CN105399060B - A kind of method of Fast back-projection algorithm two-dimensional layer nano material - Google Patents
A kind of method of Fast back-projection algorithm two-dimensional layer nano material Download PDFInfo
- Publication number
- CN105399060B CN105399060B CN201510626627.2A CN201510626627A CN105399060B CN 105399060 B CN105399060 B CN 105399060B CN 201510626627 A CN201510626627 A CN 201510626627A CN 105399060 B CN105399060 B CN 105399060B
- Authority
- CN
- China
- Prior art keywords
- source
- nano material
- projection algorithm
- dimensional layer
- fast back
- 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.)
- Active
Links
Landscapes
- Physical Or Chemical Processes And Apparatus (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of methods of Fast back-projection algorithm two-dimensional layer nano material, include the following steps：There is provided nano-lamellar structure material precursor A and B, and by A and B stoichiometrically Vacuum Package in reaction tube；Packaged reaction tube sample is put into microwave plasma consersion unit, nano-lamellar structure sterling is obtained by the reaction under microwave environment.The present invention implements the nano-lamellar structure such as MoS provided2、WS2Preparation method, can greatly shorten the reaction time, reduce pollution object, while obtain material have preferable pattern and reproducibility, can be applied to the fields such as energy stores, photocatalysis.In addition, the preparation method of the electrode is simple, cost is relatively low, is easy to repeat to realize, to be conducive to industrialization production.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of side of Fast back-projection algorithm two-dimensional layer nano material
Method.
Background technology
Microwave plasma technology is the new method developed in recent years, has great potential and industrial value.Meanwhile it living
Property it is strong, cleanliness without any pollution, process control is good, chemical reaction is quick, favorable reproducibility the features such as increasingly cause the concern of people, and
It is quickly applied to what nano material quickly prepared, and was sintered, is vapor-deposited etc., such as：The low temperature synthesis of carbon nanotubes, long afterglow
Luminescent material, diamond thin, nanometre scale solid film etc..
Molybdenum disulfide be with Van der Waals force combine based on lamellar compound, based on chemical bond S-Mo-S；With non-
The electro-catalysis of Chang Youyi, mechanics, photochemical properties.It is widely used in the industries such as space flight, aviation, chemical industry, metallurgy, it can also be used to urge
Change the fields such as additive, coating and sealing material.Currently, preparing MoS2Method and technology type it is various, be concentrated mainly on (1) height
Warm vulcanization；(2) presoma decomposition method；(3) hydro-thermal method；(4) solwution method；(5) electrochemical deposition method；(6) template；(7) surpass
Phonochemistry method；(8) the methods of molten-salt growth method.In all kinds of preparation methods, the reaction of sonochemistry method is not easily controlled, has pair anti-
It should occur, microwave reactor is expensive, can only be limited in laboratory and synthesize on a small scale, it is difficult to large-scale industrial production.
Electrochemical process equally faces poor reactive component dissolubility, interphase mass transfer poor performance and selectivity of product is low and energy consumption of reaction is big etc.
Problem.Template goes removing template energy consumption is big, template is not easy to remove completely, be easy to cause structure collapse, template can not recycle profit
The problems such as using.Hydro-thermal method is unable to continuous production, and plot ratio is low, efficiency is low, and the high-temperature high-pressure apparatus needed is of high cost, temperature
Crystalline form is usually imperfect when low, and industrialization is highly difficult.
Invention content
In view of the above deficiencies of the prior art, the purpose of the present invention is to provide a kind of Fast back-projection algorithm two-dimensional layers to receive
The method of rice material, realizes the quick, accurate of two-dimension nano materials, low-cost production.
In order to achieve the above objects and other related objects, technical scheme is as follows：A kind of Fast back-projection algorithm two-dimensional layer
The method of shape nano material, includes the following steps：Nano-lamellar structure material precursor A and B are provided, and by A and B based on chemistry
Amount is than Vacuum Package in reaction tube；Packaged reaction tube sample is put into microwave plasma consersion unit, in microwave ring
Nano-lamellar structure sterling is obtained by the reaction under border.
