CN107221646B - A kind of vanadium disulfide nanometer sheet and its preparation method and application of hydroxide vanadyl cladding - Google Patents

A kind of vanadium disulfide nanometer sheet and its preparation method and application of hydroxide vanadyl cladding Download PDF

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CN107221646B
CN107221646B CN201710571056.6A CN201710571056A CN107221646B CN 107221646 B CN107221646 B CN 107221646B CN 201710571056 A CN201710571056 A CN 201710571056A CN 107221646 B CN107221646 B CN 107221646B
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nanometer sheet
cladding
reaction
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vooh
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CN107221646A (en
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黄剑锋
***
曹丽云
冯亮亮
李瑞梓
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Shaanxi University of Science and Technology
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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
    • H01M4/04—Processes of manufacture in general
    • H01M4/0402—Methods of deposition of the material
    • H01M4/0416—Methods of deposition of the material involving impregnation with a solution, dispersion, paste or dry powder
    • 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
    • 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 present invention provides a kind of vanadium disulfide nanometer sheets and its preparation method and application of hydroxide vanadyl cladding, and sodium metavanadate and thioacetamide are dissolved in deionized water simultaneously under magnetic agitation state.Then, liner is then placed in homogeneous reaction instrument by sealing after above-mentioned solution being poured into reaction liner loaded on fixation in outer kettle.Finally, the VS of VOOH cladding can be obtained in washing, collection, drying after the product cooling after reaction2Nanometer sheet.The VS of VOOH cladding prepared by the present invention2Nanometer sheet chemical composition is uniform, and purity is higher, and pattern is uniform, and has specific self-assembled structures, and excellent chemical property is shown when as sodium ion battery electrode material.In addition, the disadvantage high the method overcome conventional calcination method temperature, and large scale equipment and harsh reaction condition are not needed, and raw material is cheap and easy to get, and at low cost, yield is high, is not necessarily to post-processing, and it is environmentally friendly, it can be suitble to be mass produced.

Description

A kind of vanadium disulfide nanometer sheet and its preparation method and application of hydroxide vanadyl cladding
[technical field]
The present invention relates to a kind of preparation methods of composite material, and in particular to a kind of VS of VOOH cladding2The system of nanometer sheet Preparation Method and application.
[background technique]
Sodium because of widely distributed and at low cost feature, sodium-ion battery is as next generation's large scale energy stores System is receive more and more attention.In order to find suitable anode material of lithium-ion battery, the hand that researcher passes through experiment Section explores a large amount of active material.In these negative electrode materials, since they have the layer structure of suitable interlayer space, mistake Cross metal disulfides such as MoS2、WS2And VS2Etc. being considered as a kind of very promising candidate.Although nearest research is Through showing MoS2And WS2It can show excellent storage sodium performance, but electron-transport poor caused by their characteristic of semiconductor Performance limits it and further develops.As a prototypical member in transition metal dichalcogenide family, possess excellent conduction The metallic state VS of property2It is expected to show excellent electron-transporting in the cyclic process as sodium cell negative pole material Energy.VS2Belong to a kind of hexagonal crystal system with layer structure, metallic state V, which is mixed between two layers of S, forms S-V-S layers, S-V- S is stacked in space and is formd layer structure, and space length between layers isIt can be provided for the insertion of sodium ion Sufficient space.It is noted that between layers by Van der Waals force connect, this weak connection facilitate sodium ion/ Electronics is quickly transmitted in interlayer without causing serious structure to be destroyed.In addition, correlative study also indicates that stratiform VS2With high ratio Capacity, big surface-active, low ion diffusional resistance and low open-circuit voltage, this more makes VS2Becoming one kind has prospect Sodium ion negative electrode material.However, recently about VS2Research but focus primarily upon electro-catalysis, ferromagnet, biosensor, Magnetic electron device, supercapacitor and lithium electricity.
Although first-principles calculations further demonstrate that VS2It can be shown as anode material of lithium-ion battery excellent Chemical property, but will experiment preparation VS2The report for being directly used as anode material of lithium-ion battery is seldom.In addition, In VS2As in the cyclic process of lithium ion battery electrode material, VS2Volume expansion will cause its dusting, then substantially reduce Its chemical property.When by VS2When applied to sodium-ion battery, since sodium ion has the radius bigger than lithium ion, this Kind volume expansion will become apparent.
