CN105821391B - A kind of controllable fast preparation method of vertical substrate grown tungsten selenide nano sheet film materials - Google Patents
A kind of controllable fast preparation method of vertical substrate grown tungsten selenide nano sheet film materials Download PDFInfo
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- CN105821391B CN105821391B CN201610407882.2A CN201610407882A CN105821391B CN 105821391 B CN105821391 B CN 105821391B CN 201610407882 A CN201610407882 A CN 201610407882A CN 105821391 B CN105821391 B CN 105821391B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5846—Reactive treatment
- C23C14/5866—Treatment with sulfur, selenium or tellurium
Abstract
The invention discloses a kind of controllable fast preparation method of vertical substrate grown tungsten selenide nano sheet film materials, this method is on a quartz substrate by magnetically controlled DC sputtering W film, and the method for recycling quick selenizing W film prepares the WSe of vertical substrate grown2Nanometer sheet film；This method is simple, quick, low cost, can quickly prepare the WSe of large area vertical substrate grown2Nano sheet film materials can meet the needs of electrolytic hydrogen production and electro-catalysis application.
Description
Technical field
The present invention relates to a kind of preparation method of selenizing W film, more particularly to a kind of vertical substrate grown tungsten selenide nanometer
The controllable fast preparation method of sheet film materials, belongs to technical field of semiconductor.
Background technology
Tungsten selenide (WSe2) be a type graphite laminate structure semi-conducting material, with Se-W-Se close-packed hexagonal compact reactors
The WSe that product forms2Crystal is combined into WSe by Van der Waals force2Material.WSe2The energy gap of thin-film material is 1-2eV, and
(＞ 10 especially high to visible absorption efficiency5cm-1), it can be as the absorbed layer of solar cell and photoelectric chemical electrode material
Material.General WSe2There are two kinds of texture in polycrystal film material：C axis ⊥ substrate growns texture (Van der Waals plane is parallel to substrate)
With C axis ∥ substrate growns texture (Van der Waals plane is perpendicular to substrate), as shown in Figure 1.Texture (the vertical substrate of C axis ∥ substrates
Grow WSe2Nanometer sheet) film surface is made of many dangling bonds, and suspension key surface can cause the serious of photo-generate electron-hole
It is compound, photoelectric properties are influenced, but in electrolytic hydrogen production and electro-catalysis application, suspension key surface is active site, increases C axis ∥ bases
The texture degree at bottom can promote catalytic activity.
- Waldau A etc. prepare two kinds of different texture WSe using " soft selenizing method " at first2Film passes through control
The thickness of selenylation reaction temperature processed and radio-frequency sputtering W film prepares the WSe of C axis ∥ substrates2Film, but the technique needs 18-
The longer selenizing time of 24 hours, inefficiency (Thin Solid Films, 1991,200 (1):157-164.)；
Velazquez J M etc. have prepared the thin of the C axis ∥ substrates of suitable electrolytic hydrogen production using physical vapor transport on tungsten foil
Film, but react and use WSe2Powder and WO2Cl2Etc. expensive raw materials, and need two day reaction time seriously affect its popularization and application
(Journal of Electroanalytical Chemistry,2014,716(3):45-48).
Thus, a kind of simple, quick, environmental-friendly method is developed to prepare the WSe of C axis ∥ substrates2Film is compeled in eyebrow
Eyelash.
Invention content
For the existing method for preparing vertical substrate grown tungsten selenide nano sheet film materials there are the defects of, the present invention
Purpose be to be to provide a kind of method that simple, quick, low cost prepares vertical substrate grown tungsten selenide nanometer sheet film, should
Method can prepare large area vertical substrate grown tungsten selenide nano sheet film materials, can meet electrolytic hydrogen production and electro-catalysis application
Demand.
