CN106450204A - Preparation method of high cycle performance SnS2/TiO2 sodium ion battery anode materials - Google Patents
Preparation method of high cycle performance SnS2/TiO2 sodium ion battery anode materials Download PDFInfo
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- CN106450204A CN106450204A CN201610946172.7A CN201610946172A CN106450204A CN 106450204 A CN106450204 A CN 106450204A CN 201610946172 A CN201610946172 A CN 201610946172A CN 106450204 A CN106450204 A CN 106450204A
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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
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection 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
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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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- 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 high cycle performance SnS2/TiO2 sodium ion battery anode materials. The preparation method includes the steps: 1) dissolving SnCl4.5H2O into deionized water to prepare solution A, and dissolving sodium thiosulfate into the same amount of deionized water to prepare solution B; 2) gradually dropping the solution B into the solution A under the stirring action of magnetic force, and continually stirring to obtain uniformly mixed solution C; 3) dissolving butyl titanate into absolute ethyl alcohol to obtain mixed solution D, gradually dropping the solution D into the solution C under the stirring action of magnetic force to obtain mixed solution E, and adjusting solution pH (potential of hydrogen) to reach a range from 3 to 9 to form solution F; 4) placing the solution F into a homogeneous-phase hydrothermal reaction kettle to seal, and performing reaction in the homogeneous-phase hydrothermal reaction kettle; 5) taking out precursors after reaction is finished, respectively and centrifugally washing by the deionized water and absolute ethyl alcohol, and carrying out freeze-drying to obtain the high cycle performance SnS2/TiO2 sodium ion battery anode materials. The preparation method is low in preparation cost and preparation period, and the prepared SnS2/TiO2 sodium ion battery anode materials have high cycle 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 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 and become
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 necessity 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 have 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 on the chemical property of experiment preparation method and battery, achieve greater advance.But sodium ion
Ionic radius (r=0.113nm) is than the ionic radius (r=0.076nm) about big more than 30% 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 suitably embedding sode cell material and have certain difficulty.
SnS2It is belonging to IV:The binary compound of VI main group, 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 what the sandwich structure (S-Sn-S) of tin ion was constituted.Insert a tin ion formation regular octahedron to join per six sulphions
Position, and there is weak Van der Waals force between layers and by Covalent bonding together.In addition, there are a lot of 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 multiple
Miscellaneous multistage micro nano structure.The special performance that people possess using these different structures is preparing semi-conducting material, light
Catalysis material, solar cell material, photo-translating system material and lithium ion battery material etc..Unique performance and extensively
Application cause SnS2Material becomes most one of material of application prospect.
As the composition of material, pattern, size etc. be able to can be affected 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 can also 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 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]
.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 as 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 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
Replace traditional water that solvent is made, but course of reaction needs the condition of strict control solvent thermal.
Content of the invention
It is an object of the invention to provide a kind of high circulation performance SnS2/TiO2The 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 SnS for preparing2/TiO2
Anode material of lithium-ion battery has high circulation performance.
For reaching above-mentioned purpose, the present invention is adopted the following technical scheme that：
A kind of high circulation performance SnS2/TiO2The 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):(1.0～1.53) are dissolved in sodium thiosulfate in aliquots of deionized water and are configured to solution B；
2) under magnetic agitation effect, B solution is added dropwise in solution A, the continuously stirred C that gets a uniform mixture；
3) according to elemental mole ratios nTi:nSn=(1～5):10 ratio is dissolved in butyl titanate in dehydrated alcohol is mixed
Solution D is closed, is added dropwise in mixed solution C, obtain mixed solution E by mixed solution D under magnetic agitation effect, adjusts molten
Liquid pH=3～9 form solution F；
4) solution F is put into the sealing of homogeneous hydrothermal reaction kettle, packing ratio control is put into homogeneous hydro-thermal anti-40%～60%
Device is answered to be reacted；
5) after question response terminates, presoma is taken out, through deionized water and dehydrated alcohol difference centrifuge washing, then freezes dry
Dry obtain high circulation performance SnS2/TiO2Anode material of lithium-ion battery.
