CN106450204B - A kind of high circulation performance SnS2/TiO2The preparation method of anode material of lithium-ion battery - Google Patents

A kind of high circulation performance SnS2/TiO2The preparation method of anode material of lithium-ion battery Download PDF

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CN106450204B
CN106450204B CN201610946172.7A CN201610946172A CN106450204B CN 106450204 B CN106450204 B CN 106450204B CN 201610946172 A CN201610946172 A CN 201610946172A CN 106450204 B CN106450204 B CN 106450204B
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lithium
ion battery
anode material
tio
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CN106450204A (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
刘长青
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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
    • 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
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/485Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • 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
    • 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 kind of high circulation performance SnS2/TiO2The preparation method of anode material of lithium-ion battery, 1) by SnCl4·5H2O is dissolved in deionized water, is configured to solution A, and sodium thiosulfate is dissolved in aliquots of deionized water and is configured to solution B;2) B solution is added dropwise in solution A under magnetic agitation effect, persistently stirs to get homogeneous mixture solotion C;3) butyl titanate is dissolved in absolute ethyl alcohol and obtains mixed solution D, mixed solution D is added dropwise in mixed solution C under magnetic agitation effect and obtains mixed solution E, adjusted pH value of solution=3~9 and form solution F;4) solution F is put into homogeneous hydrothermal reaction kettle to seal, is reacted in homogeneous hydrothermal reactor;5) it waits for after reaction, taking out presoma, distinguish centrifuge washing through deionized water and absolute ethyl alcohol, then freeze-drying obtains high circulation performance SnS2/TiO2Anode material of lithium-ion battery.Manufacturing cost of the present invention is low, short preparation period, and the SnS prepared2/TiO2Anode material of lithium-ion battery has high circulation performance.

Description

A kind of high circulation performance SnS2/TiO2The preparation method of anode material of lithium-ion battery
Technical field
The present invention relates to a kind of preparation methods of anode material of lithium-ion battery, and in particular to a kind of high circulation performance SnS2/TiO2The 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 at 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, has that raw material resources are abundant, price is low Honest and clean, higher than energy, the advantages that having 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 than lithium ion battery bigger 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 greater advance is achieved on the chemical property of experiment preparation method and battery.But sodium ion Ionic radius (r=0.113nm) is about bigger by 30% or more than the ionic radius of lithium ion (r=0.076nm), it is difficult to realize reversible The embedding dealkylation reaction of electrochemistry, insertion-abjection process easily causes collapsing for host lattice structure, cause material cycle performance, times Rate performance and electrochemical utilization rate performance are poor, and 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 basic unit CdI2Layered crystal structure (structure cell Parameter:A=0.3648nm, c=0.5899nm) composition, this structural unit among the sulphion of two layers of hexagonal closs packing by adding Enter sandwich structure (S-Sn-S) composition of tin ion.Every six sulphions are inserted into a tin ion formation regular octahedron and match Position, and there is weak Van der Waals force between layers and pass through Covalent bonding together.In addition, there are many crystalline substances for this layer structure Body vacancy can be used as the host lattice of intercalation.This unique layer structure makes it have excellent photoelectric characteristic.Currently, grinding 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.People prepare semi-conducting material, light using the special performance that these different structures possess Catalysis material, solar cell material, photo-translating system material and lithium ion battery material etc..Unique performance and extensively Application make SnS2Material becomes one of the material for most having application prospect.
Composition, pattern, size due to material etc. 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 sodium ion, then the capacity of material can become larger.And particle is got over It is small, specific surface area is bigger, then contact of the material with electrolyte is better, Na+Migration distance can also shorten, be more advantageous to sodium from The promotion of sub- cell negative electrode material high rate performance.In addition, these special structures such as two dimension, three-dimensional and multistage micro nano structure Its chemical property can be made to obtain prodigious breakthrough.
Currently, nanometer SnS2The preparation method of material mainly has Gu Xiangfanyingfa [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 Bao Lifa [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 Fa [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 simply and anti- The advantages that answering condition to be easy to control, but carried out in solid phase due to reacting, usually reaction is not thorough, and yield is relatively low.Mechanics is removed 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- It is often poor, it may be only available for the scientific research on basis.And solvent thermal reaction method is a kind of improved hydro-thermal reaction method, uses organic solvent Solvent is made instead of traditional water, but reaction process needs the condition of stringent control solvent heat.
