CN109809372A - A method of two tungsten selenide nanobelt of single layer is prepared based on space confinement strategy - Google Patents
A method of two tungsten selenide nanobelt of single layer is prepared based on space confinement strategy Download PDFInfo
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Abstract
The invention discloses a kind of methods for preparing two tungsten selenide nanobelt of single layer based on space confinement strategy.The flow and growth time that the present invention passes through change hydrogen, the Effective Regulation to nanometer bandwidth and thickness may be implemented, include the following steps: for tungsten trioxide powder to be uniformly spread across in a piece of substrate, then with another substrate cover above, forms the minisize reaction space of class " sandwich " structure.The growth of two tungsten selenide nanobelts is carried out using the method for aumospheric pressure cvd；The physicochemical characteristics of one-dimensional transient metal chalcogenide compound is strongly depend on its edge suspension key type, and ultra-narrow band shows metalline, and wider band shows metalline to semiconductive fundamental change from its edge to center；This special nature has a wide range of applications two tungsten selenide nanobelts in micro-nano photoelectric device；And experimental method according to the present invention, it can be achieved that two tungsten selenide nanobelts industrialized production.
Description
Technical field
The present invention relates to materials and microelectric technique, in particular to a kind of to prepare two selenizing of single layer based on space confinement strategy
The method of tungsten nanobelt.
Background technique
One-dimensional nano structure, such as nanometer rods, nano wire and nanobelt, have been widely studied in the past twenty years,
Since quantum confined effect makes one-dimensional nano structure have special electronic band structure, and show peculiar physical
Matter has important basic research value and scientific meaning.In recent years, researcher has successfully synthesized atom level thickness
The graphene nanobelt of degree, the study found that the graphene nanobelt of 10 nanometers or less width shows semiconductor property, with its system
Standby field effect transistor, on-off ratio have reached 107.This new one-dimensional carbon nanomaterial is in following nanoscale electronics
In have broad application prospects.
The semimetal characteristic of graphene nanobelt opens the research boom of a spin electric device new round.As a kind of p
Type direct band-gap semicondictor material, two tungsten selenide of single layer with electrology characteristic and its potential application cause to study because of its excellent optics
The extensive concern of personnel.Two tungsten selenides with layer structure are to be stacked by three atomic layers (Se-W-Se) by Van der Waals force
Made of, belong to hexagonal crystal system.First-principles calculations based on density functional theory are the result shows that two tungsten selenide of armchair
Nanobelt shows characteristic of semiconductor, and zigzag nanobelt then shows metallicity, in photoelectron, luminescent device and energy etc.
Field shows potential application value.Meanwhile when two tungsten selenide materials are reduced to by two dimension one-dimensional, thermoelectricity capability mentions significantly
Height, for armchair nanobelt, for thermoelectricity capability index at room temperature up to 2.2, this is mainly nanobelt edge
Existing dangling bonds introduce it is unordered caused by.Simultaneously because having edge nanostructure abundant, two tungsten selenide nanobelts
It is also with a wide range of applications in fields such as Novel super capacitor, lithium ion battery and electrocatalytic hydrogen evolution reactions.
The precondition for realizing above-mentioned physical property research and explorative research is the single layer two for preparing high quality, high-aspect-ratio
Tungsten selenide nanobelt.The method for the preparation nanobelt material reported at present is mainly template and solvent method, although both sides
Method can obtain relatively narrow nanobelt, but preparation method is complicated for operation, preparation cost is higher, cannot achieve industrial applications.
It is usually required using common chemical vapour deposition technique plus salt can just prepare two tungsten selenide nanobelts, but this method is due to salt
Use introduce impurity in the material inevitably to reduce the quality of sample, eventually affect subsequent device preparation process
With the performance of device.
Chinese invention CN201810078755 provides a kind of method for preparing two tungsten selenide monocrystalline of large area single layer, report
Road uses CVD method, with WO3For precursor preparation single layer WSe2The method of nanometer sheet, this method have generation in two-dimensional material
Table in the technical process used, only with argon gas as carrier gas, is added dropwise NaCl solution with liquid-transfering gun in growth substrate and locates in advance
Reason, but this method can only grow single layer WSe2Triangular nano piece, cannot get monodimension nanometer material, to limit the device of material
Part application, while the addition of NaCl salt inevitably can introduce foreign ion and influence the purity of product, and add after salt
The salt product occurred in growth substrate influences whether subsequent device preparation process and device performance.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing two tungsten selenide nanobelt of single layer based on space confinement strategy,
Under space confinement strategy, adjustable one-dimensional two tungsten selenide of the method controllable preparation width and thickness of aumospheric pressure cvd is utilized
Nanobelt.Two tungsten selenide nanobelts the fields such as hydrodesulfurization reaction, evolving hydrogen reaction, spintronics have show it is excellent
Performance, and two tungsten selenide nanobelts in air stablize by property, to study one dimension semiconductor transient metal chalcogenide compound material
Optics, electricity and the magnetism characteristic of material provide the platform of nanoscale experiment.