Further, step 1) in solution A concentration be 0.6～1.0mol/L.
Further, step 3) in dehydrated alcohol and step 1) in institute's deionized water cumulative volume ratio be (1～5):
(1～7).
Further, step 3) in using dropwise dilute HNO in mixed solution E3Adjust pH value of solution, dilute HNO3Concentration be
5mol/L.
Further, step 4) in reaction temperature control at 150～260 DEG C, the response time controls in 13～18h.
Further, step 5) in by presoma through centrifuge washing 3～5 times respectively of deionized water and dehydrated alcohol.
Further, step 5) 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：
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 is co-precipitated out, is conducive to the uniform mixing of two kinds of materials, crystal
Growth and reaction condition, pattern are easy to control.While this lamellar is piled up, the structure crystalline for getting up is good, electrical conductivity is excellent, piece
Hole between shape provides passage to ion and shortens path so that the migration rate of electronics is very fast, and this results in the appearance of material
Amount is high, cycle performance is more excellent.It is applied to sodium-ion battery negative pole and there is excellent cycle performance, experimental result shows
Show, under the electric current density of 300mA/g, its first discharge capacity can reach 1008mAh/g, after circulation 10 times, capacity is maintained at
485mAh/g, under high current density, the negative material has good cyclical stability.
Further, by controlling hydrothermal reaction condition, the material prepared by the present invention has that capacity is high, cycle performance is excellent
The low advantage of the simple and reaction temperature of different, preparation method, and the physical dimension of material reaches tens to hundreds of nanometer, purity is high,
Crystallinity is strong, pattern is uniform.
Description of the drawings
Fig. 1 is 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 high circulation performance SnS prepared by the embodiment of the present invention 22/TiO2The performance of anode material of lithium-ion battery
Circulation figure.
Specific embodiment
Below embodiments of the present invention are described in further detail：
A kind of high circulation performance SnS2/TiO2The 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 the solution A that concentration is 0.6～1.0mol/L, according to unit
Plain mass ratio mSn:mS=(1.85～2.8):Sodium thiosulfate 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 solution A, the continuously stirred C that gets a uniform mixture；
3) according to elemental mole ratios nTi:nSn=(1～5):10 ratio is dissolved in butyl titanate in dehydrated alcohol is mixed
Close solution D, dehydrated alcohol and step 1) in the ratio of cumulative volume of institute's deionized water be (1～5):(1～7), in magnetic agitation
Under effect, mixed solution D being added dropwise to solution E is obtained in mixed solution C, is added dropwise over 5mol/L's in mixed solution E
Dilute HNO3, adjust pH value of solution=3～9 and form solution F；
4) F solution is put into the sealing of homogeneous hydrothermal reaction kettle, packing ratio control is put into homogeneous hydro-thermal anti-40%～60%
Device is answered, reaction temperature control is at 150～260 DEG C, and the response time controls in 13～18h；
5), after question response terminates, presoma is taken out, through centrifuge washing 3～5 times respectively of deionized water and dehydrated alcohol ,-
40～-60 DEG C carry out 10～12h of lyophilization and obtain SnS2/TiO2Product.
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 solution A of the concentration for 0.6mol/L, according to element quality
Compare mSn:mS=1.85:1.0 are dissolved in sodium thiosulfate in aliquots of deionized water and are configured to solution B；
2) under magnetic agitation effect, B solution is added dropwise in solution A, the continuously stirred C that gets a uniform mixture.