As preferred：Precursor A and B are uniformly mixed to form mixed powder, are subsequently placed in vacuum sealing in reaction tube, is protected
It is 0.01-30Torr to hold reaction overpressure.
As preferred：It is 2-50 nanometers to prepare nano material lamellar spacing.
As preferred：After packaged sample is put into the tubular reactor chamber of microwave plasma consersion unit, it is passed through activity
Gas, adjustment reaction cavity pressure 0.01-100Torr, open after microwave switch carries out reaction 5-30 minutes and obtain nanoscale twins knot
Structure product.
As preferred：A diameter of 8mm-20mm of the reaction tube.
As preferred：The precursor A and B are molybdenum source and sulphur source, finally prepare sheet MoS2Nano-powder；Or
The presoma is molybdenum source and selenium source, finally prepares sheet MoSe2Nano-powder；Or presoma be tungsten source and selenium source,
Finally prepare sheet WSe2Nano-powder；Or presoma is tungsten source and sulphur source, finally prepares sheet WS2Nanometer
Powder；Presoma is niobium source and selenium source, finally prepares sheet NbSe2Nano-powder.
As preferred：Protection pipe, the air inlet pipe that the microwave plasma consersion unit includes microwave source, is placed in microwave source
The inlet end of road and outlet pipe, the air inlet pipeline and protection pipe connects, and the outlet side of the outlet pipe and protection pipe connects
It connects, control valve is both provided on the air inlet pipeline and outlet pipe, air pressure is provided on the air inlet pipeline or outlet pipe
Meter.
As preferred：The air inlet pipeline and outlet pipe are connect with protection pipe both ends by vacuum seal structure；It is described
Barometer is arranged on outlet pipe, between control valve and protection pipe.
As preferred：The outlet pipe is connected with vacuum pump by bump joint, and the control valve is needle-valve.
As preferred：Precursor A and the stoichiometric ratio of B by the molar ratio of A and B in generation substance.
As described above, the beneficial effects of the invention are as follows：The present invention implements the preparation side of the nano-lamellar structure material provided
Method can greatly shorten the reaction time, reduce pollution object, while the material obtained has preferable pattern and reproducibility,
It can be applied to the fields such as energy stores, photocatalysis.In addition, the preparation method of the electrode is simple, cost is relatively low, is easy to repeat real
It is existing, to be conducive to industrialization production.
Description of the drawings
Fig. 1 is the structural schematic diagram of microwave plasma consersion unit in the present invention；
Fig. 2 is the SEM image of sample of the present invention；
Fig. 3 is the TEM image of sample of the present invention
Fig. 4 is the diffraction image of sample of the present invention；
Fig. 5 is the Raman collection of illustrative plates of sample of the present invention.
Piece mark explanation
1 microwave source
2 protection pipes
3 reaction tubes
4 air inlet pipelines
5 outlet pipes
61,62 control valve
71,72 vacuum sealing connector
8 barometers
9 microwave switches
10 bump joints
Specific implementation mode
Illustrate that embodiments of the present invention, those skilled in the art can be by this explanations by particular specific embodiment below
Content disclosed by book understands other advantages and effect of the present invention easily.
Embodiment 1
Below in conjunction with the accompanying drawings and the specific embodiments to sheet MoS provided by the invention2Nanometer preparation method is made into one
The detailed description of step.
