CN103641173B - The preparation method of one kind Graphene tungsten disulfide nano slices - Google Patents

The preparation method of one kind Graphene tungsten disulfide nano slices Download PDF

Info

Publication number
CN103641173B
CN103641173B CN201310533441.3A CN201310533441A CN103641173B CN 103641173 B CN103641173 B CN 103641173B CN 201310533441 A CN201310533441 A CN 201310533441A CN 103641173 B CN103641173 B CN 103641173B
Authority
CN
China
Prior art keywords
tungsten disulfide
powder
disulfide nano
nano slices
preparation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN201310533441.3A
Other languages
Chinese (zh)
Other versions
CN103641173A (en
Inventor
唐华
张向华
李磊
李长生
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangsu University
Original Assignee
Jiangsu University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jiangsu University filed Critical Jiangsu University
Priority to CN201310533441.3A priority Critical patent/CN103641173B/en
Publication of CN103641173A publication Critical patent/CN103641173A/en
Application granted granted Critical
Publication of CN103641173B publication Critical patent/CN103641173B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

The invention discloses the preparation method of a kind Graphene tungsten disulfide nano slices, employing be high temperature solid phase synthesis, step is as follows: by thiocarbamide and WO 3after 20:1 ~ 41:1 mixing in molar ratio, fully grinding, loads porcelain boat by the powder after grinding; Tube furnace is warming up to 800 ~ 900 DEG C, passes into nitrogen; Porcelain boat is pushed rapidly position, tube furnace central thermal zone, constant temperature process 30 ~ 60min; Then, naturally cool to room temperature, obtain class Graphene tungsten disulfide nano slices.The inventive method technique is simple, and with low cost, the product purity prepared is high, productive rate is high, is expected to for large-scale industrial production.

Description

The preparation method of one kind Graphene tungsten disulfide nano slices
Technical field
The present invention relates to inorganic materials tungsten disulfide (WS 2) preparation field, the particularly preparation method of class Graphene tungsten disulfide nano slices.
Background technology
Graphene is as only there being monolayer carbon atomic thickness and be the two-dimension nano materials of honeycomb lattice at plane development with hexangle type, because it has unique electrical behavior and high specific surface area, become after soccerballene, carbon nanotube by the simple substance carbon family member of extensive concern; Graphene is typical two-dimensional nanostructure system, its thickness is at atomic scale, planar diameter but can reach submillimeter and above size, and the quantum confined effect that its two-dimentional yardstick high anisotropy shows and surface effects make the simple substance carbon bill of material of this individual layer reveal distinct electrical behavior, mechanical property and optics, thermal property etc. with body phase material; Be subject to the inspiration of Graphene, people start to pay close attention to the mineral compound that other have two-dimensional layer crystal structure characteristic, as having the transition metal dichalcogenide WS of single layer structure 2and MoS 2.
The two dimensional crystal material with " sandwich " laminate structure that class Graphene tungsten disulfide is made up of the single or multiple lift tungsten disulfide of hexagonal system: individual layer tungsten disulfide is made up of three layers of atomic shell, middle one deck is tungsten atom layer, two-layerly up and down be sulphur atom layer, tungsten atom layer forms class " sandwich " structure folded by two-layer sulphur atom layer, and tungsten atom and sulphur atom form two-dimensional atomic crystal with covalent bonds; Multilayer tungsten disulfide is made up of some individual layer tungsten disulfides, is generally no more than five layers, and interlayer exists weak Van der Waals force; " sandwich " laminate structure of this uniqueness makes class Graphene tungsten disulfide nano slices gather around in various fields such as lubricant, catalysis, stored energy, sensor, electroluminescent to have wide practical use; In addition, different from the Graphene with two-dimensional layered structure, class Graphene tungsten disulfide also has special energy band structure; Although Graphene has high conductivity at two dimensional surface, because pure grapheme material does not have band gap, for its at electron device as the application in transistor brings drawback; But class Graphene tungsten disulfide material but shows abundant electrical behavior, has the nature and characteristic different from body phase material; The macroscopic material of tungsten disulfide is the indirect band-gap semiconductor of band gap at 1.3eV, the direct band-gap semicondictor of the tungsten disulfide of individual layer to be then band gap be 2.1eV, this special energy band structure, makes class Graphene Wolfram disulfide nano material can be widely used in the preparation of electron device, phototransistor, energy storage device; But, general chemistry, Physical are difficult to prepare the class Graphene tungsten disulfide with laminate structure, the method that can adopt at present mainly contains the stripping method of " from top to bottom " such as micromechanical forces stripping method, lithium ion graft process, liquid phase ultrasonic methods, and the synthesis method of high temperature thermal decomposition, vapour deposition, hydrothermal method etc. " from bottom to top ", class Graphene tungsten disulfide output prepared by above method is all considerably less, high temperature solid-state method output is high, but does not also have high temperature solid-state method to prepare the report of class Graphene tungsten disulfide nano slices at present.
Summary of the invention
The object of this invention is to provide the preparation method of the preparation class Graphene tungsten disulfide nano slices that a kind of technique is simple, cost is low.
The method preparing class Graphene tungsten disulfide nano slices of the present invention, employing be high temperature solid-state method, step is as follows: by sulphur source and WO 3powder 20:1 ~ 41:1 mixing in molar ratio, to mixed powder grinding, powder is mixed, high temperature process furnances is warmed up to 800-900 DEG C, in tube furnace, pass into shielding gas simultaneously, open tube furnace outlet end flange dish, powder after grinding is inserted in high temperature process furnances, tighten ring flange rapidly, at 800-900 DEG C of insulation 30-60min, sulphur source pyrolytic decomposition generation dithiocarbonic anhydride and tungstic oxide react and generate tungsten disulfide, utilize the high temperature moment vigorous reaction of powder, produce a large amount of gas, the erosion effect of gas causes the separation of stratiform tungsten disulfide nano slices, generate ultrathin nanometer sheet, furnace cooling is to room temperature, obtain class Graphene tungsten disulfide nano slices.
In preparation process of the present invention, all reagent is commerical prod, does not need to prepare again.
Described sulphur source is thiocarbamide.
Described make powder mix finger to mixed powder grinding to utilize mortar that mixed powder is ground 30-60min powder is mixed.
The described 800-900 DEG C of finger that be warmed up to by high temperature process furnances is warmed up to 800-900 DEG C with the speed of 10 DEG C/min.
Described shielding gas is nitrogen.
The cost of the inventive method is inexpensive, and production technique is simple and easy to control, and the nanometer sheet thickness of preparation is thinner, and lateral dimension is larger, and product output capacity is high, is applicable to large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is the XRD spectra of the class Graphene tungsten disulfide nano slices that the present invention obtains.
Fig. 2 is field emission scanning electron microscope (SEM) photo of the class Graphene tungsten disulfide nano slices that the present invention obtains.
Fig. 3 is projection Electronic Speculum (TEM) photo of the class Graphene tungsten disulfide nano slices that the present invention obtains.
Embodiment
The present invention is further illustrated below in conjunction with example.
Embodiment 1:
By 0.5gWO 3use mortar grinder 45min after mixing with 4.92g thiocarbamide, the powder after grinding is loaded porcelain boat stand-by; Tube furnace temperature is increased to 850 DEG C, in tube furnace, passes into nitrogen; Tube furnace temperature-stable at 850 DEG C time open tube furnace outlet end flange dish, porcelain boat is pushed into rapidly position, tube furnace central thermal zone, insulation 1h; Then naturally cool to after room temperature until tube furnace, unload tube furnace two ends ring flange, take out porcelain boat, obtain black powder, i.e. class Graphene tungsten disulfide nano slices.
Embodiment 2:
By 0.5gWO 3use mortar grinder 30min after mixing with 3.3g thiocarbamide, the powder after grinding is loaded porcelain boat stand-by; Tube furnace temperature is increased to 800 DEG C, passes into nitrogen; Tube furnace temperature-stable at 800 DEG C time open tube furnace outlet end flange dish, porcelain boat is pushed into rapidly position, tube furnace central thermal zone, insulation 30min; Then naturally cool to after room temperature until tube furnace, obtain black powder, be i.e. class Graphene tungsten disulfide nano slices.
Embodiment 3:
By 0.5gWO 3use mortar grinder 60min after mixing with 6.6g thiocarbamide, the powder after grinding is loaded porcelain boat stand-by; Tube furnace temperature is increased to 900 DEG C, passes into nitrogen; Tube furnace temperature-stable at 900 DEG C time open tube furnace outlet end flange dish, porcelain boat is pushed into rapidly position, tube furnace central thermal zone, insulation 60min; Then naturally cool to after room temperature until tube furnace, obtain black powder, be i.e. class Graphene tungsten disulfide nano slices.
Fig. 1 is the XRD figure spectrum of prepared product, and product is pure WS 2hexagonal; Fig. 2 is the SEM photo of prepared product, and obviously can see that a large amount of ultrathin nanometer sheet generates, soilless sticking phenomenon, nanometer sheet thickness is 3-5nm; Fig. 3 is the TEM photo of prepared product, can see many class graphene nanometer sheets, and the structure of nanometer sheet is very homogeneous, and defect is less.

Claims (5)

1. the preparation method of a kind Graphene tungsten disulfide nano slices, is characterized in that comprising the steps: sulphur source and WO 3powder is mixed in proportion; mixed powder is ground; powder is mixed; high temperature process furnances is warmed up to 800-900 DEG C, in tube furnace, passes into shielding gas simultaneously, open tube furnace outlet end flange dish; powder after grinding is inserted in high temperature process furnances; tighten ring flange rapidly, at 800-900 DEG C of insulation 30-60min sulphur source pyrolytic decomposition generation dithiocarbonic anhydride and tungstic oxide react and generate tungsten disulfide, utilize the high temperature moment vigorous reaction of powder, produce a large amount of gas, the erosion effect of gas causes the separation of stratiform tungsten disulfide nano slices, generate ultrathin nanometer sheet, furnace cooling, to room temperature, obtains class Graphene tungsten disulfide nano slices;described sulphur source is thiocarbamide, wherein thiocarbamide and WO 3the mol ratio of powder is 20:1 ~ 41:1.
2. the preparation method of the kind Graphene tungsten disulfide nano slices according to right 1, is characterized in that, described makes powder mix finger to mixed powder grinding to utilize mortar that mixed powder is ground 30-60min powder is mixed.
3. the preparation method of the kind Graphene tungsten disulfide nano slices according to right 1, is characterized in that, the described 800-900 DEG C of finger that be warmed up to by high temperature process furnances is warmed up to 800-900 DEG C with the speed of 10 DEG C/min.
4. the preparation method of the kind Graphene tungsten disulfide nano slices according to right 1, it is characterized in that, described shielding gas is nitrogen.
5. the preparation method of the kind Graphene tungsten disulfide nano slices according to right 1, is characterized in that, the thickness of described class Graphene tungsten disulfide nano slices is 3 ~ 5nm.
CN201310533441.3A 2013-11-04 2013-11-04 The preparation method of one kind Graphene tungsten disulfide nano slices Expired - Fee Related CN103641173B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310533441.3A CN103641173B (en) 2013-11-04 2013-11-04 The preparation method of one kind Graphene tungsten disulfide nano slices

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310533441.3A CN103641173B (en) 2013-11-04 2013-11-04 The preparation method of one kind Graphene tungsten disulfide nano slices

Publications (2)

Publication Number Publication Date
CN103641173A CN103641173A (en) 2014-03-19
CN103641173B true CN103641173B (en) 2016-03-02

Family

ID=50246510

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310533441.3A Expired - Fee Related CN103641173B (en) 2013-11-04 2013-11-04 The preparation method of one kind Graphene tungsten disulfide nano slices

Country Status (1)

Country Link
CN (1) CN103641173B (en)

Families Citing this family (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103964507B (en) * 2014-05-08 2015-10-21 中国科学技术大学 A kind of individual layer transition metal chalcogenide film and preparation method thereof
CN104393295B (en) * 2014-11-27 2017-06-16 江苏理工学院 A kind of preparation method of flower-shaped Wolfram disulfide nano particle
CN104495938A (en) * 2014-11-27 2015-04-08 江苏理工学院 Method for preparing titanium-doped tungsten disulfide solid lubricant
CN105019029B (en) * 2015-06-30 2018-05-04 中国地质大学(北京) High-purity, high yield prepare WS2The method of lamellar nanostructured
CN105551909B (en) * 2015-12-23 2017-12-01 深圳先进技术研究院 Field-transmitting cathode and its preparation method and application
CN106229359B (en) * 2016-07-29 2017-08-29 中国地质大学(北京) A kind of efficient photoelectricity treater converter based on carbon fiber@tungsten disulfide nano slices core-shell structures and preparation method thereof
CN106277059A (en) * 2016-08-22 2017-01-04 齐齐哈尔大学 A kind of method preparing tungsten disulfide/Graphene heterojunction structure
CN106384811B (en) * 2016-10-14 2019-06-07 福州大学 A kind of indigo plant phosphorus/transition metal dichalcogenide hetero-junctions anode material and preparation method
CN107119328B (en) * 2017-04-07 2019-06-21 湖南大学 A kind of stratiform WS with complicated helical structure2Two-dimension nano materials and preparation method thereof
CN107416905B (en) * 2017-06-22 2019-03-08 河南大学 A kind of preparation method of oil-soluble tungsten disulfide nano slices
CN108539158B (en) * 2018-04-04 2020-10-02 华南师范大学 rGO/WS2Preparation method of composite material and application of composite material in positive electrode material of lithium-sulfur battery
CN109326787B (en) * 2018-10-30 2021-08-10 陕西科技大学 Preparation method of tungsten disulfide/GO composite electrode material
CN112871397B (en) * 2020-12-28 2021-10-22 浙江爱润特汽车科技有限公司 Nanoscale tungsten disulfide material and preparation method and device thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101723464A (en) * 2009-12-11 2010-06-09 中南大学 Method for preparing mono-disperse tungsten disulfide nano slices
CN102863025A (en) * 2012-09-25 2013-01-09 镇江市高等专科学校 Preparation method of piece-shaped tungsten disulfide nanometer lubricating oil additive
CN102897841A (en) * 2012-09-28 2013-01-30 浙江东晶光电科技有限公司 Preparation method of tungsten disulfide micron structure