In order to realize above-mentioned technical purpose, technical scheme of the present invention provides a kind of vertical substrate grown tungsten selenide nanometer
The controllable fast preparation method of sheet film materials, this method include the following steps：
1) after substrate is placed in magnetron sputtering room, the magnetron sputtering chamber is evacuated to 1.0 × 10-3Pa is hereinafter, with argon
Gas is working gas, using tungsten target material as sputtering source, controls the pressure of working gas in the range of 0.9Pa~10.0Pa, is carried out straight
Magnetron sputtering is flowed, W film is generated in substrate surface；
2) selenium powder is added in open-top receptacle, by the substrate cap of Surface Creation W film on the open-top receptacle, and
The selenium powder that the W film of substrate surface is faced in the open-top receptacle is placed；The open-top receptacle is placed in closed container again,
The closed container is placed in vacuum degree less than 10Pa, under conditions of temperature is 550 DEG C~1000 DEG C, is heat-treated, cooled down, i.e.,
.
Technical scheme of the present invention mainly regulates and controls presoma by controlling the process conditions of magnetically controlled DC sputtering W film
The microstructure of W film recycles quick selenizing technique to high-efficiency to prepare vertical substrate grown tungsten selenide nanometer sheet film (C axis
The WSe of ∥ substrates2Film), to meet the application requirement of electrolytic hydrogen production and electro-catalysis.Inventor is had found by numerous studies：Model
The directionality in moral Warburg Pincus face decides WSe2The growth texture of film is C axis ⊥ substrates when Van der Waals plane parallel substrate
WSe2Film is the WSe of C axis ∥ substrates when the vertical substrate of Van der Waals plane2Film.WSe is prepared by W film selenizing method2
The apparent volume expansion of W film can be caused in thin-film process, main expansion the reason is that Van der Waals plane and with parallel selenium atom
The insertion of layer, expansion direction is mainly along C axis directions.Numerous studies show：Control working gas pressure 0.9Pa~
In the range of 10.0Pa, when carrying out magnetically controlled DC sputtering, compared under hyperbar, the W film microstructure of preparation is more loose, favorably
It is inserted into W film along vertical substrate direction in Van der Waals plane and selenium atom layer in parallel, thus, W prepared by hyperbar
The Van der Waals plane that film is conducive to vertical direction is the WSe of C axis ∥ substrates2Film.
Preferred scheme, the distance between the tungsten target material and the substrate are 3~20cm.
Preferred scheme, the power of the magnetically controlled DC sputtering is 40W~150W, is biased as -200V~0V.
More preferably scheme, the magnetically controlled DC sputtering time are 2~60min.
Preferred scheme, underlayer temperature is room temperature~500 DEG C during magnetically controlled DC sputtering.
Preferred scheme, heat treatment time are 5~60 minutes.
Preferred scheme, the purity of the argon gas are not less than 99.9%.
Preferred scheme, the purity of the tungsten target material are not less than 99.99%.
Preferred scheme, quartz substrate of the invention need to generally use acetone and absolute ethyl alcohol etc. to carry out being cleaned by ultrasonic pre- place
Reason.
The open-top receptacle that the present invention uses is generally using corundum material open-top receptacle, generally using corundum crucible.
The present invention, generally also using corundum material closed container, may be used two corundum boats and tip upside down on using closed container
Simple closed container is formed together.
The heat treatment process of the present invention generally realizes that tube furnace includes the quartz ampoule of vacuum-pumping in tube furnace.
Compared with the prior art, the advantageous effect that technical scheme of the present invention is brought：
Technical scheme of the present invention can obtain the WSe of pattern rule, the C axis ∥ substrates of large area2Film.
Technical scheme of the present invention is easy to during magnetically controlled DC sputtering prepares presoma W film by controlling work
Gas pressure realizes WSe in the range of 0.9Pa~10.0Pa2The regulation and control of the vertical sheet amount of crystals of film surface, can obtain
The WSe of the C axis ∥ substrates of different application requirement2Film.
The WSe of the C axis ∥ substrates of the present invention2Thin film preparation process has the characteristics that simple, quick, at low cost, is easy to real
Existing large area production, meets industrialization production requirements.
