CN105819507B - A kind of flower-shaped VS of nanometer sheet self assembly micron2Preparation method and application - Google Patents
A kind of flower-shaped VS of nanometer sheet self assembly micron2Preparation method and application Download PDFInfo
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
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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 present invention provides a kind of flower-shaped VS of nanometer sheet self assembly micron2Preparation method and application, vanadium source solution and sulphur source solution are passed through into sodium hydroxide solution under magnetic agitation state and adjust pH value of solution to 11~14.Then, above-mentioned solution is poured into reaction liner, is then placed on liner in homogeneous reaction instrument loaded on fixation in outer kettle.Finally, by washing, collection, drying after the product cooling after reaction, you can obtain the flower-shaped VS of nanometer sheet self assembly micron2.This method is simple for process easily-controllable, the flower-shaped VS of nanometer sheet self assembly micron of preparation2Chemical composition is uniform, and purity is higher, and has specific self-assembled structures, and excellent chemical property is shown when as lithium/sodium ion battery electrode material.In addition, the method overcome the high disadvantages of conventional calcination method temperature, and do not need large scale equipment and harsh reaction condition, raw material is cheap and easy to get, at low cost, and yield is high, is not necessarily to post-processing, environmentally friendly, can be suitble to mass produce.
Description
【Technical field】
The present invention relates to a kind of preparation methods of transient metal sulfide, and in particular to a kind of nanometer sheet self assembly micro-flowers
Shape VS2Preparation method and application.
【Background technology】
The inorganic compounds such as many metal oxides, phosphoric acid salt, phyllosilicate, disulphide, which have, is similar to graphite
Layer structure.With force effect between Van der Waals force equimolecular between these compound layers, and the atom on laminate is with strong covalent
Key interacts, we are called intercalation compound.Opened the thinking that single-layer graphene is prepared in stripping method, Singapore's Nan Yang reason
Zhang Hua seminars of work university find, by the way that lithium ion is inserted into stratiform disulphide block materials interlayer, can also separate list
Layer disulphide material, and the MoS of single layer2、WS2、VS2、SnS2Deng with the dilute distinctive bulk effect of graphite, skin effect, amount
Sub- tunnel-effect and quantum size effect, can be used for some with specific function and property field [Zeng Z, Sun T,
Zhu J,et al.An effective method for the fabrication of few-layer-thick
inorganic nanosheets.[J].Angewandte Chemie, 2012,124(36):9052–9056.]。
Laminate sulfide has bigger interlamellar spacing, is conducive to the insertion and abjection of lithium ion or sodium ion, especially multiple
The graphene composite material for closing high conductivity, reveals preferable performance in lithium ion or sodium ion context table storage.Due to them
The presence of lower valency storage lithium (sodium) ability and interlayer hydrogen bond, molybdenum, tungsten and vanadium are reduced to larger interlamellar spacing, metal ion
Equal transient metal sulfides are that [uncle Zhai China sulfide is compound for a kind of more satisfactory lithium ion and anode material of lithium-ion battery
The synthesis of material and its storage lithium (sodium) performance study [D] Hunan University, 2014].
Current research is concentrated mainly on the chemical property of molybdenum sulfide and tungsten sulfide nano material.And about vanadium disulfide
The research of chemical property is seldom, only reports VS2/ graphene nanocomposite material and VS2Coat Na2Ti2O5Nano wire
Deng report.Therefore, VS is studied2Hydro-thermal controllable method for preparing and its chemical property be significantly.
【Invention content】
The purpose of the present invention is to provide a kind of flower-shaped VS of nanometer sheet self assembly micron2Preparation method and application, the party
Method prepares the flower-shaped VS of nanometer sheet self assembly micron using low-temperature hydrothermal synthetic method2, to overcome conventional calcination method temperature is high to lack
Point, and do not need large scale equipment and harsh reaction condition.
To achieve the goals above, the present invention adopts the following technical scheme that：
A kind of flower-shaped VS of nanometer sheet self assembly micron2Preparation method, according to 1:1~1:6 vanadium sulphur molar ratio, by vanadium source
Solution and the mixing of sulphur source solution, are stirred to half clear state, the concentration in vanadium source is 0.1~0.5mol/L at this time；Adjust its pH to
Hydro-thermal reaction is carried out after alkalinity, finally by product cooling, washes clean, collection, the drying after hydro-thermal reaction, you can.
Further, the adjusting pH uses sodium hydroxide solution, ammonium hydroxide or potassium hydroxide solution to alkaline.
Further, the pH value of the alkalinity is 11~14.
Further, it needs constantly to be stirred during adjusting pH；The stirring is magnetic agitation.