3) according to elemental mole ratios nTi:nSn=1:10 ratio butyl titanate is dissolved in dehydrated alcohol obtain mixing molten
Liquid D, dehydrated alcohol is 1 with the cumulative volume ratio of deionized water:1, under magnetic agitation effect, mixed solution D is added dropwise to mix
Close in solution C and obtain solution E.The dilute HNO of 5mol/L is added dropwise in mixed solution E3, adjust pH value of solution=3 and form solution F；
4) F solution is put into the sealing of homogeneous hydrothermal reaction kettle, packing ratio control is put into homogeneous hydrothermal reactor 40%,
Reaction temperature control is at 150 DEG C, and the response time controls in 18h；
5) after question response terminates, presoma is taken out, through deionized water and dehydrated alcohol centrifuge washing 3 times respectively, at -60 DEG C
Lyophilization 10h obtains SnS2/TiO2Product.
Embodiment 2
1) by SnCl4·5H2O is dissolved in deionized water, is configured to solution A of the concentration for 0.8mol/L, according to element quality
Compare mSn:mS=2.0:1.3 are dissolved in sodium thiosulfate in aliquots of deionized water and are configured to solution B；
2) under magnetic agitation effect, B solution is added dropwise in solution A, the continuously stirred C that gets a uniform mixture.
3) according to elemental mole ratios nTi:nSn=3:10 ratio butyl titanate is dissolved in dehydrated alcohol obtain mixing molten
Liquid D, dehydrated alcohol is 2 with the cumulative volume ratio of deionized water:3, under magnetic agitation effect, mixed solution D is added dropwise to mix
Close in solution C and obtain solution E.The dilute HNO of 5mol/L is added dropwise in mixed solution E3, adjust pH value of solution=7 and form solution F；
4) F solution is put into the sealing of homogeneous hydrothermal reaction kettle, packing ratio control is put into homogeneous hydrothermal reactor 50%,
Reaction temperature control is at 200 DEG C, and the response time controls in 15h；
5) after question response terminates, presoma is taken out, through deionized water and dehydrated alcohol centrifuge washing 4 times respectively, -50 DEG C cold
The dry 11h of lyophilizing obtains SnS2/TiO2Product.
As can be seen from Figure 1 sample structure prepared by the present embodiment is got up by many flake-assembly mode, nanometer sheet
The size of shape is probably between 80-200 nanometer.Data analysiss from Fig. 2 understand, sample manufactured in the present embodiment is in 300mA/
Under the high current density of g, its first discharge capacity can reach 1008mAh/g, after circulation 10 times, capacity is maintained at 485mAh/g,
Under high current density, the negative material has good cyclical stability and capability retention.
Embodiment 3
1) by SnCl4·5H2O is dissolved in deionized water, is configured to solution A of the concentration for 1.0mol/L, according to element quality
Compare mSn:mS=2.8:1.53 are dissolved in sodium thiosulfate in aliquots of deionized water and are configured to solution B；
2) under magnetic agitation effect, B solution is added dropwise in solution A, the continuously stirred C that gets a uniform mixture.
3) according to elemental mole ratios nTi:nSn=1:2 ratio is dissolved in butyl titanate in dehydrated alcohol and obtains mixed solution
D, dehydrated alcohol is 5 with the cumulative volume ratio of deionized water:7, under magnetic agitation effect, mixed solution D is added dropwise to mixing
Solution E is obtained in solution C.The dilute HNO of 5mol/L is added dropwise in mixed solution E3, adjust pH value of solution=9 and form solution F；
4) F solution is put into the sealing of homogeneous hydrothermal reaction kettle, packing ratio control is put into homogeneous hydrothermal reactor 60%,
Reaction temperature control is at 260 DEG C, and the response time controls in 13h；
5) after question response terminates, presoma is taken out, through deionized water and dehydrated alcohol centrifuge washing 5 times respectively, -40 DEG C cold
The dry 12h of lyophilizing obtains SnS2/TiO2Product.