Currently, alleviating volume expansion then improves VS2The main method of chemical property be with graphene, carbon nanotube and The Material claddings such as organic polymer.However, these materials are to VS2The inhibition of volume expansion only occurs in the direction of contact point On, resulting in inapparent chemical property improves.In addition, these materials needs are prepared separately or buy, can make entirely to synthesize Process becomes complicated, inefficient and Gao Chengben.
Therefore, efficient, simple and inexpensive method is explored, to inhibit VS2Volume expansion, with finally promoted its store up sodium Performance is to be highly desirable, and significantly.
[summary of the invention]
The purpose of the present invention is to provide the VS that a kind of efficient, simple and inexpensive preparation has excellent storage sodium performance2It is negative Pole material, in particular to a kind of VS of VOOH cladding2The preparation method and applications of nanometer sheet, this method use a step water at low temperature Heat is in VS2Nanometer sheet surface in situ grown VOOH, and this method reaction process is simple, and reaction temperature is low, and does not need large size Equipment and harsh reaction condition.
The invention adopts the following technical scheme:
A kind of preparation method of the vanadium disulfide nanometer sheet of hydroxide vanadyl cladding, rubs according to the vanadium sulphur of 1:2.5~1:3.5 Sodium metavanadate and thioacetamide are dissolved in deionized water, stirring to half clear state by that ratio simultaneously；Then hydro-thermal is carried out Reaction, hydro-thermal reaction carries out under rotation condition, to guarantee hydroxide vanadyl in the homoepitaxial on vanadium disulfide surface.
Before hydro-thermal reaction occurs, pH will be reacted with ammonium hydroxide and will be adjusted to 10.3~10.5.
The process for adjusting pH is to adjust dropwise, i.e., stirs after one drop ammonium hydroxide of addition and do not change to pH value of solution, under being then added One drop ammonium hydroxide, until the last pH value of solution reaches 10.3~10.5.
It needs constantly to carry out magnetic agitation during adjusting pH.
The packing ratio of the hydro-thermal reaction is 55~65%, the detailed process of hydro-thermal reaction are as follows: by configured good mixing Solution pours into reaction liner, is then placed on liner after sealing in homogeneous reaction instrument loaded on fixation in outer kettle, then 5~ 15r/min, under conditions of 155~165 DEG C, 23~25h is reacted.
The washing is that alternately washing and alcohol is washed after taking out the product cooled down after hydro-thermal reaction；The drying temperature It is 55~65 DEG C, the time is 10~15h.
A kind of vanadium disulfide nanometer sheet of hydroxide vanadyl cladding, products therefrom is the VS of crystal VOOH cladding2Nanometer sheet.
After adjusting pH value of solution is 10.3~10.5 before hydro-thermal reaction, products therefrom is the VS of amorphous VOOH cladding2Nanometer Piece.
The nanometer sheet in self assembly micron it is flower-shaped, and nanometer sheet with a thickness of 30~50nm.
A kind of application of the vanadium disulfide nanometer sheet of hydroxide vanadyl cladding, the nanometer sheet are applied to the negative of sodium-ion battery Pole material, the anode material of lithium-ion battery show excellent chemical property, 100,200,500,1000,2000, 5000mAg-1Current density under, show up to 384,364,316,224,140,113mAhg-1Specific capacity；? 200mAg-1Current density under, circulation 150 circle after still maintain 330mAhg-1Specific capacity, capacity retention ratio is up to 94%.
Compared with the existing technology, the present invention at least has the advantages that
The present invention is prepared for the VS of VOOH cladding using a step low-temperature hydrothermal synthetic method for the first time2Nanometer sheet, and report for the first time Chemical property of this material as anode material of lithium-ion battery.Specifically have the beneficial effect that:
(1) this method is since it using a step hydro-thermal reaction directly synthesizes final product, thus has low synthesis Temperature, simple synthesis path do not need large scale equipment and harsh reaction condition, and raw material is cheap and easy to get, at low cost, yield Height is not necessarily to post-processing, environmentally friendly, can be suitble to be mass produced.
(2) this method is prepared for VS by a step hydro-thermal reaction simultaneously2With two kinds of materials of VOOH, and VOOH is to coat completely In VS2Nanometer sheet surface can limit volume expansion of the VS2 electrode material in charge and discharge process from more dimensions, To promote its cyclical stability.