Further, the hydrothermal reaction process is：The solution that pH is adjusted to alkalinity pours into reaction liner, then will be interior
Lining is placed on loaded on fixation in outer kettle in homogeneous reaction instrument, then under conditions of 5~50r/min, 120~200 DEG C, reaction 6
~48h.
Further, the washing is to carry out washing and alcohol successively after taking out the product of hydro-thermal reaction postcooling to wash.
Further, the drying temperature is 40~120 DEG C, and the time is 12~48h.
Further, the vanadium source is one kind or several in sodium vanadate, ammonium metavanadate, vanadic anhydride and potassium metavanadate
Kind；The sulphur source is one kind in thioacetamide, vulcanized sodium, ammonium sulfide, sodium oiethyl dithiocarbamate and sulphur simple substance
Or it is several.
A kind of flower-shaped VS of nanometer sheet self assembly micron prepared by above-mentioned method2Application, the nanometer sheet self assembly
The flower-shaped VS of micron2Negative material applied to sodium/lithium ion battery.
For the sodium/lithium ion battery negative material under the current density of 50mA/g, specific capacity reaches 900mAh/g, and recycles 10
After circle, capacity retention ratio is up to 90%.
Compared with the existing technology, the present invention at least has the advantages that：
The present invention is prepared for the flower-shaped VS of nanometer sheet self assembly micron using low-temperature hydrothermal synthetic method2, the method overcome biographies
The high disadvantage of method for calcinating temperature of uniting, and large scale equipment and harsh reaction condition are not needed, raw material is cheap and easy to get, at low cost,
Yield is high, is not necessarily to post-processing, environmentally friendly, can be suitble to mass produce.Meanwhile this method is simple for process easily-controllable, system
The standby flower-shaped VS of nanometer sheet self assembly micron2Chemical composition is uniform, and purity is higher, is used as lithium/sodium ion battery electrode material
When show excellent chemical property.In addition, there is special self assembly by vanadium disulfide nanometer prepared by this method
Structure, i.e., the nanometer sheet for being about 30nm by thickness are self-assembled into the micro-flowers that diameter is about 4um.
【Description of the drawings】
Fig. 1 is the flower-shaped VS of nanometer sheet self assembly micron prepared by the embodiment of the present invention 12X-ray diffraction (XRD) collection of illustrative plates；
Fig. 2 is the flower-shaped VS of nanometer sheet self assembly micron prepared by the embodiment of the present invention 12Scanning electron microscope (SEM) photo.
【Specific implementation mode】
Invention is further described in detail with reference to the accompanying drawings and embodiments.
A kind of flower-shaped VS of nanometer sheet self assembly micron2Preparation method, include the following steps：
Step 1：It weighs vanadium source and sulphur source and is dissolved in deionized water, control vanadium sulphur molar ratio is 1:1~1:6, magnetic force stirs
It mixes 10~60min and obtains half clear solution A, the concentration in vanadium source is 0.1~0.5mol/L at this time.Vanadium source is sodium vanadate, metavanadic acid
One or more of ammonium, vanadic anhydride and potassium metavanadate；Sulphur source is thioacetamide, vulcanized sodium, ammonium sulfide, diethyl
One or more of thiocarbamic acid sodium and sulphur simple substance.
Step 2：The sodium hydroxide solution B for preparing 1~4mol/L, is then added dropwise solution B into solution A, until pH value of solution
Value reaches 11~14, obtains solution C.It needs constantly to carry out magnetic agitation to solution A in the process, and pH value don't fail to be controlled
System can control the existence of sulphur and v element in the solution, and then realize redox reaction in this way between 11~14
Control.The sodium hydroxide solution can use ammonium hydroxide or potassium hydroxide solution to substitute.
Step 3：Solution C is poured into reaction liner, liner is then placed on homogeneous reaction instrument loaded on fixation in outer kettle
In, then under conditions of 5~50r/min, 6~48h is reacted at 120~200 DEG C.The progress of the reaction must be in rotation strip
It is carried out under part, is conducive to the full and uniform contact of reactant in this way, thereby may be ensured that element sulphur fully plays reduction
With offer S2-Effect.
Step 4：The product for reacting postcooling is taken out, product is collected after 3~8 washings and 3~8 alcohol are washed, and
Under the conditions of 40~120 DEG C, 12~48h is dried, you can obtain the flower-shaped VS of nanometer sheet self assembly micron2。
A kind of flower-shaped VS of nanometer sheet self assembly micron prepared by the above method2Application, the nanometer sheet self assembly is micro-
Popped rice shape VS2When applied to sodium/lithium ion battery, excellent chemical property is shown, is used as sodium-ion battery cathode
Material is under the current density of 50mA/g, and specific capacity can reach 900mAh/g, and after 10 circle of cycle, capacity retention ratio exists
90% or more.In addition, under the current density of 100mA/g, specific capacity still can reach 800mAh/g.