Description of the drawings
【Fig. 1】WSe2Film texture figure；
【Fig. 2】Quick selenizing device figure and selenidation process；
【Fig. 3】WSe obtained by Examples 1 to 32The surface SEM figures of film；
【Fig. 4】WSe obtained by Examples 1 to 32The X ray diffracting spectrum of film.
Specific embodiment
Following embodiment is intended to further illustrate the content of present invention rather than limits the scope of the invention.Embodiment 1
The present embodiment includes the following steps：
(1) substrate processing
Using 25mm × 25mm × 1mm quartz glass as substrate, it is sequentially placed into acetone and absolute ethyl alcohol and is ultrasonically treated
15min is then immersed in absolute ethyl alcohol, is dried up for use with high pure nitrogen (99.999%) when being directly placed into sputtering chamber；
(2) magnetically controlled DC sputtering bilayer W film
Using high-purity tungsten target material (99.995%) of a diameter of 60mm, W film is prepared using magnetically controlled DC sputtering.By magnetic control
The vacuum of sputtering chamber is evacuated to less than or equal to 4.1 × 10-4Pa, target are set as 15.3cm, base reservoir temperature room temperature, nothing with substrate distance
Operating pressure with high-purity argon gas (99.999%) for working gas, is adjusted to 0.9Pa and splashed by sputtering bias-voltage, sputtering power 120W
10min is penetrated, prepares W film.
(3) quick selenizing
The high-purity selenium powders of 0.7g are weighed, are put into 3mm corundum crucibles, sputtering is had into tipping upside down on crucible on one side for W film,
It puts it into two and is buckled to and together, serve in certain closed corundum boat, then boat is put into tube furnace.Utilize machine
Quartz ampoule vacuum is evacuated to less than or equal to 1.0Pa by tool pump.There is not sample area to be heated to 600 DEG C in sliding rail stove, then by it
The sample area that furnace body is pushed into quickly heats sample, keeps the temperature 30 minutes, and heating terminates, and closes power supply, sample cooled to room temperature.
Embodiment 2
The operating air pressure of the deposition of step (2) second layer W film is 2.0Pa in the present embodiment, other implementation conditions and reality
It is identical to apply example 1.
Embodiment 3
The present embodiment includes the following steps：
(1) substrate processing
Using 25mm × 25mm × 1mm quartz glass as substrate, it is sequentially placed into acetone and absolute ethyl alcohol and is ultrasonically treated
15min is then immersed in absolute ethyl alcohol, is dried up for use with high pure nitrogen (99.999%) when being directly placed into sputtering chamber；
(2) magnetically controlled DC sputtering bilayer W film
Using high-purity tungsten target material (99.995%) of a diameter of 60mm, W film is prepared using magnetically controlled DC sputtering.By magnetic control
The vacuum of sputtering chamber is evacuated to less than or equal to 8.0 × 10-4Pa, target are set as 20cm with substrate distance, and 300 DEG C of base reservoir temperature is splashed
Bias is penetrated as -100V, sputtering power 80W, with high-purity argon gas (99.999%) for working gas, operating pressure is adjusted to 5Pa
40min is sputtered, prepares W film.
(3) quick selenizing
The high-purity selenium powders of 0.7g are weighed, are put into 3mm corundum crucibles, sputtering is had into tipping upside down on crucible on one side for W film,
It puts it into two and is buckled to and together, serve in certain closed corundum boat, then boat is put into tube furnace.Utilize machine
Quartz ampoule vacuum is evacuated to less than or equal to 1.0Pa by tool pump.There is not sample area to be heated to 820 DEG C in sliding rail stove, then by it
The sample area that furnace body is pushed into quickly heats sample, keeps the temperature 15 minutes, and heating terminates, and closes power supply, sample cooled to room temperature.