In order to achieve the above objectives, the technical solution adopted by the present invention are as follows:
A method of two tungsten selenide nanobelt of single layer is prepared based on space confinement strategy, is included the following steps:
(1) substrate is started the cleaning processing；
It (2) will by air-flow by the sequence of upstream to downstream by the heated center of treated substrate is placed in high temperature process furnances
Aluminium oxide boat equipped with selenium powder is placed in upstream (close to nozzle), and the boat equipped with tungstic acid and substrate is placed in the heating in downstream
Center；
(3) it is passed through argon gas and hydrogen into the reaction chamber of high temperature process furnances, reaction chamber is cleaned；
(4) temperature of tube furnace is increased to 800~850 DEG C, so that the temperature of selenium powder be made to control in 400~450 DEG C, three oxygen
The temperature for changing tungsten is controlled at 800~850 DEG C, carries out the growth of two tungsten selenides；
After (5) two tungsten selenides are grown, temperature is down to room temperature, simultaneously closes off argon gas and hydrogen to get two selenium of single layer is arrived
Change tungsten nanobelt.
Preferably, in step (1), substrate is silica substrate, sapphire substrates, graphene-based bottom, mica substrate, glass
One or both of glass substrate and monocrystal silicon substrate.
Preferably, in step (1), the mass ratio of selenium powder and tungstic acid is 430~500:15~30.
Preferably, in step (2), the boat equipped with tungstic acid and substrate is device by the following method: by one piece of substrate
Piece is smooth to be placed on aluminium oxide boat upward, then tungsten trioxide powder is sprinkled upon thereon, then smooth with another piece of substrate sheet
It covers on tungsten trioxide powder face-down, forms the reaction microchamber of class " sandwich " structure.
Preferably, in step (2), substrate before use, successively cleaned in acetone, isopropanol, ethyl alcohol and deionized water, then
With being dried with nitrogen, the cleaning of substrate is completed.
Preferably, in step (3), argon gas accounts for the 6~9% of argon gas and hydrogen total volume.
Preferably, in step (3), the flow of argon gas is 60~80sccm, and the flow of hydrogen is 7~15sccm.
Preferably, in step (4), growth time is 8 to 30 minutes.
The present invention has the advantages that compared with prior art
(1) present invention realizes two tungsten selenide nanobelt of single layer using chemical vapour deposition technique by space confinement strategy
Successful preparation, for two tungsten selenide nanobelt width range of gained at 0.17-1.62 microns, single layer nanometer tape thickness is about 0.7 to receive
Rice.
(2) carrier gas of the invention is gaseous mixture, and trace hydrogen can react acquisition as one of reactant with tungstic acid
Micro W can also react with selenium powder and generate micro H2Se, experiment, which shows trace hydrogen just, can remarkably promote the progress of reaction,
Improve yield.
(3) method of the invention does not need volume outside heating, avoids and introduces foreign ion into product, and at high temperature not
Tube furnace and quartz ampoule can be caused to corrode, and also do not have salt product in growth substrate, it will not be to the preparation of subsequent device
Journey and performance have an impact, therefore not only quality is more excellent, upper also advantageously in application.
(4) the main device tube furnace that the present invention uses is common tube furnace, does not need to carry out zonal control to temperature, only
Reaction requirement is just only able to satisfy by the appropriate adjustment of placement position, it is low for equipment requirements.
(5) aumospheric pressure cvd method reproducibility of the invention is good, and high uniform, two selenizing of high quality may be implemented
It is prepared by the batch of tungsten nanobelt.
(6) resulting materials of the present invention are two tungsten selenide nanobelts, i.e. monodimension nanometer material, and it is aobvious can directly to carry out atomic force
The characterization such as micro mirror, Kelvin probe microscope, scanning electron microscope, transmission electron microscope, and then it is microcosmic that its may be implemented
The exploration of pattern and electronic structure；
(7) present invention is designed by presoma, may be implemented what chemical vapour deposition technique grew two tungsten selenide nanobelts
Regulation.