(3) VS can be made by adjusting pH value in reaction using this method2Surface coats crystal VOOH and unformed The material of two kinds of VOOH of VOOH, and the VOOH of both claddings can promote VS2The chemical property of nanometer sheet.And due to crystal The structure of VOOH steady ordered, to VS2The promotion of nanometer sheet chemical property is more significant.When not adjusting solution ph, The VOOH of cladding is crystal structure, and when adjusting pH value of solution to 10.3~10.5 with ammonium hydroxide, the VOOH of cladding is undefined structure.
(4) VOOH is in addition to VS2Play the role of outside protection, there are also activate VS2The effect on nanometer sheet surface enables the surface VS2 Enough absorption/desorption sodium ions faster and more.
(5) this method simple process is easily-controllable, main control parameters be sodium metavanadate and thioacetamide concentration and proportion, Reaction temperature, time, packing ratio, pH value and stirring, core control parameter are pH value in reaction, and the control of these parameters is all easy In realization.This method takes full advantage of the characteristic of vanadium oxyphie in aqueous solution, passes through control reactant concentration and proportion, reaction The parameters such as temperature, time and pH, successfully synthesize VS2Later, it grown VOOH in its surface in situ.
(6) VS of the VOOH cladding of this method preparation2Nanometer sheet forms micro-flowers by way of self assembly, i.e., by thickness Degree is about that the nanometer sheet of 30~50nm is self-assembled into the micro-flowers that diameter is about 3~5um, VS2The surface coated VOOH of nanometer sheet Thickness is less than 10nm.This self assembly mode is very beneficial for carrying in the electrolyte free entry and exit of sodium ion, while also very Be conducive to electrolyte and VS2Nanometer sheet comes into full contact with, and can then greatly enhance its chemical property.
(7) the product chemistry composition of this method preparation is uniform, and purity is high, pattern is uniform, is used as sodium-ion battery electrode Excellent chemical property can be shown when material.
(8) in the synthesis process of material, VS2The formation of nanometer sheet surface VOOH, sufficiently inhibits VS2Nanometer sheet into One step growth, thus the nanometer sheet synthesized has lesser thickness, is conducive to the inside that sodium ion enters nanometer sheet, provides More storage sodium sites, are also beneficial to the smooth disengaging of sodium ion and electronics, so as to substantially improve chemical property.
[Detailed description of the invention]
Fig. 1 is the VS of crystal VOOH cladding prepared by the embodiment of the present invention 12X-ray diffraction (XRD) map of nanometer sheet；
Fig. 2 is the VS coated by crystal VOOH prepared by the embodiment of the present invention 12Nanometer sheet is self-assembled into the scanning of micro-flowers Electronic Speculum (SEM) photo.
Fig. 3 is the VS coated by crystal VOOH prepared by the embodiment of the present invention 12Nanometer sheet is self-assembled into the amplification of micro-flowers Scanning electron microscope (SEM) photo.
Fig. 4 is the VS coated by crystal VOOH prepared by the embodiment of the present invention 12Nanometer sheet is self-assembled into the transmission of micro-flowers Electronic Speculum (TEM) photo
Fig. 5 is the VS coated by crystal VOOH prepared by the embodiment of the present invention 12The high-resolution-ration transmission electric-lens of nanometer sheet (HRTEM) photo.
Fig. 6 is the VS coated by crystal VOOH prepared by the embodiment of the present invention 12Nanometer sheet transmits element energy spectrum diagram (STEM- ) and scan element energy spectrum diagram (SEM-EDS) EDS.
[specific embodiment]
Invention is further described in detail with reference to the accompanying drawings and embodiments.
A kind of VS of VOOH cladding2The preparation method of nanometer sheet, comprising the following steps:
Step 1: weighing sodium metavanadate and thioacetamide and is added in 55~65ml deionized water simultaneously, controls vanadium Sulphur molar ratio is 1:2.5~1:3.5, and 20~40min of magnetic agitation obtains half clear solution A, and the concentration of sodium metavanadate is at this time 0.1~0.15mol/L.
Solution A: being poured into sealing after reacting in liner by step 2, is then placed on liner homogeneously loaded on fixed in outer kettle It reacts in instrument, then under conditions of 5~15r/min, 23~25h is reacted at 155~165 DEG C.Wherein reaction-filling ratio is answered The control is 55~65%.The progress of the reaction must carry out under rotation condition, be conducive to the full and uniform of reactant in this way Contact, thereby may be ensured that VOOH in VS2The homoepitaxial on surface.