Claims (7)
1. a kind of high circulation performance SnS2/TiO2The preparation method of anode material of lithium-ion battery, it is characterised 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):(1.0～1.53) are dissolved in sodium thiosulfate in aliquots of deionized water and are configured to solution B；
2) under magnetic agitation effect, B solution is added dropwise in solution A, the continuously stirred C that gets a uniform mixture；
3) according to elemental mole ratios nTi:nSn=(1～5):10 ratio butyl titanate is dissolved in dehydrated alcohol obtain mixing molten
Mixed solution D is added dropwise to obtain mixed solution E in mixed solution C under magnetic agitation effect, adjusts pH value of solution by liquid D
=3～9 form solution F；
4) solution F is put into the sealing of homogeneous hydrothermal reaction kettle, packing ratio control is put into homogeneous hydrothermal reactor 40%～60%
Reacted；
5) after question response terminates, presoma is taken out, through deionized water and dehydrated alcohol difference centrifuge washing, then lyophilization 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,
Characterized in that, step 1) in solution A concentration be 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,
Characterized in that, step 3) in dehydrated alcohol and step 1) in institute's deionized water cumulative volume ratio be (1～5):(1～7).
4. a kind of high circulation performance SnS according to claim 12/TiO2The preparation method of anode material of lithium-ion battery,
Characterized in that, step 3) in using dropwise dilute HNO in mixed solution E3Adjust pH value of solution, dilute HNO3Concentration be 5mol/L.
5. a kind of high circulation performance SnS according to claim 12/TiO2The preparation method of anode material of lithium-ion battery,
Characterized in that, step 4) in reaction temperature control at 150～260 DEG C, the response time controls in 13～18h.
6. a kind of high circulation performance SnS according to claim 12/TiO2The preparation method of anode material of lithium-ion battery,
Characterized in that, step 5) in by presoma through centrifuge washing 3～5 times respectively of deionized water and dehydrated alcohol.
7. a kind of high circulation performance SnS according to claim 12/TiO2The preparation method of anode material of lithium-ion battery,
Characterized in that, step 5) in cryodesiccated temperature be -40～-60 DEG C, the time be 10～12h.
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| CN107175097A (en) * | 2017-06-22 | 2017-09-19 | 陕西科技大学 | A kind of stannic disulfide parcel titanium dioxide composite photocatalyst and preparation method thereof |
| CN107349936A (en) * | 2017-06-05 | 2017-11-17 | 陕西科技大学 | A kind of bar-shaped titanium disulfide and composite titania material preparation method |
| 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 |
| CN108786849A (en) * | 2018-06-08 | 2018-11-13 | 西北师范大学 | A kind of preparation and application of artificial gold/composite titania material |
| CN109935804A (en) * | 2019-01-09 | 2019-06-25 | 上海大学(浙江·嘉兴)新兴产业研究院 | A kind of long-life vulcanization tin negative pole material and preparation method thereof |
| CN111517363A (en) * | 2020-04-30 | 2020-08-11 | 浙江理工大学 | Cu2O@SnS2Sheet-shaped hollow pipe and preparation method thereof |
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| CN105514392A (en) * | 2016-01-25 | 2016-04-20 | 陕西科技大学 | SnS2-SnO2 nanometer flake-shaped sodium ion battery cathode material and preparation method thereof |
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| CN107349936A (en) * | 2017-06-05 | 2017-11-17 | 陕西科技大学 | A kind of bar-shaped titanium disulfide and composite titania material preparation method |
| CN107175097A (en) * | 2017-06-22 | 2017-09-19 | 陕西科技大学 | A kind of stannic disulfide parcel titanium dioxide composite photocatalyst and preparation method thereof |
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| CN108786849A (en) * | 2018-06-08 | 2018-11-13 | 西北师范大学 | A kind of preparation and application of artificial gold/composite titania material |
| CN109935804A (en) * | 2019-01-09 | 2019-06-25 | 上海大学(浙江·嘉兴)新兴产业研究院 | A kind of long-life vulcanization tin negative pole material and preparation method thereof |
| 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 |
| CN111517363A (en) * | 2020-04-30 | 2020-08-11 | 浙江理工大学 | Cu2O@SnS2Sheet-shaped hollow pipe and preparation method thereof |
| CN111517363B (en) * | 2020-04-30 | 2022-04-01 | 浙江理工大学 | Cu2O@SnS2Sheet-shaped hollow pipe and preparation method thereof |
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