CN105819507A - Preparation method and application of nanosheet self-assembled microflower-shaped VS2 - Google Patents
Preparation method and application of nanosheet self-assembled microflower-shaped VS2 Download PDFInfo
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- CN105819507A CN105819507A CN201610285755.XA CN201610285755A CN105819507A CN 105819507 A CN105819507 A CN 105819507A CN 201610285755 A CN201610285755 A CN 201610285755A CN 105819507 A CN105819507 A CN 105819507A
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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 invention provides a preparation method and application of nanosheet self-assembled microflower-shaped VS2. The preparation method comprises the steps that firstly, the pH of a vanadium source solution and the pH of a sulfur source solution are regulated to be 11-14 under the magnetic stirring state through a sodium hydroxide solution; secondly, the solutions are poured into a reaction inner lining, the inner lining is contained in an outer kettle and fixed, and then the outer kettle is placed in a homogeneous reaction instrument; finally, a product obtained after a reaction is cooled, washed, collected and dried, and then the nanosheet self-assembled microflower-shaped VS2 can be obtained. The technology of the method is simple and easy to control, and the prepared nanosheet self-assembled microflower-shaped VS2 is uniform in chemical constitution and high in purity, has a specific self-assembled structure and shows the excellent electrochemical property when the nanosheet self-assembled microflower-shaped VS2 serves as a lithium-sodium ion battery electrode material. In addition, the method has the advantages that the defect that a traditional calcination method is high in temperature is overcome, large equipment and harsh reaction conditions are not needed, the raw materials are cheap and easy to obtain, the cost is low, the yield is high, aftertreatment is not needed, and the method is friendly to the environment and can be suitable for large-scale production.
Description
[technical field]
The present invention relates to the preparation method of a kind of transient metal sulfide, be specifically related to a kind of nanometer sheet flower-shaped VS of self assembly micron2Preparation method and application.
[background technology]
The inorganic compound such as many metal-oxide, phosphoric acid salt, phyllosilicate, disulphide have the layer structure being similar to graphite.With power effect between Van der Waals force equimolecular between these compound layers, and the atom on laminate interacts with strong covalent bond, and we are called intercalation compound.By opening the thinking preparing single-layer graphene in stripping method, Zhang Hua seminar of Nanyang Technological University finds, by lithium ion inserts stratiform disulphide block materials interlayer, it is also possible to separate monolayer disulphide material, and the MoS of monolayer2、WS2、VS2、SnS2Etc. having the dilute distinctive bulk effect of graphite, skin effect, quantum tunneling effect and quantum size effect, can be used for some field [ZengZ with specific function and property, SunT, ZhuJ, etal.Aneffectivemethodforthefabricationoffew-layer-thick inorganicnanosheets. [J] .AngewandteChemie, 2012,124 (36): 9,052 9056.].
Laminate sulfide has embedding and the abjection of bigger interlamellar spacing, beneficially lithium ion or sodium ion, is particularly combined the graphene composite material of high conductivity, reveals preferable performance at lithium ion or sodium ion context table storage.Due to they there is bigger interlamellar spacing, reducing metal ions is lower valency storage lithium (sodium) ability and the existence of interlayer hydrogen bond, the transient metal sulfides such as molybdenum, tungsten and vanadium be a comparatively ideal lithium ion of analogy and anode material of lithium-ion battery [Zhai Baihua. the synthesis of sulfide composite and storage lithium (sodium) performance study [D] thereof. Hunan University, 2014].
Current research is concentrated mainly on molybdenum sulfide and the chemical property of tungsten sulfide nano material.And research about vanadium disulfide chemical property is little, only report VS2/ graphene nanocomposite material and VS2Cladding Na2Ti2O5The report of nano wire etc..Therefore, research VS2Hydro-thermal controllable method for preparing and chemical property be significantly.
[summary of the invention]
It is an object of the invention to provide a kind of nanometer sheet flower-shaped VS of self assembly micron2Preparation method and application, the method use low-temperature hydrothermal synthetic method prepare the nanometer sheet flower-shaped VS of self assembly micron2, to overcome the shortcoming that conventional calcination method temperature is high, and need not main equipment and harsh reaction condition.
To achieve these goals, the present invention adopts the following technical scheme that
A kind of nanometer sheet flower-shaped VS of self assembly micron2Preparation method, according to the vanadium sulfur mol ratio of 1:1～1:6, vanadium source solution and sulfur source solution are mixed, stirring is to half clear state, and now the concentration in vanadium source is 0.1～0.5mol/L；Regulate its pH to carrying out hydro-thermal reaction after alkalescence, finally by the product cooling after hydro-thermal reaction, washes clean, collect, be dried,.
Further, described regulation pH uses sodium hydroxide solution, ammonia or potassium hydroxide solution to alkalescence.
Further, the pH value of described alkalescence is 11～14.
Further, need constantly to be stirred during regulation pH；Described stirring is magnetic agitation.
Further, described hydrothermal reaction process is: the solution that pH is adjusted to alkalescence is poured in reaction liner, and liner is loaded in outer still fixing being placed in homogeneous reaction instrument then, then under conditions of 5～50r/min, 120～200 DEG C, reacts 6～48h.
Further, described washing is to wash carrying out washing successively after the product cooled down after hydro-thermal reaction taking-up with alcohol.
Further, described baking temperature is 40～120 DEG C, and the time is 12～48h.
Further, described vanadium source is one or more in vanadic acid sodium, ammonium metavanadate, vanadic anhydride and potassium metavanadate；Described sulfur source is one or more in thioacetamide, sodium sulfide, ammonium sulfide, sodium oiethyl dithiocarbamate and sulfur simple substance.
A kind of nanometer sheet flower-shaped VS of self assembly micron prepared by above-mentioned method2Application, this nanometer sheet flower-shaped VS of self assembly micron2It is applied to the negative material of sodium/lithium ion battery.
This sodium/lithium ion battery negative material is under the electric current density of 50mA/g, and after specific capacity reaches 900mAh/g, and circulation 10 circle, its capability retention reaches 90%.
Relative to prior art, the present invention at least has the advantages that
The present invention uses low-temperature hydrothermal synthetic method to be prepared for the nanometer sheet flower-shaped VS of self assembly micron2, the method overcoming the shortcoming that conventional calcination method temperature is high, and need not main equipment and harsh reaction condition, cheaper starting materials is easy to get, low cost, and productivity is high, it is not necessary to the later stage processes, environmentally friendly, can be suitable for large-scale production.Meanwhile, the method technique is simple and easy to control, the nanometer sheet flower-shaped VS of self assembly micron of preparation2Chemical composition is homogeneous, and purity is higher, shows the chemical property of excellence when it is as lithium/sodium ion battery electrode material.Additionally, the vanadium disulfide nanometer prepared by the method has special self-assembled structures, i.e. it is self-assembled into, by the nanometer sheet of thickness about 30nm, the micro-flowers that diameter is about 4um.
[accompanying drawing explanation]
Fig. 1 is the nanometer sheet flower-shaped VS of self assembly micron of the embodiment of the present invention 1 preparation2X-ray diffraction (XRD) collection of illustrative plates；
Fig. 2 is the nanometer sheet flower-shaped VS of self assembly micron of the embodiment of the present invention 1 preparation2Scanning electron microscope (SEM) photo.
[detailed description of the invention]
Below in conjunction with the accompanying drawings and the present invention is described in further detail by embodiment.
A kind of nanometer sheet flower-shaped VS of self assembly micron2Preparation method, comprise the following steps:
Step one: weigh vanadium source and sulfur source and be dissolved in deionized water, controlling vanadium sulfur mol ratio is 1:1～1:6, and magnetic agitation 10～60min obtains half settled solution A, and now the concentration in vanadium source is 0.1～0.5mol/L.Vanadium source is one or more in vanadic acid sodium, ammonium metavanadate, vanadic anhydride and potassium metavanadate；Sulfur source is one or more in thioacetamide, sodium sulfide, ammonium sulfide, sodium oiethyl dithiocarbamate and sulfur simple substance.
Step 2: the sodium hydroxide solution B of preparation 1～4mol/L, then drips solution B in solution A, until solution ph reaches 11～14, obtains solution C.Need solution A is constantly carried out magnetic agitation in the process, and pH value don't fail to control between 11～14, so can control sulfur and v element existence in the solution, and then realize redox reaction control.Described sodium hydroxide solution can substitute with ammonia or potassium hydroxide solution.
Step 3: solution C poured in reaction liner, is loaded in outer still fixing being placed in homogeneous reaction instrument then by liner, then under conditions of 5～50r/min, reacts 6～48h at 120～200 DEG C.The carrying out of this reaction must be carried out under the conditions of rotating, and is so conducive to the full and uniform contact of reactant, thereby may be ensured that element sulphur fully plays reduction and provides S2-Effect.
Step 4: taken out by the product cooled down after reaction, collects product after 3～8 washings and 3～8 alcohol are washed, and under the conditions of 40～120 DEG C, dries 12～48h, i.e. can get the nanometer sheet flower-shaped VS of self assembly micron2。
A kind of nanometer sheet flower-shaped VS of self assembly micron prepared by said method2Application, this nanometer sheet flower-shaped VS of self assembly micron2When being applied to sodium/lithium ion battery, showing the chemical property of excellence, it is as anode material of lithium-ion battery under the electric current density of 50mA/g, and specific capacity can reach 900mAh/g, and after circulating 10 circles, capability retention is more than 90%.Additionally, under the electric current density of 100mA/g, specific capacity still can reach 800mAh/g.
Embodiment 1
Step one: weigh sodium metavanadate and thioacetamide and be dissolved in deionized water, controlling vanadium sulfur mol ratio is 1:1, and magnetic agitation 10min obtains half settled solution A, and now the concentration in vanadium source is 0.2mol/L.
Step 2: the sodium hydroxide solution B of preparation 3mol/L, then drips solution B in solution A, until solution ph reaches 13, obtains solution C.Need solution A is constantly carried out magnetic agitation in the process.
Step 3: solution C poured in reaction liner, is loaded in outer still fixing being placed in homogeneous reaction instrument then by liner, then under conditions of 10r/min, reacts 24h at 160 DEG C.
Step 4: taken out by the product cooled down after reaction, collects product after 3 washings and 3 alcohol are washed, and under the conditions of 60 DEG C, dries 12h, i.e. can get the nanometer sheet flower-shaped VS of self assembly micron2。
From figure 1 it appears that all of X-ray powder diffraction peak can index be all the nanometer sheet flower-shaped VS of self assembly micron2, and occur almost without other impurity peaks, therefore embodiment 1 is the high-purity nano-sheet flower-shaped VS of self assembly micron of synthesis2。
Can understand to see that the nanometer sheet of thickness about 30nm is self-assembled into the micro-flowers that diameter is about 4um from Fig. 2.
Embodiment 2
Step one: weigh sodium metavanadate and thioacetamide and be dissolved in deionized water, controlling vanadium sulfur mol ratio is 1:3, and magnetic agitation 20min obtains half settled solution A, and now the concentration in vanadium source is 0.1mol/L.
Step 2: the sodium hydroxide solution B of preparation 1mol/L, then drips solution B in solution A, until solution ph reaches 11, obtains solution C.Need solution A is constantly carried out magnetic agitation in the process.
Step 3: solution C poured in reaction liner, is loaded in outer still fixing being placed in homogeneous reaction instrument then by liner, then under conditions of 5r/min, reacts 6h at 120 DEG C.
Step 4: taken out by the product cooled down after reaction, collects product after 4 washings and 4 alcohol are washed, and under the conditions of 40 DEG C, dries 18h, i.e. can get the nanometer sheet flower-shaped VS of self assembly micron2。
Embodiment 3
Step one: weigh sodium metavanadate and thioacetamide and be dissolved in deionized water, controlling vanadium sulfur mol ratio is 1:5, and magnetic agitation 30min obtains half settled solution A, and now the concentration in vanadium source is 0.4mol/L.
Step 2: the sodium hydroxide solution B of preparation 2mol/L, then drips solution B in solution A, until solution ph reaches 12, obtains solution C.Need solution A is constantly carried out magnetic agitation in the process.
Step 3: solution C poured in reaction liner, is loaded in outer still fixing being placed in homogeneous reaction instrument then by liner, then under conditions of 30r/min, reacts 36h at 140 DEG C.
Step 4: taken out by the product cooled down after reaction, collects product after 5 washings and 5 alcohol are washed, and under the conditions of 100 DEG C, dries 36h, i.e. can get the nanometer sheet flower-shaped VS of self assembly micron2。
Embodiment 4
Step one: weigh sodium metavanadate and thioacetamide and be dissolved in deionized water, controlling vanadium sulfur mol ratio is 1:6, and magnetic agitation 60min obtains half settled solution A, and now the concentration in vanadium source is 0.5mol/L.
Step 2: the sodium hydroxide solution B of preparation 4mol/L, then drips solution B in solution A, until solution ph reaches 14, obtains solution C.Need solution A is constantly carried out magnetic agitation in the process.
Step 3: solution C poured in reaction liner, is loaded in outer still fixing being placed in homogeneous reaction instrument then by liner, then under conditions of 50r/min, reacts 48h at 200 DEG C.
Step 4: taken out by the product cooled down after reaction, collects product after 8 washings and 8 alcohol are washed, and under the conditions of 120 DEG C, dries 48h, i.e. can get the nanometer sheet flower-shaped VS of self assembly micron2。
Relative to prior art, the present invention at least has the advantages that
The present invention uses low-temperature hydrothermal synthetic method to be prepared for the nanometer sheet flower-shaped VS of self assembly micron2, the method overcoming the shortcoming that conventional calcination method temperature is high, and need not main equipment and harsh reaction condition, cheaper starting materials is easy to get, low cost, and productivity is high, it is not necessary to the later stage processes, environmentally friendly, can be suitable for large-scale production.Meanwhile, the method technique is simple and easy to control, the nanometer sheet flower-shaped VS of self assembly micron of preparation2Chemical composition is homogeneous, and purity is higher, shows the chemical property of excellence when it is as lithium/sodium ion battery electrode material, its as anode material of lithium-ion battery under the electric current density of 50mA/g, specific capacity can reach 900mAh/g, and after circulating 10 circles, capability retention is more than 90%.Under the electric current density of 100mA/g, specific capacity still can reach 800mAh/g.Additionally, the vanadium disulfide nano material prepared by the method has special self-assembled structures, i.e. it is self-assembled into, by the nanometer sheet of thickness about 30nm, the micro-flowers that diameter is about 4um.
Claims (10)
1. the nanometer sheet flower-shaped VS of self assembly micron2Preparation method, it is characterised in that according to the vanadium sulfur mol ratio of 1:1～1:6, vanadium source solution and sulfur source solution being mixed, stirring is to half clear state, and now the concentration in vanadium source is 0.1～0.5mol/L；Regulate its pH to carrying out hydro-thermal reaction after alkalescence, finally by the product cooling after hydro-thermal reaction, washes clean, collect, be dried,.
A kind of nanometer sheet flower-shaped VS of self assembly micron the most according to claim 12Preparation method, it is characterised in that described regulation pH uses sodium hydroxide solution, ammonia or potassium hydroxide solution to alkalescence.
A kind of nanometer sheet flower-shaped VS of self assembly micron the most according to claim 1 and 22Preparation method, it is characterised in that the pH value of described alkalescence is 11～14.
A kind of nanometer sheet flower-shaped VS of self assembly micron the most according to claim 1 and 22Preparation method, it is characterised in that regulation pH during need constantly to be stirred；Described stirring is magnetic agitation.
A kind of nanometer sheet flower-shaped VS of self assembly micron the most according to claim 12Preparation method, it is characterized in that, described hydrothermal reaction process is: the solution that pH is adjusted to alkalescence is poured in reaction liner, and liner is loaded in outer still fixing being placed in homogeneous reaction instrument then, then, under conditions of 5～50r/min, 120～200 DEG C, 6～48h are reacted.
A kind of nanometer sheet flower-shaped VS of self assembly micron the most according to claim 12Preparation method, it is characterised in that described washing be by the product cooled down after hydro-thermal reaction take out after successively carry out washing and alcohol wash.
A kind of nanometer sheet flower-shaped VS of self assembly micron the most according to claim 12Preparation method, it is characterised in that described baking temperature is 40～120 DEG C, and the time is 12～48h.
8. according to any one nanometer sheet flower-shaped VS of self assembly micron described in claim 1-72Preparation method, it is characterised in that described vanadium source is one or more in vanadic acid sodium, ammonium metavanadate, vanadic anhydride and potassium metavanadate；Described sulfur source is one or more in thioacetamide, sodium sulfide, ammonium sulfide, sodium oiethyl dithiocarbamate and sulfur simple substance.
9. the nanometer sheet flower-shaped VS of self assembly micron that prepared by a method according to claim 12Application, it is characterised in that this nanometer sheet flower-shaped VS of self assembly micron2It is applied to the negative material of sodium/lithium ion battery.
The nanometer sheet flower-shaped VS of self assembly micron the most according to claim 92Application, it is characterised in that this anode material of lithium-ion battery is under the electric current density of 50mA/g, and specific capacity reaches 900mAh/g, and after circulation 10 circle, its capability retention reaches 90%.
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| CN106430306A (en) * | 2016-08-30 | 2017-02-22 | 南开大学 | Preparation method for vanadium dioxide micro-nanometer structure material |
| CN107221646A (en) * | 2017-07-13 | 2017-09-29 | 陕西科技大学 | A kind of vanadium disulfide nanometer sheet of hydroxide vanadyl cladding and its preparation method and application |
| CN107482161A (en) * | 2017-08-25 | 2017-12-15 | 武汉理工大学 | Graphene modified vanadium disulfide micron floral material and preparation method thereof and the application as aluminium ion cell positive material |
| CN107840368A (en) * | 2017-11-21 | 2018-03-27 | 陕西科技大学 | A kind of nanometer sheet self assembly sub-micrometer flower-shape M-phase vanadium dioxide powder and preparation method thereof |
| CN107902697A (en) * | 2017-11-02 | 2018-04-13 | 陕西科技大学 | A kind of nanometer sheet self assembled three-dimensional VS of (001) orientation2Micron bar and preparation method thereof |
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| CN108550829A (en) * | 2018-05-10 | 2018-09-18 | 中南大学 | One kind having rose shape vanadium disulfide/carbon quantum dot composite material and preparation method and application |
| CN108585042A (en) * | 2018-07-02 | 2018-09-28 | 陕西科技大学 | A kind of extra small flower-shaped VS of nanometer sheet self assembly2Powder and preparation method thereof |
| CN108821348A (en) * | 2018-09-17 | 2018-11-16 | 陕西科技大学 | A kind of cobalt sulfide nanometer sheet material and preparation method thereof |
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