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101723464A (en) * 2009-12-11 2010-06-09 中南大学 Method for preparing mono-disperse tungsten disulfide nano slices
CN102863025A (en) * 2012-09-25 2013-01-09 镇江市高等专科学校 Preparation method of piece-shaped tungsten disulfide nanometer lubricating oil additive
CN102897841A (en) * 2012-09-28 2013-01-30 浙江东晶光电科技有限公司 Preparation method of tungsten disulfide micron structure

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
机械活化制法制备WS2纳米片;徐泽众等;《机械工程加工》;20130331;第37卷(第3期);第61-64、76页 *
片状超细WS2粉末的制备及其润滑性能研究;唐宜等;《润滑与密封》;20110430;第36卷(第4期);第102-104页 *

Also Published As

Publication number Publication date
CN103641173A (en) 2014-03-19

Similar Documents

Publication Publication Date Title
CN103641173B (en) The preparation method of one kind Graphene tungsten disulfide nano slices
Li et al. Hierarchical MoS2 hollow architectures with abundant Mo vacancies for efficient sodium storage
Wang et al. Two-dimensional nanomaterials with engineered bandgap: Synthesis, properties, applications
Sun et al. Atomically-thick two-dimensional crystals: electronic structure regulation and energy device construction
Zheng et al. Vertically oriented few-layered HfS2 nanosheets: growth mechanism and optical properties
Zou et al. Well-aligned arrays of CuO nanoplatelets
Piao et al. Hydrothermal synthesis of stable metallic 1T phase WS2 nanosheets for thermoelectric application
Popuri et al. Rapid hydrothermal synthesis of VO2 (B) and its conversion to thermochromic VO2 (M1)
Paul et al. Nanoporous Ca3Co4O9 thin films for transferable thermoelectrics
Shi et al. Surfactant-assisted hydrothermal growth of single-crystalline ultrahigh-aspect-ratio vanadium oxide nanobelts
Song et al. Bottom-up approach design, band structure, and lithium storage properties of atomically thin γ-FeOOH nanosheets
Deng et al. Quantum confinement effects and electronic properties of SnO2 quantum wires and dots
Liu et al. Novel single-crystalline hierarchical structured ZnO nanorods fabricated via a wet-chemical route: combined high gas sensing performance with enhanced optical properties
Qi et al. Fabrication of graphene with CuO islands by chemical vapor deposition
Chahal et al. Microwave synthesis of hematene and other two-dimensional oxides
Nurdiwijayanto et al. Stability and nature of chemically exfoliated MoS2 in aqueous suspensions
Qin et al. Facial grinding method for synthesis of high-purity CuS nanosheets
Zhang et al. Interface-induced enhanced electromagnetic wave absorption property of metal-organic frameworks wrapped by graphene sheets
Xu et al. Indirect-direct band transformation of few-layer BiOCl under biaxial strain
Pham A library of doped-graphene images via transmission electron microscopy
Alli et al. Chemical functionalisation of 2D materials by batch and continuous hydrothermal flow synthesis
Zhong et al. Double salt-template strategy for the growth of N, S-codoped graphitic carbon nanoframes on the graphene toward high-performance electromagnetic wave absorption
Li et al. ZnO quantum dot/MXene nanoflake hybrids for ultraviolet photodetectors
Wang et al. Synthetic versatility of nanoparticles: A new, rapid, one-pot, single-step synthetic approach to spherical mesoporous (metal) oxide nanoparticles using supercritical alcohols
Pol et al. Facile synthesis of novel photoluminescent ZnO micro-and nanopencils

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20160302

Termination date: 20191104