Detailed description of the invention
Fig. 1 is that the optics of the two tungsten selenide nanobelt of single layer based on the preparation of space confinement strategy corresponding to embodiment 1 is aobvious
Micro mirror characterization result；
Fig. 2 is the Raman table of the two tungsten selenide nanobelt of single layer based on the preparation of space confinement strategy corresponding to embodiment 3
Levy result；
Fig. 3 is the atomic force of the two tungsten selenide nanobelt of single layer based on the preparation of space confinement strategy corresponding to embodiment 2
Microscopic characterization result.
Fig. 4 is the scanning electricity of the two tungsten selenide nanobelt of single layer based on the preparation of space confinement strategy corresponding to embodiment 2
Sub- microscopic characterization result.
Specific embodiment
With the drawings and specific embodiments, the present invention is described in further detail below, but the present invention is not limited to
This.
Embodiment 1
The titanium dioxide silicon wafer of purchase is sequentially placed into ethyl alcohol and deionized water and is cleaned, followed in turn by being dried with nitrogen.
Cleaned titanium dioxide silicon wafer is placed in the heated center of high temperature process furnances, according to air-flow by the sequence of upstream to downstream,
It is sequentially placed into selenium powder (close to the upstream of nozzle), tungstic acid and titanium dioxide silicon wafer (heated center in downstream), (anhydrous wolframic acid powder
End is sprinkled upon between two panels silicon wafer).The quality of selenium powder and tungstic acid is respectively 430~500mg and 15~30mg, selenium powder and three oxygen
Changing the distance between tungsten is 24cm.Then to argon gas (500sccm) is passed through in reaction chamber, reaction chamber is cleaned, chamber is discharged
Remaining air in vivo, scavenging period are 30 minutes.Subsequent temperature programming control tubular type furnace temperature is 800~850 DEG C, so that control
The temperature of selenium powder and anhydrous wolframic acid powder processed is respectively 400~450 DEG C and 800~850 DEG C.Argon gas (80sccm) and hydrogen (7~
It 15sccm) is used as carrier gas, the reactivity species of two tungsten selenides are transported to the life for realizing two tungsten selenides in silica substrate
Long, the growth time of two tungsten selenides is 8~30 minutes adjustable.After growth, it is down to room temperature to tubular type furnace temperature, is simultaneously closed off
Argon gas and hydrogen begin to speak to take out sample.
Two tungsten selenide nanometer carry sample of gained is subjected to optical microscopy, Raman, atomic force microscope, scanning electron microscopy
Mirror characterization, as a result as shown in figures 1-4.It can be seen that by optical microscopy characterize data, on two selenizing W film of single layer, two selenium
Change tungsten nanobelt to be grown according to certain rules on it, by surrounding to centre, spiral growth.It can be seen by Raman characterization data
Out, sample is in 250cm-1And 260cm-1Neighbouring appearance is two tungsten selenide E through comparing with document really2g 1And A1gPeak.By atom
Force microscope and scanning electron microscope characterize data can be seen that single nanobelt average height is 0.7nm, and mean breadth is
300nm, and be evenly distributed.
Embodiment 2~36
By the silica in embodiment 1-silica substrate sapphire-sapphire substrates, graphene-graphite
Alkenyl bottom, mica-mica substrate, glass-substrate of glass, monocrystalline silicon-monocrystalline silicon silicon base and any two kinds of these substrates
Combination replaces, other preparation conditions are constant, and the preferable two tungsten selenides nanobelt of quality also can be obtained.
Embodiment 37~72
The substrate of various two panels combination in embodiment 2~36 is subjected to vertical stacking, other preparation conditions are constant, can also
Obtain the preferable two tungsten selenides nanobelt of quality.
It should be noted last that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting.Although ginseng
It is described the invention in detail according to embodiment, it will be apparent to an ordinarily skilled person in the art that technical side of the invention
Case is modified or replaced equivalently, and without departure from the spirit and scope of technical solution of the present invention, should all be covered in the present invention
Scope of the claims in.