It prepares
As shown in figure 3, the WSe prepared to Examples 1 to 32Film surface has carried out SEM detections.Wherein, from embodiment 1
WSe2The WSe of Fig. 3 .a and embodiment 22Fig. 3 .b can see, and when other conditions are identical, is prepared by low pressure W film
The WSe arrived2Less (the embodiment 1 of the vertical flat crystal of film surface:Fig. 3 a).And with the raising of air pressure, film surface sheet
Brilliant density dramatically increases, and can obtain the WSe of C axis ∥ base plane texture2Film (embodiment 2:Fig. 3 b).
As shown in figure 4, the WSe prepared to Examples 1 to 32Film surface has carried out XRD detections.By the WSe of embodiment 12
The WSe of Fig. 4 .a and embodiment 22Result in Fig. 4 .b, with the raising of air pressure, is prepared as it can be seen that when other conditions are identical
WSe2Film (002) crystal orientation characteristic peak gradually weakens (Examples 1 and 2).When air pressure reaches 5.0Pa, WSe2Film (002)
Crystal orientation characteristic peak almost disappears, only WSe2Film (100) (110) characteristic peak (embodiment 3) according to Fig. 1, obtains C axis ∥ bases
The WSe of baseplane texture2Film.XRD results fit like a glove unanimously with SEM results.
Claims (2)
1. a kind of controllable fast preparation method of vertical substrate grown tungsten selenide nano sheet film materials, it is characterised in that：Including
Following steps：
1) after substrate is placed in magnetron sputtering room, the magnetron sputtering chamber is evacuated to 1.0 × 10-3Pa hereinafter, using argon gas as
Working gas using tungsten target material as sputtering source, controls the pressure of working gas in the range of 0.9Pa~10.0Pa, carries out DC magnetic
Control sputtering generates W film in substrate surface；The distance between the tungsten target material and the substrate are 3~20cm；The direct current
The power of magnetron sputtering is 40W~150W, is biased as -200V~0V；The magnetically controlled DC sputtering time is 2~60min；Directly
It is room temperature~500 DEG C to flow underlayer temperature in magnetron sputtering process；
2) selenium powder is added in open-top receptacle, by the substrate cap of Surface Creation W film on the open-top receptacle, and substrate
The selenium powder that the W film on surface is faced in the open-top receptacle is placed；The open-top receptacle is placed in closed container again, it is described
Closed container is placed in vacuum degree less than 10Pa, under conditions of temperature is 550 DEG C~1000 DEG C, is heat-treated, cool down to get；
Heat treatment time is 5~60 minutes.
2. the controllable fast preparation method of vertical substrate grown tungsten selenide nano sheet film materials according to claim 1,
It is characterized in that：The purity of the argon gas is not less than 99.9%；The purity of the tungsten target material is not less than 99.99%.
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| CN106835062A (en) * | 2017-01-22 | 2017-06-13 | 福州大学 | A kind of method that utilization laser quickly prepares Transition-metal dichalcogenide |
| CN107475694B (en) * | 2017-06-20 | 2019-10-18 | 广东工业大学 | A kind of method and its application preparing two tungsten selenide semiconductive thin films on FTO substrate |
| CN108546924B (en) * | 2018-05-14 | 2021-02-02 | 中南大学 | Molybdenum diselenide/graphite composite material and preparation method and application thereof |
| CN110195214A (en) * | 2019-07-15 | 2019-09-03 | 中南大学 | A kind of MSe2Thin-film material and its preparation method and application |
| CN111690897B (en) * | 2020-06-23 | 2021-06-08 | 南京大学 | Tungsten diselenide thin film of single primitive cell layer and growth method thereof |
| CN114645247B (en) * | 2022-03-23 | 2022-11-04 | 中南大学 | Iron diselenide nano film with controllable shape as nano rod and preparation method thereof |
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| US20160093491A1 (en) * | 2014-09-29 | 2016-03-31 | University Of North Texas | LARGE SCALE AND THICKNESS-MODULATED MoS2 NANOSHEETS |
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