CN106374090A - Preparation method of core-shell structured carbon coated SnS2 lithium ion battery negative electrode material - Google Patents

Preparation method of core-shell structured carbon coated SnS2 lithium ion battery negative electrode material Download PDF

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CN106374090A
CN106374090A CN201610946936.2A CN201610946936A CN106374090A CN 106374090 A CN106374090 A CN 106374090A CN 201610946936 A CN201610946936 A CN 201610946936A CN 106374090 A CN106374090 A CN 106374090A
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lithium ion
ion battery
preparation
battery negative
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CN106374090B (en
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殷立雄
程如亮
张峰
黄剑锋
房佳萌
孔新刚
柴思敏
张�浩
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Shaanxi University of Science and Technology
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/362Composites
    • H01M4/366Composites as layered products
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/38Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/387Tin or alloys based on tin
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection 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
    • H01M4/581Chalcogenides or intercalation compounds thereof
    • H01M4/5815Sulfides
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection 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
    • H01M4/583Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624Electric conductive fillers
    • H01M4/625Carbon or graphite
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention discloses a preparation method of a core-shell structured carbon coated SnS2 lithium ion battery negative electrode material. The preparation method comprises the steps of 1) dissolving SnC<14>.5H<2>O in deionized water to prepare a solution A, and dissolving thioacetamide in the equivalent amount of deionized water to prepare a solution B; 2) dropwise adding the solution B to the solution A under the effect of magnetic stirring, continuing to stir to form a uniform mixed solution C, and adding graphite to the mixed solution C under the effect of magnetic stirring until the graphite is completely and uniformly mixed to obtain a mixed solution D; 3) regulating pH of the mixed solution D under the effect of the magnetic stirring to form a solution E; 4) placing the solution E in a uniform-phase hydrothermal reaction kettle for sealing, and placing the solution E in a uniform-phase hydrothermal reaction device for reaction; and 5) taking out a precursor after reaction is completed, respectively and centrifugally washing the precursor with deionized water and absolute ethyl alcohol, and performing freezing and drying to obtain the coated SnS2 lithium ion battery negative electrode material. The preparation method has the advantages of low cost and short preparation period and is simple to operate, and the prepared carbon coated SnS2 lithium ion battery negative electrode material is excellent in performance.