Invention content
The purpose of the present invention is to provide a kind of high circulation performance SnS2/TiO2The preparation side of anode material of lithium-ion battery Method, to overcome the problems of the above-mentioned prior art, manufacturing cost of the present invention is low, short preparation period, and the SnS prepared2/TiO2 Anode material of lithium-ion battery has high circulation performance.
In order to achieve the above objectives, the present invention adopts the following technical scheme that:
A kind of high circulation performance SnS2/TiO2The preparation method of anode material of lithium-ion battery, includes 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):Sodium thiosulfate is dissolved in aliquots of deionized water by (1.0~1.53) is configured to solution B;
2) B solution is added dropwise in solution A under magnetic agitation effect, persistently stirs to get homogeneous mixture solotion C;
3) according to elemental mole ratios nTi:nSn=(1~5):Butyl titanate is dissolved in absolute ethyl alcohol by 10 ratio to be mixed Solution D is closed, mixed solution D is added dropwise in mixed solution C under magnetic agitation effect and obtains mixed solution E, is adjusted molten Liquid pH=3~9 forms solution F;
4) solution F is put into homogeneous hydrothermal reaction kettle to seal, packing ratio is controlled 40%~60%, and it is anti-to be put into homogeneous hydro-thermal Device is answered to be reacted;
5) it waits for after reaction, taking out presoma, distinguishes centrifuge washing through deionized water and absolute ethyl alcohol, then freezing is dry It is dry to obtain high circulation performance SnS2/TiO2Anode material of lithium-ion battery.
Further, in step 1) solution A a concentration of 0.6~1.0mol/L.
Further, the ratio of absolute ethyl alcohol and the total volume of deionized water used in step 1) is (1~5) in step 3): (1~7).
Further, using dilute HNO dropwise into mixed solution E in step 3)3Adjust pH value of solution, dilute HNO3It is a concentration of 5mol/L。
Further, at 150~260 DEG C, the reaction time controls in 13~18h for reaction temperature control in step 4).
Further, presoma is distinguished into centrifuge washing 3~5 times through deionized water and absolute ethyl alcohol in step 5).
Further, the temperature being freeze-dried in step 5) is -40~-60 DEG C, and the time is 10~12h.
Compared with prior art, the present invention has technique effect beneficial below:
The present invention is to prepare a kind of high circulation performance SnS2/TiO2Anode material of lithium-ion battery, in preparation method, this Invention product in using hydro-thermal method preparation process be co-precipitation out, be conducive to the uniform mixing of two kinds of substances, crystal Growth and reaction condition, pattern are easy to control.The next structure crystalline of this sheet heap is good simultaneously, conductivity is excellent, piece Hole between shape provides channel to ion and shortens path so that the migration rate of electronics is very fast, this results in the appearance of material Amount is high, cycle performance is more excellent.Being applied to sodium-ion battery cathode has excellent cycle performance, experimental result aobvious Show, under the current density of 300mA/g, discharge capacity can reach 1008mAh/g for the first time, and after recycling 10 times, capacity is maintained at 485mAh/g, the negative material has good cyclical stability under high current density.
Further, by controlling hydrothermal reaction condition, the material prepared by the present invention has capacity height, cycle performance excellent Different, the simple advantage low with reaction temperature of preparation method, and the structure size of material reaches tens to hundreds of nanometers, purity is high, Crystallinity is strong, pattern is uniform.
Description of the drawings
Fig. 1 is the high circulation performance SnS prepared by the embodiment of the present invention 22/TiO2The SEM of anode material of lithium-ion battery Figure;
Fig. 2 is the high circulation performance SnS prepared by the embodiment of the present invention 22/TiO2The performance of anode material of lithium-ion battery Cycle figure.