The present invention provides a kind of applied to Fast back-projection algorithm sheet MoS2The preparation method of nano material：By molybdenum source A and sulphur
Source B presses MoS2Molar ratio is uniformly mixed to form mixed powder.Wherein molybdenum source A is 0.1 mole, and sulphur source B is 0.2 mole, wherein molybdenum
Source is the molybdenum powder of simple substance, and sulphur source is simple substance sulfur powder.The mixture is placed in the reaction tube 3 of a diameter 8-20mm, is reacted
Pipe 3 is quartz ampoule, and by its vacuum sealing, it is 0.01-30Torr to keep reaction overpressure；It is then placed in knot as shown in Figure 1
In the microwave plasma apparatus of structure, and the tube chamber pressure for adjusting plasma apparatus protection pipe 2 opens microwave in 0.01-100Torr
Switch 9 (power 300W-1000W) carries out reaction 5-30 minutes up to sheet MoS2Powder, powder style test result is as schemed
Shown in 2-5, as a result show that product more crystal structure is preferable, 2-30 nanometers of lamellar spacing, the lamella ruler shown from SEM pictures
Very little distribution is uniform, indicates that particle dispersion is preferable.TEM image indicates that nanoscale twins cleanliness factor is preferable.Raman peaks only have in Fig. 5
396 and 405 nanometers of two peaks, expression composition are more pure.
This method has the characteristics that quick, inexpensive, clean and pollution-free；Meanwhile MoS2Nano-powder is as a kind of high-purity
Kollag, the characteristics such as chemical property with excellent high temperature resistant, resistance to compression and stabilization, is widely used in space flight, aviation, change
The industries such as work, metallurgy, it can also be used to the fields such as catalytic additive, coating and sealing material.
As shown in Figure 1, microwave plasma apparatus includes microwave source 1, the protection pipe 2 that is placed in microwave source, 4 and of air inlet pipeline
Outlet pipe 5, microwave source 1 are that protection pipe 2 and reaction tube 3 provide microwave environment, and with microwave switch 9, air inlet pipeline 4 passes through
Vacuum sealing joint 71 is connect with the inlet end of protection pipe 2, and outlet pipe 5 is gone out by vacuum sealing joint 72 and protection pipe 2
Gas end connects, and control valve 61,62 is both provided on air inlet pipeline 4 and outlet pipe 5, for adjusting the air pressure in protection pipe 2, into
It is provided with barometer 8 on air pipe 4 or outlet pipe 5.
Barometer 8 described in this example is arranged on outlet pipe 5, between control valve 62 and the outlet side of protection pipe 2,
It can also make to form vacuum environment, institute in protection pipe 2 by 10 connection vacuum pumps for being evacuated in the outlet side of outlet pipe 5
It is needle-valve to state control valve 61,62.
2 both ends of protection pipe are sealingly connected to pipeline by the microwave plasma apparatus after reaction tube 3 is put into protection pipe 2
In, it is evacuated by 2 outlet side of protection pipe, inlet end is passed through gas, and adjusts gas size by control valve 61,62, to control
For pressure in protection pipe 2 processed in claimed range, it can be inert gas or other active gases that air inlet pipeline 4, which is passed through gas,
Reaction is cannot participate in, pressure is mainly adjusted and the rough vacuum in protection pipe 2 is maintained to act on, plasma is enable to generate.
It should be noted that：The method of the present invention is not rely on the microwave plasma apparatus provided in the present invention, may be used also
To use other microwave plasma apparatus in the prior art.
Embodiment 2
The present embodiment and the embodiment 1 are essentially identical, and difference lies in the active material precursor A, B are respectively molybdenum
Source and selenium source finally prepare sheet MoSe2Nano-powder.
A kind of Fast back-projection algorithm sheet MoSe2The preparation method of nano material：Molybdenum source A and selenium source B are uniformly mixed to form
Mixed powder.The molybdenum elemental powders that wherein molybdenum source A is 0.1 mole, the selenium elemental powders that selenium source B is 0.2 mole.By the mixture
It is placed in the reaction tube 3 of a diameter 8-20mm, reaction tube 3 is quartz ampoule, and by its vacuum sealing, and holding reaction overpressure is
2-10Torr；It is then placed in the microwave plasma apparatus of structure as shown in Figure 1, and adjusts the pipe of plasma apparatus protection pipe 2
Cavity pressure opens microwave switch 9 (power 770W) and carries out reaction 20 minutes up to sheet MoSe in 20-30Torr2Powder, powder
Body style test result shows that product more structure is more complete, 20-30 nanometers of lamellar spacing, and with preferable dispersibility.