Step 3: hydro-thermal reaction terminates, and reaction kettle is naturally cooled to room temperature, then takes the product cooled down after reaction Out, product is collected after 2~5 washings and 2~5 alcohol are alternately cleaned, and under the conditions of 55~65 DEG C, dries 10~15h, The VS of VOOH cladding can be obtained2Nanometer sheet.
A kind of VS of the VOOH cladding prepared by the above method2The application of nanometer sheet, the nanometer sheet are self-assembled into micron It is flower-shaped when being applied to sodium/lithium ion battery, excellent chemical property is shown, is existed as anode material of lithium-ion battery 100,200,500,1000,2000,5000mAg-1Current density under, show up to 384,364,316,224,140, 113mAhg-1Specific capacity.In 200mAg-1Current density under, first charge-discharge capacity can achieve 364 Hes 442mAhg-1, circulation 150 are still able to maintain 330mAhg after enclosing-1Specific capacity, capacity retention ratio is up to 94%.
Embodiment 1
Step 1: weighing sodium metavanadate and thioacetamide and is added in 60ml deionized water simultaneously, and control vanadium sulphur rubs You are than obtaining half clear solution A for 1:3.0, magnetic agitation 30min, and the concentration of sodium metavanadate is 0.137mol/L at this time.
Solution A: being poured into sealing after reacting in liner by step 2, is then placed on liner homogeneously loaded on fixed in outer kettle It reacts in instrument, then under conditions of 10r/min, is reacted for 24 hours at 160 DEG C.Wherein reaction-filling ratio should be controlled 60%.
Step 3: hydro-thermal reaction terminates, and reaction kettle is naturally cooled to room temperature, then takes the product cooled down after reaction Out, product is collected after 3 washings and 3 alcohol are alternately cleaned, and under the conditions of 60 DEG C, dries 12h, VOOH packet can be obtained The VS covered2Nanometer sheet.
From figure 1 it appears that X-ray powder diffraction peak has been directed toward VS simultaneously2And VOOH, therefore embodiment 1 is synthesis VOOH cladding VS2Nanometer sheet.
It can understand to see the VS of VOOH cladding from Fig. 22It is flower-shaped that nanometer sheet has been self-assembled into micron, and micro-flowers Diameter be about 3um.
This it appears that the VS of VOOH cladding from Fig. 32The thickness of nanometer sheet is about 30~50nm.
It can be it is also seen that the VS coated by VOOH from Fig. 42Nanometer sheet self assembly micron flower-like structure.
Can more intuitively it find out from Fig. 5, VS2Nanometer sheet surface has coated a layer crystal body VOOH.
From fig. 6, it can be seen that element S is apparently higher than its peak intensity in STEM-EDS spectrum, meaning in the peak intensity that SEM-EDS is composed Taste the substance that is detected of STEM-EDS be not VS2But VOOH, the investigative range in conjunction with STEM-EDS are < 10nm, therefore It is coated on VS2The thickness of the crystal VOOH on nanometer sheet surface is less than 10nm.
Embodiment 2
Step 1: weighing sodium metavanadate and thioacetamide and is added in 55ml deionized water simultaneously, and control vanadium sulphur rubs You are than obtaining half clear solution A for 1:2.5, magnetic agitation 20min, and the concentration of sodium metavanadate is 0.1mol/L at this time.
Solution A: being poured into sealing after reacting in liner by step 2, is then placed on liner homogeneously loaded on fixed in outer kettle It reacts in instrument, then under conditions of 5r/min, reacts 23h at 155 DEG C.
Step 3: hydro-thermal reaction terminates, and reaction kettle is naturally cooled to room temperature, then takes the product cooled down after reaction Out, product is collected after 2 washings and 5 alcohol are alternately cleaned, and under the conditions of 55 DEG C, dries 10h, VOOH packet can be obtained The VS covered2Nanometer sheet.
Embodiment 3
Step 1: weighing sodium metavanadate and thioacetamide and is added in 55~65ml deionized water simultaneously, controls vanadium Sulphur molar ratio is 1:3.2, and magnetic agitation 35min obtains half clear solution A, and the concentration of sodium metavanadate is 0.12mol/L at this time.