Claims (8)
1. a kind of method for preparing two tungsten selenide nanobelt of single layer based on space confinement strategy, which is characterized in that including walking as follows
It is rapid:
(1) substrate is started the cleaning processing；
(2) heated center of treated substrate is placed in high temperature process furnances will be equipped with by air-flow by the sequence of upstream to downstream
The aluminium oxide boat of selenium powder is placed in upstream, and the boat equipped with tungstic acid and substrate is placed in the heated center in downstream；
(3) it is passed through argon gas and hydrogen into the reaction chamber of high temperature process furnances, reaction chamber is cleaned；
(4) temperature of tube furnace is increased to 800~850 DEG C, so that the temperature of selenium powder be made to control in 400~450 DEG C, tungstic acid
Temperature control at 800~850 DEG C, carry out two tungsten selenides growth；
After (5) two tungsten selenides are grown, temperature is down to room temperature, simultaneously closes off argon gas and hydrogen to get two tungsten selenide of single layer is arrived
Nanobelt.
2. the method according to claim 1 for preparing two tungsten selenide nanobelt of single layer based on space confinement strategy, feature
It is, in step (1), substrate is silica substrate, sapphire substrates, graphene-based bottom, mica substrate, substrate of glass and list
One or both of crystal silicon substrate.
3. the method according to claim 1 for preparing two tungsten selenide nanobelt of single layer based on space confinement strategy, feature
It is, in step (1), the mass ratio of selenium powder and tungstic acid is 430~500:15~30.
4. the method according to claim 1 for preparing two tungsten selenide nanobelt of single layer based on space confinement strategy, feature
It is, in step (2), the boat equipped with tungstic acid and substrate is device by the following method: by one piece of substrate sheet shiny surface court
Shangdi is placed on aluminium oxide boat, then tungsten trioxide powder is sprinkled upon thereon, is then covered face-down with another piece of substrate sheet is smooth
On tungsten trioxide powder, the reaction microchamber of class " sandwich " structure is formed.
5. the method according to claim 1 for preparing two tungsten selenide nanobelt of single layer based on space confinement strategy, feature
It is, in step (2), substrate in acetone, isopropanol, ethyl alcohol and deionized water before use, successively clean, then blown with nitrogen
It is dry, complete the cleaning of substrate.
6. the method according to claim 1 for preparing two tungsten selenide nanobelt of single layer based on space confinement strategy, feature
It is, in step (3), argon gas accounts for the 6~9% of argon gas and hydrogen total volume.
7. the method according to claim 1 for preparing two tungsten selenide nanobelt of single layer based on space confinement strategy, feature
It is, in step (3), the flow of argon gas is 60~80sccm, and the flow of hydrogen is 7~15sccm.
8. the method according to claim 1 for preparing two tungsten selenide nanobelt of single layer based on space confinement strategy, feature
It is, in step (4), growth time is 8 to 30 minutes.
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| CN110155959A (en) * | 2019-05-31 | 2019-08-23 | 西北工业大学 | The confinement chemical gas-phase deposition process for preparing of two-dimentional transition metal alloy chalcogenide |
| CN110510585A (en) * | 2019-09-30 | 2019-11-29 | 福州大学 | A kind of preparation method of large area thin layer two dimension tellurium alkene |
| CN110790313A (en) * | 2019-12-18 | 2020-02-14 | 湘潭大学 | Preparation method of 3R phase transition metal chalcogenide two-dimensional nanosheet |
| CN112938909A (en) * | 2021-03-29 | 2021-06-11 | 湘潭大学 | Preparation method of tungsten ditelluride nanoribbon |
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| CN113511681A (en) * | 2020-04-09 | 2021-10-19 | 北京大学 | Method for locally growing transition metal chalcogenide with assistance of chalcogenide wafer |
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| CN110155959B (en) * | 2019-05-31 | 2022-08-23 | 西北工业大学 | Method for preparing two-dimensional transition metal alloy chalcogenide by limited-area chemical vapor deposition |
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| CN113511681A (en) * | 2020-04-09 | 2021-10-19 | 北京大学 | Method for locally growing transition metal chalcogenide with assistance of chalcogenide wafer |
| CN112938909A (en) * | 2021-03-29 | 2021-06-11 | 湘潭大学 | Preparation method of tungsten ditelluride nanoribbon |
| CN113173562A (en) * | 2021-05-17 | 2021-07-27 | 福州大学 | Preparation method of metallic ditelluride |
| CN113173562B (en) * | 2021-05-17 | 2022-10-21 | 福州大学 | Preparation method of metallic ditelluride |
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