Embodiment 3
The present embodiment and the embodiment 1 are essentially identical, and difference lies in the electrode active material precursor A, B difference
For tungsten source and selenium source, sheet WSe is finally prepared2Nano-powder.
A kind of Fast back-projection algorithm sheet WSe2The preparation method of nano material：Molybdenum source A and selenium source B are uniformly mixed to form mixed
Close powder.Wherein molybdenum source A is the elemental powders of 0.1 mole of tungsten, and selenium source B is the elemental powders of 0.2 mol selenium.The mixture is set
In the reaction tube 3 of a diameter 8-20mm, reaction tube 3 is quartz ampoule, and by its vacuum sealing, it is 2- to keep reaction overpressure
10Torr；It is then placed in the microwave plasma apparatus of structure as shown in Figure 1, and adjusts the tube chamber of plasma apparatus protection pipe 2
Pressure opens microwave switch 9 (power 600W) and carries out reaction 15-20 minutes up to sheet WSe in 15-30Torr2Powder, powder
Body style test result shows that product more structure is more complete, 15-30 nanometers of lamellar spacing, and with preferable dispersibility.
Embodiment 4
The present embodiment and the embodiment 1 are essentially identical, and difference lies in the electrode active material precursor A, B difference
For tungsten source and sulphur source, sheet WS is finally prepared2Nano-powder.
A kind of Fast back-projection algorithm sheet WS2The preparation method of nano material：Tungsten source and sulphur source are uniformly mixed to form mixing
Powder.Wherein tungsten source is 0.1 mole, and sulphur source is 0.2 mole, and tungsten source is tungsten elemental powders, and sulphur source is sulphur simple substance powder.This is mixed
It closes object to be placed in the reaction tube 3 of a diameter 8-20mm, reaction tube 3 is quartz ampoule, and by its vacuum sealing, keeps reaction tube internal pressure
Power is 8-15Torr；It is then placed in the microwave plasma apparatus of structure as shown in Figure 1, by being passed through gas or pumping adjustment etc.
The tube chamber pressure of ion device protection pipe 2 opens microwave switch 9 (power 800W) and carries out reaction 5-10 minutes in 10-20Torr
Up to sheet WS2Powder, powder style test result show product it is more complete, 30-50 nanometer of lamellar spacing, and have compared with
Good dispersibility.
Embodiment 5
The present embodiment and the embodiment 1 are essentially identical, and difference lies in the electrode active material precursor A, B difference
For niobium source and selenium source, sheet NbSe is finally prepared2Nano-powder.
A kind of Fast back-projection algorithm sheet NbSe2The preparation method of nano material：The elemental powders of niobium and selenium are uniformly mixed
Form mixed powder.Wherein niobium source is 0.1 mole, and selenium source is 0.2 mole, and niobium source is niobium elemental powders, and selenium source is selenium simple substance powder
End.The mixture is placed in the reaction tube 3 of a diameter 8-20mm, reaction tube 3 is quartz ampoule, and by its vacuum sealing, is kept
Reaction overpressure is 2-5Torr；It is then placed in the microwave plasma apparatus of structure as shown in Figure 1, and adjusts plasma and set
The tube chamber pressure of standby protection pipe 2 opens microwave switch 9 (power 650W) and carries out reaction 20-30 minutes up to piece in 20-40Torr
Stratiform NbSe2Powder, powder style test result show that product is more pure, 2-30 nanometers of lamellar spacing, and with preferable
Dispersibility.
It should be noted that the purpose of the present invention is to provide above-mentioned preparation method, reaction overpressure therein, official jargon
Pressure, microwave power and reaction time etc. can be arranged according to specific reactant.
Preferred embodiment above is merely illustrative of the technical solution of the present invention and unrestricted, any person skilled in the art
It can all carry out modifications and changes to above-described embodiment without violating the spirit and scope of the present invention.Therefore, such as belonging to technology
Have all that usually intellectual is completed without departing from the spirit and technical ideas disclosed in the present invention in field equivalent to repair
Decorations change, and should be covered by the claim of the present invention.