Specific implementation mode
Embodiments of the present invention are described in further detail below:
A kind of high circulation performance SnS2/TiO2The preparation method of anode material of lithium-ion battery, includes the following steps:
1) by SnCl4·5H2O is dissolved in deionized water, the solution A of a concentration of 0.6~1.0mol/L is configured to, according to member Plain mass ratio mSn:mS=(1.85~2.8):(1.0~1.53) by sodium thiosulfate be dissolved in aliquots of deionized water (i.e. with dissolving SnCl4·5H2The deionized water dosage 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 to get homogeneous mixture solotion C;
3) according to elemental mole ratios nTi:nSn=(1~5):Butyl titanate is dissolved in absolute ethyl alcohol by 10 ratio to be mixed Solution D is closed, the ratio between absolute ethyl alcohol and the total volume of deionized water used in step 1) are (1~5):(1~7), in magnetic agitation Mixed solution D is added dropwise in mixed solution C under effect and obtains solution E, 5mol/L is added dropwise into mixed solution E Dilute HNO3, adjust pH value of solution=3~9 and form solution F;
4) F solution is put into homogeneous hydrothermal reaction kettle to seal, packing ratio is controlled 40%~60%, and it is anti-to be put into homogeneous hydro-thermal Device is answered, at 150~260 DEG C, the reaction time controls in 13~18h for reaction temperature control;
5) it waits for after reaction, taking out presoma, distinguishes centrifuge washing 3~5 times through deionized water and absolute ethyl alcohol ,- 40~-60 DEG C carry out 10~12h of freeze-drying and obtain SnS2/TiO2Product.
The present invention is described in further detail with reference to embodiment:
Embodiment 1
1) by SnCl4·5H2O is dissolved in deionized water, is configured to the solution A of a concentration of 0.6mol/L, according to element quality Compare mSn:mS=1.85:Sodium thiosulfate 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 to get homogeneous mixture solotion C.
3) according to elemental mole ratios nTi:nSn=1:10 ratio butyl titanate is dissolved in absolute ethyl alcohol obtain mixing it is molten The total volume ratio of liquid D, absolute ethyl alcohol and deionized water is 1:1, mixed solution D is added dropwise under magnetic agitation effect mixed It closes in solution C and obtains solution E.The dilute HNO of 5mol/L are added dropwise into mixed solution E3, adjust pH value of solution=3 and form solution F;
4) F solution homogeneous hydrothermal reaction kettle being put into seal, packing ratio is controlled 40%, is put into homogeneous hydrothermal reactor, At 150 DEG C, the reaction time controls in 18h for reaction temperature control;
5) it waits for after reaction, taking out presoma, distinguishes centrifuge washing 3 times, -60 DEG C through deionized water and absolute ethyl alcohol Lower freeze-drying 10h obtains SnS2/TiO2Product.
Embodiment 2
1) by SnCl4·5H2O is dissolved in deionized water, is configured to the solution A of a concentration of 0.8mol/L, according to element quality Compare mSn:mS=2.0:Sodium thiosulfate is dissolved in aliquots of deionized water and is configured to solution B by 1.3;
2) B solution is added dropwise in solution A under magnetic agitation effect, persistently stirs to get homogeneous mixture solotion C.
3) according to elemental mole ratios nTi:nSn=3:10 ratio butyl titanate is dissolved in absolute ethyl alcohol obtain mixing it is molten The total volume ratio of liquid D, absolute ethyl alcohol and deionized water is 2:3, mixed solution D is added dropwise under magnetic agitation effect mixed It closes in solution C and obtains solution E.The dilute HNO of 5mol/L are added dropwise into mixed solution E3, adjust pH value of solution=7 and form solution F;
4) F solution homogeneous hydrothermal reaction kettle being put into seal, packing ratio is controlled 50%, is put into homogeneous hydrothermal reactor, At 200 DEG C, the reaction time controls in 15h for reaction temperature control;
5) it waits for after reaction, taking out presoma, distinguishes centrifuge washing 4 times, -50 DEG C through deionized water and absolute ethyl alcohol Freeze-drying 11h obtains SnS2/TiO2Product.
As can be seen from Figure 1 sample structure prepared by the present embodiment is got up by many flake-assembly modes, nanometer sheet The size of shape is probably between 80-200 nanometers.From the data analysis in Fig. 2 it is found that sample manufactured in the present embodiment is in 300mA/ Under the high current density of g, discharge capacity can reach 1008mAh/g for the first time, and after recycling 10 times, capacity is maintained at 485mAh/g, The negative material has good cyclical stability and capacity retention ratio under high current density.