Embodiment 1
Step 1：It weighs sodium metavanadate and thioacetamide and is dissolved in deionized water, control vanadium sulphur molar ratio is 1:1,
Magnetic agitation 10min obtains half clear solution A, and the concentration in vanadium source is 0.2mol/L at this time.
Step 2：The sodium hydroxide solution B for preparing 3mol/L, is then added dropwise solution B into solution A, until solution ph
Reach 13, obtains solution C.It needs constantly to carry out magnetic agitation to solution A in the process.
Step 3：Solution C is poured into reaction liner, liner is then placed on homogeneous reaction instrument loaded on fixation in outer kettle
In, then under conditions of 10r/min, reacted for 24 hours at 160 DEG C.
Step 4：The product for reacting postcooling is taken out, collects product after 3 washings and 3 alcohol are washed, and at 60 DEG C
Under the conditions of, dry 12h, you can obtain the flower-shaped VS of nanometer sheet self assembly micron2。
From figure 1 it appears that all X-ray powder diffraction peaks can refer to be designated as nanometer sheet self assembly micron it is flower-shaped
VS2, and occur almost without other impurity peaks, therefore the high-purity nano-sheet self assembly micron that embodiment 1 is synthesis is flower-shaped
VS2。
It can understand to see that the nanometer sheet that thickness is about 30nm is self-assembled into the micro-flowers that diameter is about 4um from Fig. 2.
Embodiment 2
Step 1：It weighs sodium metavanadate and thioacetamide and is dissolved in deionized water, control vanadium sulphur molar ratio is 1:3,
Magnetic agitation 20min obtains half clear solution A, and the concentration in vanadium source is 0.1mol/L at this time.
Step 2：The sodium hydroxide solution B for preparing 1mol/L, is then added dropwise solution B into solution A, until solution ph
Reach 11, obtains solution C.It needs constantly to carry out magnetic agitation to solution A in the process.
Step 3：Solution C is poured into reaction liner, liner is then placed on homogeneous reaction instrument loaded on fixation in outer kettle
In, then under conditions of 5r/min, react 6h at 120 DEG C.
Step 4：The product for reacting postcooling is taken out, collects product after 4 washings and 4 alcohol are washed, and at 40 DEG C
Under the conditions of, dry 18h, you can obtain the flower-shaped VS of nanometer sheet self assembly micron2。
Embodiment 3
Step 1：It weighs sodium metavanadate and thioacetamide and is dissolved in deionized water, control vanadium sulphur molar ratio is 1:5,
Magnetic agitation 30min obtains half clear solution A, and the concentration in vanadium source is 0.4mol/L at this time.
Step 2：The sodium hydroxide solution B for preparing 2mol/L, is then added dropwise solution B into solution A, until solution ph
Reach 12, obtains solution C.It needs constantly to carry out magnetic agitation to solution A in the process.
Step 3：Solution C is poured into reaction liner, liner is then placed on homogeneous reaction instrument loaded on fixation in outer kettle
In, then under conditions of 30r/min, react 36h at 140 DEG C.
Step 4：The product for reacting postcooling is taken out, collects product after 5 washings and 5 alcohol are washed, and at 100 DEG C
Under the conditions of, dry 36h, you can obtain the flower-shaped VS of nanometer sheet self assembly micron2。
Embodiment 4
Step 1：It weighs sodium metavanadate and thioacetamide and is dissolved in deionized water, control vanadium sulphur molar ratio is 1:6,
Magnetic agitation 60min obtains half clear solution A, and the concentration in vanadium source is 0.5mol/L at this time.
Step 2：The sodium hydroxide solution B for preparing 4mol/L, is then added dropwise solution B into solution A, until solution ph
Reach 14, obtains solution C.It needs constantly to carry out magnetic agitation to solution A in the process.
Step 3：Solution C is poured into reaction liner, liner is then placed on homogeneous reaction instrument loaded on fixation in outer kettle
In, then under conditions of 50r/min, react 48h at 200 DEG C.