Description

A kind of nucleocapsid structure carbon coating sns2The preparation method of lithium ion battery negative material
Technical field
The present invention relates to a kind of preparation method of lithium ion battery negative material is and in particular to a kind of nucleocapsid structure carbon coating sns2The preparation method of lithium ion battery negative material.
Background technology
Lithium ion battery, as a kind of rechargeable secondary cell, relies primarily on lithium ion deintercalation between a positive electrode and a negative electrode To be operated.In addition, it has, running voltage is high, have extended cycle life, specific capacity is big, have a safety feature, self discharge is little, no remember Recall the advantages such as effect.This advantage makes its range of application widely, at present mainly as mobile phone, photographing unit, notebook The ideal source of the portable sets such as computer.Passed through in lithium ion battery charge/discharge capacity, multiplying power property, cycle performance in recent years Etc. the continuous development of aspect and improvement, its use in fields such as new-energy automobile, electric tool, Aero-Space and energy storage by Flaring is big.As can be seen here, lithium ion battery can become the Main way of following secondary cell development.Under this background, lithium from Sub- battery is subject to the extensive concern of countries in the world research worker and government, enterprise, critical material and correlation technique to grind in recent years Study carefully and quickly grow.But still the problem having many needs to solve, such as: not, this makes for high cost, capacity requirement and cycle performance We will research and develop suitable battery material and become to attach most importance to.
sns2It is belonging to the binary compound of iv:vi main group, by hexagonal phase elementary cell cdi2Layered crystal structure (structure cell Parameter: a=0.3648nm, c=0.5899nm) composition, this construction unit is by addition in the middle of the sulphion of two-layer hexagonal closs packing The sandwich structure (s-sn-s) of tin ion is constituted.Every six sulphions insert a tin ion and form regular octahedron coordination, And there is weak Van der Waals force between layers and pass through Covalent bonding together.In addition, there are a lot of crystal in this layer structure Room, can be used as the host lattice of intercalation.This unique layer structure makes it have excellent photoelectric characteristic.At present, study Persons prepare the sns of different structure or size by different methods2, main structure has stannic disulfide nanoparticle, receives Zero dimension, the one-dimensional and two-dimentional or 3-D nano, structures such as rice ball, nanometer sheet, nanotube, nano-plates, in addition also increasingly complex Multistage micro nano structure.People prepare semi-conducting material using the special performance that these different structures possess, light is urged Change material, solar cell material, photo-translating system material and lithium ion battery material etc..Unique performance and widely Application makes sns2Material becomes one of material of application prospect most.
Because the composition of material, pattern, size etc. can be able to affect to the chemical property of sample.Two dimension, Three-dimensional and multidimensional or porous structure and morphology is conducive to the deintercalation of lithium ion, then the capacity of material can become big.And granule is got over Little, specific surface area is bigger, then the contact with electrolyte for the material is better, li+Migration distance also can 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-dimentional, three-dimensional and multistage micro nano structure Its chemical property is made 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] 2013,5 (20): 9,666 9670.] .nanoscale, 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 answer condition to be easily controlled, but because reaction is carried out 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 obtains, 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, use organic solvent Replace traditional water to make solvent, but course of reaction needs the strict condition controlling solvent thermal.
Content of the invention
It is an object of the invention to provide a kind of nucleocapsid structure carbon coating sns2The preparation side of lithium ion battery negative material Method, with the defect overcoming above-mentioned prior art to exist, preparation cost of the present invention is low, simple to operate, short preparation period, the core of preparation Shell structure carbon coating sns2Lithium ion battery negative material excellent performance.
For reaching above-mentioned purpose, the present invention adopts the following technical scheme that
A kind of nucleocapsid structure carbon coating sns2The preparation method of lithium ion battery negative material, 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): (1.0~1.53) thioacetamide are dissolved in aliquots of deionized water and are configured to solution b;
2) under magnetic agitation effect, b solution is added dropwise in a solution, continuously stirred uniformly mixed solution c, in magnetic Element mass ratio m is pressed under power stirring actionsn:mc=(9~12): 1 adds in mixed solution c graphite until graphite is thoroughly mixed Uniformly obtain mixed solution d;
3) ph=1~8 adjusting mixed solution d under magnetic agitation effect form solution e;
4) solution e is put into the sealing of homogeneous hydrothermal reaction kettle, packing ratio controls 40%~60%, puts into homogeneous hydro-thermal reaction Instrument is reacted;
5) after question response terminates, take out presoma, through deionized water and dehydrated alcohol centrifuge washing respectively, then freeze dry Dry obtain carbon coating sns2Lithium ion battery negative material.
Further, in step 1), the concentration of solution a is 0.6~1.0mol/l.
Further, in step 3) using in mixed solution d dropwise dilute hydrochloric acid adjust solution ph, the concentration of dilute hydrochloric acid is 5mol/l.
Further, in step 4), reaction temperature controls at 120~200 DEG C, and the response time controls in 8~23h.
Further, in step 5) by presoma through centrifuge washing 3~5 times respectively of deionized water and dehydrated alcohol.
Further, in step 5), cryodesiccated temperature is -40~-60 DEG C, and the time is 10~12h.
Compared with prior art, the present invention has a following beneficial technique effect:
Present invention preparation has nucleocapsid structure carbon coating sns2Lithium ion battery negative material, in preparation method, homogeneously Hydro-thermal reaction method makes the material in hydrothermal reaction kettle sufficiently be stirred due to the rotation of support, thus reaction rate is very fast, Reaction is fully thorough, and product crystallinity is strong, pattern is special, grain growth is controlled and even size distribution, and it eliminates tradition and adds The thermal loss of hot mode, have that firing rate is fast, homogeneous heating no thermograde, no hysteresis effect the features such as.Furthermore it is possible to Control very well and be coated on sns2The thickness of surface carbon, realizes uniformly coating.The purity of prepared material is high, crystallinity is strong, shape Looks uniformly, are applied to lithium ion battery negative and have excellent charge-discharge magnification performance.Experimental result shows, in 100ma/ Under the electric current density of g, its first discharge capacity can reach 400mah/g, after circulation 40 times, capacity is maintained at 210mah/g Left and right, has higher stability under high current density.
Further, the present invention passes through to control response parameter, and obtained has nucleocapsid structure carbon coating sns2Lithium ion The size of cell negative electrode material reaches tens and arrives hundreds of nanometer, in sns2Coated with carbon can also improve the stability of structure, So that structure is not susceptible to subside in charge and discharge process, the sei film being formed in electrolyte surface has stability.Meanwhile, Electron transfer rate in structure is improved so that the cyclical stability of battery material and capacity improve further.
Brief description
Fig. 1 is that have nucleocapsid structure carbon coating sns prepared by the embodiment of the present invention 12Lithium ion battery negative material Sem schemes;
Fig. 2 is nucleocapsid structure carbon coating sns prepared by the embodiment of the present invention 12The multiplying power of lithium ion battery negative material Performance map.
Specific embodiment
Below embodiments of the present invention are described in further detail:
A kind of nucleocapsid structure carbon coating sns2The preparation method of lithium ion battery negative material, comprises the following steps:
1) by sncl4·5h2O is dissolved in deionized water, is configured to the solution a that concentration is 0.6~1.0mol/l, 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) under magnetic agitation effect, b solution is added dropwise in a solution, continuously stirred uniformly mixed solution c, in magnetic M is pressed under power stirring actionsn:mc=(9~12): 1 adds in mixed solution c graphite until graphite is mixed thoroughly and is mixed Close solution d;
3) under magnetic agitation effect to mixed solution d in be added dropwise over 5mol/l dilute hydrochloric acid, adjust solution ph=1~8 shape Become solution e;
4) solution e is put into the sealing of homogeneous hydrothermal reaction kettle, packing ratio controls 40%~60%, puts into homogeneous hydro-thermal reaction Instrument, reaction temperature controls at 120~200 DEG C, and the response time controls in 8~20h;
5), after question response terminates, take out presoma, through centrifuge washing 3~5 times respectively of deionized water and dehydrated alcohol, -40 ~-60 DEG C of lyophilization 10~12h obtain the sns of carbon coating2Product.
With reference to embodiment, the present invention is described in further detail:
Embodiment 1
1) by sncl4·5h2O is dissolved in deionized water, is configured to the solution a that concentration is 0.6mol/l, according to element quality Compare msn:ms=1.85:1.0 thioacetamide is dissolved in aliquots of deionized water and is configured to solution b;
2) under magnetic agitation effect, b solution is added dropwise in a solution, continuously stirred uniformly mixed solution c, in magnetic M is pressed under power stirring actionsn:mc=9:1 graphite is added in mixed solution c until nickel foam be mixed thoroughly obtain mixing molten Liquid d;
3) under magnetic agitation effect to mixed solution d in be added dropwise over 5mol/l dilute hydrochloric acid, adjust solution ph=1 and formed Solution e;
4) solution e is put into the sealing of homogeneous hydrothermal reaction kettle, packing ratio controls 40%, puts into homogeneous hydro-thermal reaction instrument, instead Answer temperature control at 120 DEG C, the response time controls in 8h;
5) after question response terminates, take out presoma, through deionized water and dehydrated alcohol centrifuge washing 3 times respectively, -60 DEG C cold The dry 10h of lyophilizing obtains the sns of carbon coating2Product.
As can be seen from Figure 1 nucleocapsid structure carbon coating sns prepared by the present embodiment2Lithium ion battery negative material is core Shell structure, and the size of nucleocapsid structure is about 30nm-80nm.As can be seen from Figure 2 the nucleocapsid knot prepared by the present embodiment Structure carbon coating sns2Lithium ion battery negative material under different electric current densities the capacity attenuation of battery very slow, and have certain Cyclical stability.
Embodiment 2
1) by sncl4·5h2O is dissolved in deionized water, is configured to the solution a that concentration is 0.8mol/l, according to element quality Compare msn:ms=2.0:1.3 thioacetamide is dissolved in aliquots of deionized water and is configured to solution b;
2) under magnetic agitation effect, b solution is added dropwise in a solution, continuously stirred uniformly mixed solution c, in magnetic M is pressed under power stirring actionsn:mc=11:1 adds in mixed solution c graphite until graphite is mixed thoroughly and obtains mixed solution d;
3) under magnetic agitation effect to mixed solution d in be added dropwise over 5mol/l dilute hydrochloric acid, adjust solution ph=5 and formed Solution e;
4) solution e is put into the sealing of homogeneous hydrothermal reaction kettle, packing ratio controls 50%, puts into homogeneous hydro-thermal reaction instrument, instead Answer temperature control at 160 DEG C, the response time controls in 16h;
5) after question response terminates, take out presoma, through deionized water and dehydrated alcohol centrifuge washing 4 times respectively, -50 DEG C cold The dry 11h of lyophilizing obtains the sns of carbon coating2Product.
Embodiment 3
1) by sncl4·5h2O is dissolved in deionized water, is configured to the solution a that concentration is 1.0mol/l, according to element quality Compare msn:ms=2.8:1.53 thioacetamide is dissolved in aliquots of deionized water and is configured to solution b;
2) under magnetic agitation effect, b solution is added dropwise in a solution, continuously stirred uniformly mixed solution c, in magnetic M is pressed under power stirring actionsn:mc=12:1 adds in mixed solution c graphite until graphite is mixed thoroughly and obtains mixed solution d;
3) under magnetic agitation effect to mixed solution d in be added dropwise over 5mol/l dilute hydrochloric acid, adjust solution ph=8 and formed Solution e;
4) solution e is put into the sealing of homogeneous hydrothermal reaction kettle, packing ratio controls 60%, puts into homogeneous hydro-thermal reaction instrument, instead Answer temperature control at 200 DEG C, the response time controls in 20h;
5) after question response terminates, take out presoma, through deionized water and dehydrated alcohol centrifuge washing 5 times respectively, -40 DEG C cold The dry 12h of lyophilizing obtains the sns of carbon coating2Product.