Claims (9)
1. a kind of method of Fast back-projection algorithm two-dimensional layer nano material, which is characterized in that include the following steps：Nanoscale twins are provided
Structural material precursor A and B, and by Vacuum Package after A and B mixing in reaction tube, it is 0.01- to keep reaction overpressure
30Torr；Packaged reaction tube sample is put into microwave plasma consersion unit, nanometer is obtained by the reaction under microwave environment
Lamellar structure sterling, microwave power 300-1000W；The tubulose that packaged sample is put into microwave plasma consersion unit is anti-
After answering chamber, it is passed through gas, adjustment reaction cavity pressure 0.01-100Torr, opens after microwave switch carries out reaction 5-30 minutes and obtains
Nano-lamellar structure product.
2. a kind of method of Fast back-projection algorithm two-dimensional layer nano material according to claim 1, it is characterised in that：By forerunner
Body A and B are uniformly mixed to form mixed powder, are subsequently placed in vacuum sealing in reaction tube.
3. a kind of method of Fast back-projection algorithm two-dimensional layer nano material according to claim 1, it is characterised in that：Preparation obtains
It is 2-50 nanometers to obtain nano material lamellar spacing.
4. a kind of method of Fast back-projection algorithm two-dimensional layer nano material according to claim 1, it is characterised in that：It is described anti-
Should pipe a diameter of 8mm-20 mm.
5. a kind of method of Fast back-projection algorithm two-dimensional layer nano material according to claim 1, it is characterised in that：Before described
It is molybdenum source and sulphur source to drive body A and B, finally prepares sheet MoS2Nano-powder；Or the presoma be molybdenum source and selenium source,
Finally prepare sheet MoSe2Nano-powder；Or presoma is tungsten source and selenium source, finally prepares sheet WSe2It receives
Rice flour body；Or presoma is tungsten source and sulphur source, finally prepares sheet WS2Nano-powder；Presoma be niobium source and selenium source,
Finally prepare sheet NbSe2Nano-powder.
6. a kind of method of Fast back-projection algorithm two-dimensional layer nano material according to claim 1, it is characterised in that：It is described micro-
Protection pipe, air inlet pipeline and the outlet pipe that wave plasma reaction equipment includes microwave source, is placed in microwave source, the air inlet pipe
The inlet end of road and protection pipe connects, and the outlet side of the outlet pipe and protection pipe connects, the air inlet pipeline and escape pipe
Road is both provided with control valve, and barometer is provided on the air inlet pipeline or outlet pipe.
7. a kind of method of Fast back-projection algorithm two-dimensional layer nano material according to claim 6, it is characterised in that：It is described into
Air pipe and outlet pipe are connect with protection pipe both ends by vacuum seal structure；The barometer is arranged on outlet pipe,
Between control valve and protection pipe.
8. a kind of method of Fast back-projection algorithm two-dimensional layer nano material according to claim 7, it is characterised in that：It is described go out
Air pipe is connected with vacuum pump by bump joint, and the control valve is needle-valve.
