation effect, persistently stirs the C that gets a uniform mixture, adjust PH
It is worth for 4～8, obtains forming solution D；
3) solution D is placed in microwave hydrothermal reaction, packing ratio is controlled 15%～30%, is put into homogeneous hydrothermal reactor and is entered
Row reaction；
4) after question response terminates, presoma, Jing deionized waters and dehydrated alcohol difference centrifuge washing are taken out, then lyophilization is
Obtain granule and assemble spherical SnS2Anode material of lithium-ion battery.
2. a kind of granule according to claim 1 assembles spherical SnS2The preparation method of anode material of lithium-ion battery, it is special
Levy and be, step 1) in the concentration of solution A be 0.6～1.3mol/L.
3. a kind of granule according to claim 1 assembles spherical SnS2The preparation method of anode material of lithium-ion battery, it is special
Levy and be, step 2) in pH value is adjusted using NaOH solution, and the concentration of NaOH solution is 0.5mol/L.
4. a kind of granule according to claim 1 assembles spherical SnS2The preparation method of anode material of lithium-ion battery, it is special
Levy and be, step 2) in add and persistently stir 0.5～2h after NaOH solution.
5. a kind of granule according to claim 1 assembles spherical SnS2The preparation method of anode material of lithium-ion battery, it is special
Levy and be, step 3) in reaction temperature control at 150～230 DEG C, the response time is controlled in 8～13h.
6. a kind of granule according to claim 1 assembles spherical SnS2The preparation method of anode material of lithium-ion battery, it is special
Levy and be, step 4) in by presoma Jing deionized waters and dehydrated alcohol difference centrifuge washing 3～5 times.
7. a kind of granule according to claim 1 assembles spherical SnS2The preparation method of anode material of lithium-ion battery, it is special
Levy and be, step 4) in cryodesiccated temperature be -40～-60 DEG C, the time is 10～12h.
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Cited By (3)
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| CN107026265A (en) * | 2017-06-05 | 2017-08-08 | 深圳职业技术学院 | A kind of lithium ion battery SnS2The preparation method of/SnSb composite negative pole materials |
| CN107416892A (en) * | 2017-07-24 | 2017-12-01 | 东北大学 | A kind of SnS with hierarchy2Hydrothermal preparing process |
| CN109286009A (en) * | 2018-09-25 | 2019-01-29 | 陕西科技大学 | A kind of preparation method of nanometer sheet self assembled three-dimensional nano flower artificial gold/graphitization carbonitride lithium ion battery negative material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107026265A (en) * | 2017-06-05 | 2017-08-08 | 深圳职业技术学院 | A kind of lithium ion battery SnS2The preparation method of/SnSb composite negative pole materials |
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| CN107416892A (en) * | 2017-07-24 | 2017-12-01 | 东北大学 | A kind of SnS with hierarchy2Hydrothermal preparing process |
| CN109286009A (en) * | 2018-09-25 | 2019-01-29 | 陕西科技大学 | A kind of preparation method of nanometer sheet self assembled three-dimensional nano flower artificial gold/graphitization carbonitride lithium ion battery negative material |
| CN109286009B (en) * | 2018-09-25 | 2021-06-08 | 陕西科技大学 | Preparation method of nano-sheet self-assembled three-dimensional nano-flower tin sulfide/graphitized carbon nitride lithium ion battery cathode material |
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| CN106564934B (en) | 2018-03-27 |
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