Step 4：The product for reacting postcooling is taken out, collects product after 8 washings and 8 alcohol are washed, and 120
Under the conditions of DEG C, 48h is dried, you can obtain the flower-shaped VS of nanometer sheet self assembly micron2。
Compared with the existing technology, the present invention at least has the advantages that：
The present invention is prepared for the flower-shaped VS of nanometer sheet self assembly micron using low-temperature hydrothermal synthetic method2, the method overcome biographies
The high disadvantage of method for calcinating temperature of uniting, and large scale equipment and harsh reaction condition are not needed, raw material is cheap and easy to get, at low cost,
Yield is high, is not necessarily to post-processing, environmentally friendly, can be suitble to mass produce.Meanwhile this method is simple for process easily-controllable, system
The standby flower-shaped VS of nanometer sheet self assembly micron2Chemical composition is uniform, and purity is higher, is used as lithium/sodium ion battery electrode material
When show excellent chemical property, as anode material of lithium-ion battery under the current density of 50mA/g, specific volume
Amount can reach 900mAh/g, and after 10 circle of cycle, capacity retention ratio is 90% or more.In the current density of 100mA/g
Under, specific capacity still can reach 800mAh/g.In addition, the vanadium disulfide nano material prepared by this method is with special
Self-assembled structures, i.e., the nanometer sheet for being about 30nm by thickness are self-assembled into the micro-flowers that diameter is about 4um.
Claims (9)
1. a kind of flower-shaped VS of nanometer sheet self assembly micron2Preparation method, which is characterized in that according to 1:1~1:6 vanadium sulphur mole
Than, weigh vanadium source and sulphur source and be dissolved in deionized water, stirring to half clear state, at this time the concentration in vanadium source be 0.1~
0.5mol/L；Carry out hydro-thermal reaction after adjusting its pH value to alkalinity, finally by after hydro-thermal reaction product cooling, washes clean,
It collects, is dry, you can；The hydrothermal reaction process is：The solution that pH is adjusted to alkalinity pours into reaction liner, then by liner
It is placed in homogeneous reaction instrument loaded on fixation in outer kettle, then under conditions of 5~50r/min, 120~200 DEG C, reaction 6~
The pH value of 48h, the alkalinity are 11~14.
2. a kind of flower-shaped VS of nanometer sheet self assembly micron according to claim 12Preparation method, which is characterized in that it is described
It adjusts pH value to alkalinity and uses sodium hydroxide solution, ammonium hydroxide or potassium hydroxide solution.
3. a kind of flower-shaped VS of nanometer sheet self assembly micron according to claim 1 or 22Preparation method, which is characterized in that
It needs constantly to be stirred during adjusting pH value；The stirring is magnetic agitation.
4. a kind of flower-shaped VS of nanometer sheet self assembly micron according to claim 12Preparation method, which is characterized in that it is described
Washing is to carry out washing and alcohol successively after taking out the product of hydro-thermal reaction postcooling to wash.
5. a kind of flower-shaped VS of nanometer sheet self assembly micron according to claim 12Preparation method, which is characterized in that it is described
Drying temperature is 40~120 DEG C, and the time is 12~48h.
6. a kind of flower-shaped VS of nanometer sheet self assembly micron according to claims 1 or 2 or 4 or 52Preparation method, feature
It is, the vanadium source is one or more of sodium vanadate, ammonium metavanadate, vanadic anhydride and potassium metavanadate；The sulphur source
For one or more of thioacetamide, vulcanized sodium, ammonium sulfide, sodium oiethyl dithiocarbamate and sulphur simple substance.
7. a kind of flower-shaped VS of nanometer sheet self assembly micron according to claim 32Preparation method, which is characterized in that it is described
Vanadium source is one or more of sodium vanadate, ammonium metavanadate, vanadic anhydride and potassium metavanadate；The sulphur source is thioacetyl
One or more of amine, vulcanized sodium, ammonium sulfide, sodium oiethyl dithiocarbamate and sulphur simple substance.
8. the flower-shaped VS of nanometer sheet self assembly micron prepared by a kind of method according to claim 112Application, feature exists
In the flower-shaped VS of the nanometer sheet self assembly micron2Negative material applied to sodium-ion battery.
9. the flower-shaped VS of nanometer sheet self assembly micron according to claim 82Application, which is characterized in that the sodium-ion battery
Negative material is under the current density of 50mA/g, and specific capacity reaches 900mAh/g, and after 10 circle of cycle, capacity retention ratio reaches
90%.
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| CN102010004B (en) * | 2010-12-27 | 2012-05-30 | 中国科学技术大学 | Method for preparing vanadium disulphide nano powder |
| CN105226277A (en) * | 2015-09-10 | 2016-01-06 | 中国科学院上海硅酸盐研究所 | A kind of high-performance transition metal dichalcogenide nanometer sheet radial direction assembling micro-sphere material and preparation method thereof |
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