Solution A: being poured into sealing after reacting in liner by step 2, is then placed on liner homogeneously loaded on fixed in outer kettle It reacts in instrument, then under conditions of 12r/min, reacts 24.5h at 162 DEG C.
Step 3: hydro-thermal reaction terminates, and reaction kettle is naturally cooled to room temperature, then takes the product cooled down after reaction Out, product is collected after 4 washings and 4 alcohol are alternately cleaned, and under the conditions of 62 DEG C, dries 14h, VOOH packet can be obtained The VS covered2Nanometer sheet.
Embodiment 4
Step 1: weighing sodium metavanadate and thioacetamide and is added in 55~65ml deionized water simultaneously, controls vanadium Sulphur molar ratio is 1:3.5, and magnetic agitation 40min obtains half clear solution A, and the concentration of sodium metavanadate is 0.15mol/L at this time.
Solution A: being poured into sealing after reacting in liner by step 2, is then placed on liner homogeneously loaded on fixed in outer kettle It reacts in instrument, then under conditions of 15r/min, reacts 25h at 165 DEG C.
Step 3: hydro-thermal reaction terminates, and reaction kettle is naturally cooled to room temperature, then takes the product cooled down after reaction Out, product is collected after 5 washings and 5 alcohol are alternately cleaned, and under the conditions of 65 DEG C, dries 15h, VOOH packet can be obtained The VS covered2Nanometer sheet.

Claims (6)

1. a kind of preparation method of the vanadium disulfide nanometer sheet of hydroxide vanadyl cladding, which is characterized in that according to 1:2.5~1: Sodium metavanadate and thioacetamide are dissolved in deionized water, stirring to half clear state by 3.5 vanadium sulphur molar ratio simultaneously； Then hydro-thermal reaction is carried out, hydro-thermal reaction carries out under rotation condition, to guarantee hydroxide vanadyl in the equal of vanadium disulfide surface Even growth；
Before hydro-thermal reaction occurs, pH will be reacted with ammonium hydroxide and will be adjusted to 10.3~10.5, the process for adjusting pH is to adjust dropwise, It stirs after one drop ammonium hydroxide of addition and does not change to pH value of solution, next drop ammonium hydroxide is then added, until the last pH value of solution reaches 10.3~10.5, magnetic agitation is constantly carried out during adjusting pH；
The packing ratio of the hydro-thermal reaction is 55~65%, the detailed process of hydro-thermal reaction are as follows: by prepared mixed solution It pours into reaction liner, is then placed on liner after sealing in homogeneous reaction instrument loaded on fixation in outer kettle, then in 5~15r/ Min, under conditions of 155~165 DEG C, 23~25h is reacted.
2. a kind of preparation method of the vanadium disulfide nanometer sheet of hydroxide vanadyl cladding according to claim 1, feature It is, the product cooled down after hydro-thermal reaction is taken out, washed, dried；The washing is the production that will be cooled down after hydro-thermal reaction Alternately washing and alcohol is washed after object takes out；The drying temperature is 55~65 DEG C, and the time is 10~15h.
3. a kind of a kind of vanadium disulfide nanometer sheet of hydroxide vanadyl cladding based on the preparation of claim 1 the method, special Sign is that products therefrom is the VS of crystal VOOH cladding2Nanometer sheet.
4. a kind of vanadium disulfide nanometer sheet of hydroxide vanadyl cladding according to claim 3, it is characterised in that: in hydro-thermal After adjusting pH value of solution is 10.3~10.5 before reaction, products therefrom is the VS of amorphous VOOH cladding2Nanometer sheet.
5. a kind of vanadium disulfide nanometer sheet of hydroxide vanadyl cladding according to claim 3 or 4, it is characterised in that: institute State nanometer sheet in self assembly micron it is flower-shaped, and nanometer sheet with a thickness of 30~50nm.
6. a kind of application of the vanadium disulfide nanometer sheet of the hydroxide vanadyl cladding of method according to claim 11 preparation, It is characterized in that, the nanometer sheet is applied to the negative electrode material of sodium-ion battery, and the anode material of lithium-ion battery, 100,200, 500,1000,2000,5000mAg-1Current density under, show 384,364,316,224,140,113mAhg-1Specific volume Amount；In 200mAg-1Current density under, circulation 150 circle after keep 330mAhg-1Specific capacity, capacity retention ratio 94%.
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