9. a kind of method of Fast back-projection algorithm two-dimensional layer nano material according to claim 1, it is characterised in that：Presoma
The stoichiometric ratio of A and B is molar ratio.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510626627.2A CN105399060B (en) | 2015-09-28 | 2015-09-28 | A kind of method of Fast back-projection algorithm two-dimensional layer nano material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510626627.2A CN105399060B (en) | 2015-09-28 | 2015-09-28 | A kind of method of Fast back-projection algorithm two-dimensional layer nano material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105399060A CN105399060A (en) | 2016-03-16 |
| CN105399060B true CN105399060B (en) | 2018-09-25 |
Family
ID=55464875
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510626627.2A Active CN105399060B (en) | 2015-09-28 | 2015-09-28 | A kind of method of Fast back-projection algorithm two-dimensional layer nano material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105399060B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107601443B (en) * | 2017-11-09 | 2020-01-14 | 安徽大学 | Preparation method of ultrathin tungsten selenide nanosheets |
| CN108793096B (en) * | 2018-06-04 | 2022-03-01 | 武汉理工大学 | NbSe with nano-sized surface2Electrode material and preparation method and application thereof |
| CN109879315B (en) * | 2019-04-09 | 2021-06-01 | 陕西科技大学 | Two-dimensional layered porous hexagonal nano titanium dioxide and preparation method and application thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102732834B (en) * | 2012-06-18 | 2013-11-20 | 徐明生 | Apparatus for preparing two-dimensional nanometer film |
| CN102923677B (en) * | 2012-11-08 | 2014-08-13 | 镇江中孚复合材料有限公司 | Method for preparing NbSe2 nano material |
| CN103693693A (en) * | 2013-12-26 | 2014-04-02 | 湛江师范学院 | Preparation method for synthesizing molybdenum sulfide nanospheres by microwave-assisted liquid phase deposition |
-
2015
- 2015-09-28 CN CN201510626627.2A patent/CN105399060B/en active Active
Non-Patent Citations (2)
| Title |
|---|
| Synthesis of nanocrystalline MoS2 and WS2 in a microwave plasma;D. Vollath 等;《Materials Letters 》;19980531;第35卷;第236-244页 * |
| 纳米片状MoS2的固态杂化微波合成;谢绵钰 等;《人工晶体学报》;20150531;第44卷(第5期);第1394-1397页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105399060A (en) | 2016-03-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Liu et al. | Crystalline red phosphorus nanoribbons: large‐scale synthesis and electrochemical nitrogen fixation | |
| Gao et al. | High-yield synthesis of boron nitride nanosheets with strong ultraviolet cathodoluminescence emission | |
| Li et al. | Electrochemically active MnO2/RGO nanocomposites using Mn powder as the reducing agent of GO and the MnO2 precursor | |
| CN110038607A (en) | Titanium carbide nanometer sheet/stratiform indium sulfide hetero-junctions and its application in degradation removal water pollutant | |
| CN108002374A (en) | A kind of ultra-thin two-dimension stratified material nanometer sheet and preparation method thereof | |
| CN108273541B (en) | Green and efficient preparation method and application of graphite-phase carbon nitride nanosheets | |
| CN106517171B (en) | A kind of preparation method of graphene aerogel | |
| CN105399060B (en) | A kind of method of Fast back-projection algorithm two-dimensional layer nano material | |
| CN103787288B (en) | A kind of preparation method of boron nitride alkene nanometer sheet | |
| Cao et al. | Influences of carrier gas flow rate on the morphologies of MoS2 flakes | |
| CN105668555B (en) | A kind of method for preparing three-dimensional grapheme | |
| CN107651708A (en) | A kind of method that microwave hydrothermal prepares 1T@2H MoS2 | |
| US11142459B2 (en) | Dense graphene balls for hydrogen storage | |
| CN113479849A (en) | Preparation method of nano metal oxide | |
| US20160167011A1 (en) | Method for producing a graphene | |
| CN105858632A (en) | Cobaltous phosphate nanotube material, preparation method thereof and application of cobaltous phosphate nanotube material in photosplitting water into oxygen | |
| CN103771521B (en) | Method for preparing tungsten disulfide nano sheet | |
| Duan et al. | Elemental phosphorus for recent sustainable processes: rules and strategies in preparation and applications | |
| CN105714266A (en) | Preparing method for cuprous sulfide nanosheets | |
| CN108314333A (en) | A kind of Electrostatic Absorption preparation method of Graphene glass | |
| CN107337233A (en) | A kind of method of one step vulcanization method synthesis of titanium dioxide and titanium disulfide composite | |
| Long et al. | Facile synthesis of various carbon nanotube/metal oxide nanocomposites with high quality | |
| CN107742704B (en) | Preparation method of molybdenum disulfide/graphene battery anode material based on three-dimensional framework formed by graphene self-assembly | |
| KR101894543B1 (en) | Method for fabricating reduced graphene oxide and its suspension | |
| CN111039318B (en) | Method for preparing SnS nano material by direct current arc plasma |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |