CN104393295B - A kind of preparation method of flower-shaped Wolfram disulfide nano particle - Google Patents
A kind of preparation method of flower-shaped Wolfram disulfide nano particle Download PDFInfo
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- CN104393295B CN104393295B CN201410695175.9A CN201410695175A CN104393295B CN 104393295 B CN104393295 B CN 104393295B CN 201410695175 A CN201410695175 A CN 201410695175A CN 104393295 B CN104393295 B CN 104393295B
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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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- 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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- 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 kind of preparation method of flower-shaped Wolfram disulfide nano particle, high temperature vulcanized synthetic method is used, step is as follows：By simple substance sulphur powder, thiocarbamide and WO3In molar ratio 10:10:1~20:20:It is fully ground after 1 mixing, the powder tablet press machine after grinding is depressed into a diameter of 25~30mm in the pressure of 25MPa~35Mpa, thickness is the disk of 4~6mm；The disk that will be suppressed is put into crucible, and crucible is pushed into tube furnace middle position；To being passed through argon gas in tube furnace, and tube furnace is brought rapidly up to 800~850 DEG C with the speed of 10~12 DEG C/min, and constant temperature processes 30~60 min；Then, room temperature is naturally cooled to, flower-shaped Wolfram disulfide nano particle is obtained.The inventive method process is simple, with low cost, the product purity for preparing is high, yield is high, is expected to be used for large-scale industrial production.
Description
Technical field
The present invention relates to field of inorganic materials, more particularly to a kind of preparation method of flower-shaped Wolfram disulfide nano particle.
Background technology
With the increasingly depleted of various resources such as oil, coal etc. on the earth, the various alternative energy sources of exploitation become the whole world and are permitted
The vital task of many research institutions.Along with the worsening shortages of petroleum resources, motor corporation has started various new-energy automobiles
Exploitation, electric automobile is exactly important a member therein.And it is battery to restrict the major reason that electric automobile promotes the use of at present
Finite capacity, vehicle driving mileage is limited after causing often to fill once electricity.Therefore, only develop that capacity is high, charge efficiency soon simultaneously
And the good batteries of electric automobile of security is possible to popularize electric automobile.Lithium ion battery is because with high power capacity and height
The features such as power, become the first-selection of batteries of electric automobile.Want to develop the lithium ion battery suitable for electric automobile, it is first-selected
The material of lithium ion battery is studied, including positive electrode, negative material and barrier film etc..Stratiform transient metal sulfide
The lithium ion battery negative material with very big potential is had proved to be, because they can be provided capacity and power density far surpassing
Cross conventional graphite.In these sulfide, the research that the molybdenum bisuphide with layer structure feature is carried out is concentrated the most.Respectively
The molybdenum bisuphide and its composite for planting different-shape have been used as lithium cell cathode material, while result of study also indicates that them
With very high power capacity and good cyclical stability.
It is another stratiform mistake for being well suited for and being stored for lithium ion to have mutually isostructural tungsten disulfide with molybdenum bisuphide
Cross metal sulfide.Tungsten disulfide crystal is formed by the S-W-S elementary layer stackings with sandwich structure form, its elementary layer by
Upper and lower two-layer sulphur atom layer is formed by connecting with middle one layer of tungsten atom layer by covalent bond, and each unit interlayer only has faint model
De Huali interacts, and this special structure causes that it is widely used in lubrication, scanning probe microscopy, catalysis, field effect
The fields such as transistor and photoelectric sensor are answered, meanwhile, it is embedded and de- that this special layer structure also causes that lithium ion is easy to
It is embedding.There are many researchers to carry out the tungsten disulfide of different-shape and size as the research of lithium cell cathode material, visit
Its chemical property is begged for.By research, it has been found that the pattern of Wolfram disulfide nano material has very big to its chemical property
Influence, when its lamellar structure is changed into individual layer or few layer, there is material now bigger specific surface area, reaction high to live
Property, electronics or ionic conductance high, can so be conducive to the insertion and deintercalation of lithium ion, and at this moment, lithium ion it is embedding
Enter influences smaller with deintercalation on its size, so that material has chemical property higher.When ultra-thin tungsten disulfide is received
When rice piece is assembled into flower-like structure, advantageously in its specific surface area is increased, so as to the chemical property of material can be greatly improved.
But the Wolfram disulfide nano material of current flower-like structure is mainly by hydro-thermal method preparation, and hydro-thermal method preparation yield is relatively low, unfavorable
In batch production, therefore, preparing flower-shaped Wolfram disulfide nano material we have proposed using simple high temperature vulcanized method.
The content of the invention
It is an object of the invention to provide a kind of process is simple, the preparation for preparing flower-shaped Wolfram disulfide nano particle of low cost
Method.
To achieve these goals, the present invention uses following technical scheme：A kind of system of flower-shaped Wolfram disulfide nano particle
Preparation Method, comprises the following steps：By sulphur powder, thiocarbamide and WO3Powder mixes in proportion, and mixed powder is ground, and mixes powder equal
Even, pressed by powder is into disk after then grinding, and disk is put into crucible, then by crucible push-in tube furnace middle position, will
Tube furnace is warmed up to 800~850 DEG C with the speed of 10~12 DEG C/min, while to being passed through protective gas in tube furnace, 800~
850 DEG C of 30~60min of insulation, furnace cooling obtains flower-shaped Wolfram disulfide nano particle to room temperature.
The sulphur powder, thiocarbamide and WO3The mol ratio of powder is 10:10:1~20: 20:1.
It is 20~30min to the mixed powder milling time, is well mixed powder.
A diameter of 25~the 30mm of former piece, thickness is 4~6mm.
Described protective gas is argon gas.
In preparation process of the present invention, all reagents are commercial product, it is not necessary to prepare again.
The cost of the inventive method is inexpensive, and simple production process is easily-controllable, and the nano flower pattern of preparation is more homogeneous, and product is produced
Extracting rate is high, is adapted to large-scale industrial production.
Brief description of the drawings
Fig. 1 is the XRD spectra of the flower-shaped Wolfram disulfide nano particle obtained by embodiment 1.
Fig. 2 is the field emission scanning electron microscope of the flower-shaped Wolfram disulfide nano particle obtained by embodiment 1（SEM）Photo.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is described further.
Embodiment 1：
By 1gWO3Mortar grinder 20min is used after mixing with 1.38g sulphur powders and 3.28g thiocarbamides, the powder after grinding is utilized
Tablet press machine depresses to a diameter of 25mm in 25MPa pressure, and thickness is the disk of 4mm；Disk is put into crucible, and crucible is pushed
Tube furnace central thermal zone position, 800 DEG C are warming up to by tube furnace with the speed of 8 DEG C/min, while to being passed through argon gas in tube furnace；
Tube furnace is incubated 30min at 800 DEG C；Then after tube furnace naturally cools to room temperature, tube furnace two ends ring flange is unloaded, is taken
Go out porcelain boat, obtain black powder, as flower-shaped tungsten disulfide nano slices, the yield of prepared tungsten disulfide is 87%.
Embodiment 2：
By 1gWO3Mortar grinder 30min is used after mixing with 2.76g sulphur powders and 6.56g thiocarbamides, the powder after grinding is utilized
Tablet press machine depresses to a diameter of 25mm in 30MPa pressure, and thickness is the disk of 6mm；Disk is put into crucible, and crucible is pushed
Tube furnace central thermal zone position, 850 DEG C are warming up to by tube furnace with the speed of 10 DEG C/min, while to being passed through argon in tube furnace
Gas；Tube furnace is incubated 60min at 850 DEG C；Then after tube furnace naturally cools to room temperature, the end flanges of tube furnace two are unloaded
Disk, takes out porcelain boat, obtains black powder, as flower-shaped tungsten disulfide nano slices, and the yield of prepared tungsten disulfide is 91%.
Embodiment 3：
By 1gWO3Mortar grinder 25min is used after mixing with 1.38g sulphur powders and 6.56g thiocarbamides, the powder after grinding is utilized
Tablet press machine depresses to a diameter of 25mm in 35MPa pressure, and thickness is the disk of 5mm；Disk is put into crucible, and crucible is pushed
Tube furnace central thermal zone position, 850 DEG C are warming up to by tube furnace with the speed of 8 DEG C/min, while to being passed through argon gas in tube furnace；
Tube furnace is incubated 30min at 850 DEG C；Then after tube furnace naturally cools to room temperature, tube furnace two ends ring flange is unloaded, is taken
Go out porcelain boat, obtain black powder, as flower-shaped tungsten disulfide nano slices, the yield of prepared tungsten disulfide is 89%.
Fig. 1 is the XRD spectrum of the product prepared by embodiment 1, and product is pure WS2Hexagonal；Fig. 2 is embodiment 1
The SEM photograph of prepared product, it can clearly be seen that a large amount of flower-like structures are generated, flower-like structure is mainly received by many ultra-thin
Rice piece composition nanometer sheet thickness is 3~5 nm.
Although the present invention is disclosed as above with preferred embodiment, embodiment and accompanying drawing be not for limiting the present invention,
It is any to be familiar with this those skilled in the art, without departing from the spirit and scope of the invention, can make various changes or retouch from working as, but equally exist
Within protection scope of the present invention.Therefore protection scope of the present invention should be defined with claims hereof protection domain
Be defined.
Claims (2)
1. a kind of preparation method of flower-shaped Wolfram disulfide nano particle, it is characterised in that comprise the following steps：By sulphur powder, thiocarbamide and
WO3Powder mixes in proportion, and mixed powder is ground, and is well mixed powder, then using tablet press machine in 25MPa or 30MPa or
Pressed by powder is into disk after being ground under 35MPa pressure, and disk is put into crucible, then crucible is pushed into tube furnace center position
Put, tube furnace is warmed up to 850 DEG C with the speed of 12 DEG C/min, while to protective gas is passed through in tube furnace, in 850 DEG C of insulations
30min, furnace cooling obtains flower-shaped Wolfram disulfide nano particle to room temperature；The sulphur powder, thiocarbamide and WO3The mol ratio of powder is
10:10:1, it is 20min to the mixed powder milling time, powder is well mixed, a diameter of 25~30mm of disk,
Thickness is 4~6mm.
2. the preparation method of flower-shaped Wolfram disulfide nano particle according to claim 1, it is characterised in that：Described protection
Gas is argon gas.
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| CN106186073A (en) * | 2016-07-12 | 2016-12-07 | 兰州大学 | There is the N doping WS of bigger serface2nanometer sheet preparation method |
| CN107539964B (en) * | 2017-09-30 | 2019-11-26 | 江苏理工学院 | A kind of two selenizing molybdenum powder body material of hexagonal flake and preparation method thereof |
| CN112111788A (en) * | 2020-09-10 | 2020-12-22 | 吉林大学 | Method for preparing titanium disulfide crystal and product |
| CN115784309B (en) * | 2022-11-28 | 2024-04-09 | 国网陕西省电力有限公司电力科学研究院 | Flower-like tungsten disulfide micron particles, and preparation method and application thereof |
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| CN103641173B (en) * | 2013-11-04 | 2016-03-02 | 江苏大学 | The preparation method of one kind Graphene tungsten disulfide nano slices |
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