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 PDFInfo
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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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- 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
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- 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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/387—Tin or alloys based on 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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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 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
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 |
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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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Cited By (5)
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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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