Claims (6)

1. a kind of nucleocapsid structure carbon coating sns2The preparation method of lithium ion battery negative material is it is characterised in that include following walking Rapid:
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): (1.0~1.53) thioacetamide are dissolved in aliquots of deionized water and are configured to solution b;
2) under magnetic agitation effect, b solution is added dropwise in a solution, continuously stirred uniformly mixed solution c, stirs in magnetic force Mix under effect by element mass ratio msn:mc=(9~12): 1 adds in mixed solution c graphite until graphite is mixed thoroughly Obtain mixed solution d;
3) ph=1~8 adjusting mixed solution d under magnetic agitation effect form solution e;
4) solution e is put into the sealing of homogeneous hydrothermal reaction kettle, packing ratio controls 40%~60%, puts into homogeneous hydro-thermal reaction instrument Reacted;
5) after question response terminates, take out presoma, through deionized water and dehydrated alcohol centrifuge washing respectively, then lyophilization is Obtain carbon coating sns2Lithium ion battery negative material.
2. a kind of nucleocapsid structure carbon coating sns according to claim 12The preparation method of lithium ion battery negative material, its Be characterised by, step 1) in solution a concentration be 0.6~1.0mol/l.
3. a kind of nucleocapsid structure carbon coating sns according to claim 12The preparation method of lithium ion battery negative material, its Be characterised by, step 3) in using in mixed solution d dropwise dilute hydrochloric acid adjust solution ph, the concentration of dilute hydrochloric acid is 5mol/l.
4. a kind of nucleocapsid structure carbon coating sns according to claim 12The preparation method of lithium ion battery negative material, its Be characterised by, step 4) in reaction temperature control at 120~200 DEG C, the response time controls in 8~20h.
5. a kind of nucleocapsid structure carbon coating sns according to claim 12The preparation method of lithium ion battery negative material, its Be characterised by, step 5) in by presoma through centrifuge washing 3~5 times respectively of deionized water and dehydrated alcohol.
6. a kind of nucleocapsid structure carbon coating sns according to claim 12The preparation method of lithium ion battery negative material, its Be characterised by, step 5) in cryodesiccated temperature be -40~-60 DEG C, the time be 10~12h.
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CN108390042A (en) * 2018-03-01 2018-08-10 中国科学院福建物质结构研究所 A kind of carbon packet SnS2Composite material and preparation method and application
CN109360950A (en) * 2018-09-17 2019-02-19 陕西科技大学 A kind of cobalt sulfide/carbon composite and preparation method thereof
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Publication number Priority date Publication date Assignee Title
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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CN108390042A (en) * 2018-03-01 2018-08-10 中国科学院福建物质结构研究所 A kind of carbon packet SnS2Composite material and preparation method and application
CN109360950A (en) * 2018-09-17 2019-02-19 陕西科技大学 A kind of cobalt sulfide/carbon composite and preparation method thereof
CN111785967A (en) * 2020-06-30 2020-10-16 北京高压科学研究中心 Core-shell structure chalcogenide negative electrode material and preparation method thereof

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