Embodiment 3
1) by SnCl4·5H2O is dissolved in deionized water, is configured to the solution A of a concentration of 1.0mol/L, according to element quality Compare mSn:mS=2.8:Sodium thiosulfate 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 to get homogeneous mixture solotion C.
3) according to elemental mole ratios nTi:nSn=1:Butyl titanate is dissolved in absolute ethyl alcohol by 2 ratio obtains mixed solution The total volume ratio of D, absolute ethyl alcohol and deionized water is 5:7, mixed solution D is added dropwise to mixing under magnetic agitation effect Solution E is obtained in solution C.The dilute HNO of 5mol/L are added dropwise into mixed solution E3, adjust pH value of solution=9 and form solution F;
4) F solution homogeneous hydrothermal reaction kettle being put into seal, packing ratio is controlled 60%, is put into homogeneous hydrothermal reactor, At 260 DEG C, the reaction time controls in 13h for reaction temperature control;
5) it waits for after reaction, taking out presoma, distinguishes centrifuge washing 5 times, -40 DEG C through deionized water and absolute ethyl alcohol Freeze-drying 12h obtains SnS2/TiO2Product.

Claims (5)

1. a kind of high circulation performance SnS2/TiO2The preparation method of anode material of lithium-ion battery, which is characterized in that including following Step:
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):Sodium thiosulfate is dissolved in aliquots of deionized water by (1.0~1.53) is configured to solution B;
2) B solution is added dropwise in solution A under magnetic agitation effect, persistently stirs to get homogeneous mixture solotion C;
3) according to elemental mole ratios nTi:nSn=(1~5):10 ratio butyl titanate is dissolved in absolute ethyl alcohol obtain mixing it is molten Mixed solution D is added dropwise in mixed solution C under magnetic agitation effect and obtains mixed solution E, adjusts pH value of solution by liquid D =3~9 form solution F, and the ratio of wherein absolute ethyl alcohol and the total volume of deionized water used in step 1) is (1~5):(1~ 7);
4) solution F is put into homogeneous hydrothermal reaction kettle to seal, packing ratio is controlled 40%~60%, is put into homogeneous hydrothermal reactor It is reacted, at 150~260 DEG C, the reaction time controls in 13~18h for reaction temperature control;
5) it waits for after reaction, taking out presoma, distinguishes centrifuge washing through deionized water and absolute ethyl alcohol, then freeze-drying is Obtain high circulation performance SnS2/TiO2Anode material of lithium-ion battery.
2. a kind of high circulation performance SnS according to claim 12/TiO2The preparation method of anode material of lithium-ion battery, It is characterized in that, in step 1) solution A a concentration of 0.6~1.0mol/L.
3. a kind of high circulation performance SnS according to claim 12/TiO2The preparation method of anode material of lithium-ion battery, It is characterized in that, using dilute HNO dropwise into mixed solution E in step 3)3Adjust pH value of solution, dilute HNO3A concentration of 5mol/L.
4. a kind of high circulation performance SnS according to claim 12/TiO2The preparation method of anode material of lithium-ion battery, It is characterized in that, presoma is distinguished centrifuge washing 3~5 times through deionized water and absolute ethyl alcohol in step 5).
5. a kind of high circulation performance SnS according to claim 12/TiO2The preparation method of anode material of lithium-ion battery, It is characterized in that, the temperature being freeze-dried in step 5) is -40~-60 DEG C, the time is 10~12h.
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CN107175097B (en) * 2017-06-22 2019-10-11 陕西科技大学 A kind of stannic disulfide package titanium dioxide composite photocatalyst and preparation method thereof
CN107799743A (en) * 2017-09-29 2018-03-13 华南师范大学 A kind of stannic disulfide titanium dioxide compound and its preparation method and application
CN108786849B (en) * 2018-06-08 2021-08-17 西北师范大学 Preparation and application of tin sulfide/titanium dioxide composite material
CN109935804B (en) * 2019-01-09 2022-06-03 上海大学(浙江·嘉兴)新兴产业研究院 Long-life tin sulfide negative electrode material and preparation method thereof
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