CN108766864A - A method of preparing two-dimentional tungsten selenide rule laminar sheet in quartz plate substrate - Google Patents
A method of preparing two-dimentional tungsten selenide rule laminar sheet in quartz plate substrate Download PDFInfo
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- CN108766864A CN108766864A CN201810265876.7A CN201810265876A CN108766864A CN 108766864 A CN108766864 A CN 108766864A CN 201810265876 A CN201810265876 A CN 201810265876A CN 108766864 A CN108766864 A CN 108766864A
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- rule
- quartz plate
- laminar sheet
- tungsten selenide
- dimentional
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02057—Cleaning during device manufacture
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
Abstract
The method that the invention discloses a kind of to prepare tungsten selenide rule laminar sheet in quartz plate substrate, includes the following steps：S1：Prior surface cleaning treatment is carried out to quartz plate；S2：Solvent, selenium source, tungsten source and reproducibility reagent are uniformly mixed obtained reaction precursor liquid；S3：The reaction precursor liquid of quartz plate and step S2 through step S1 cleaning treatments is come into full contact with, after fully being reacted under conditions of high temperature and pressure, two-dimentional tungsten selenide rule laminar sheet is prepared on quartz plate.The tungsten selenide rule stratiform method for preparing slices of the present invention have many advantages, such as preparation process it is simple, it is at low cost, can directly obtain that purity is higher, the smaller tungsten selenide rule laminar sheet of thickness, and by the tungsten selenide rule laminar sheet prepared by the present invention in optical detector and field-effect transistor with good application.
Description
Technical field
The present invention relates to semiconductor rule laminar sheet preparing technical fields, especially relate to a kind of based on solvent heat seal
Method and the application of two-dimensional tungsten selenide rule laminar sheet are directly prepared on quartz plate at technology.
Background technology
Quartz plate has silica (SiO2) content up to 99.99% or more, has high temperature resistant, electrical insulation capability good
The features such as.For tungsten selenide (WSe2), it is defeated with unique band structure (energy gap is about 1.66eV), good electronics
Transport characteristic, it is of low cost and without toxic element, steady performance.Therefore, it is remembered as a kind of excellent for developing
The material of good photoelectric device.
Currently, common WSe2The preparation method of regular layer structure is generally mechanical stripping method, chemical vapor deposition
The methods of (CVD).And relative to chemical vapor deposition, solvent-thermal process rule has simple for process, low production cost, energy consumption
It is small and can directly obtain object mutually uniformly, purity is higher, thickness is smaller product the advantages that.And pass through solvent-thermal method or hydro-thermal
Method prepares the more understatement road of two-dimensional regular layer structure.
Invention content
In order to solve the problem above-mentioned, the object of the present invention is to provide one kind preparing two-dimentional tungsten selenide in quartz plate substrate
The method of regular laminar sheet.
The technical solution adopted in the present invention is：One kind preparing two-dimentional tungsten selenide rule laminar sheet in quartz plate substrate
Method, include the following steps：
S1：Prior surface cleaning treatment is carried out to quartz plate；
S2：Solvent, selenium source, tungsten source and reproducibility reagent are uniformly mixed obtained reaction precursor liquid；
S3：The reaction precursor liquid of quartz plate and step S2 through step S1 cleaning treatments is come into full contact with, in high temperature and pressure
Under conditions of fully react after, two-dimentional tungsten selenide rule laminar sheet is prepared on quartz plate.The step S1 is specially：
Quartz plate is put into beaker, uses acetone, absolute ethyl alcohol to be respectively cleaned by ultrasonic 10min successively, after cleaning, with clean tweezer
Son rinses quartz plate with deionized water after being taken out in beaker, is finally dried up with hair-dryer.
The step S2 is specially：After reproducibility reagent first is added in a solvent, magnetic agitation is utilized；Then, add successively
After entering selenium source and tungsten source, using magnetic agitation to abundant dissolving, it is uniformly mixed and obtains reaction precursor liquid.
The step S3 is specially：The quartz plate cleaned up is put into the clean inner liner of reaction kettle of 100ml, is leant against
Inner liner of reaction kettle bottom interior wall；Then the reaction precursor liquid of step S2 is poured slowly into the inner liner of reaction kettle, puts on stainless steel
Outer lining, which is put into air blast thermostatic drying chamber, carries out isothermal reaction, and after isothermal reaction, quartz plate is taken out from reactor bottom,
It is finally dried to obtain two-dimentional tungsten selenide rule laminar sheet in a natural environment.
In step S2, the selenium source is selenium powder, and the tungsten source is sodium tungstate, and the reproducibility reagent is sodium borohydride.
In step S2, the tungsten source, selenium source, reproducibility reagent amount ratio be：1mmol：2-2.2mmol：1.3-
1.5mmol。
In step S2, the tungsten source, selenium source, reproducibility reagent amount ratio be：(2-4)mmol：(4-8.8)mmol：
(2.6-6)mmol。
In step S2, magnetic agitation 1-2 hours；In step S3, reaction kettle is put into air blast thermostatic drying chamber and carries out perseverance
When temperature reaction, setting condition is：Reaction temperature is 200 DEG C -220 DEG C, reaction time 24-48h.
Application of the prepared two-dimentional tungsten selenide rule laminar sheet in making optical detector.
Application of the prepared two-dimentional tungsten selenide rule laminar sheet in making field-effect transistor.
Compared with prior art, the beneficial effects of the invention are as follows：The system of the two-dimentional tungsten selenide rule laminar sheet of the present invention
Preparation Method simple, low production cost with preparation process, can directly obtain the selenium that object is mutually uniform, purity is higher, thickness is smaller
The advantages that changing tungsten rule laminar sheet.
It, can be making light for the preparation-obtained two-dimentional tungsten selenide rule laminar sheet of method through the invention
Detector and field-effect transistor, obtain good photoelectric properties, reduce the system of tungsten selenide photoelectric device to a certain extent
Make cost.
Description of the drawings
Fig. 1 is the optical microscope image for the two-dimentional tungsten selenide rule laminar sheet that embodiment one is prepared；
Fig. 2 is the surface SEM figures for the two-dimentional tungsten selenide rule laminar sheet that embodiment one is prepared；
Fig. 3 is the AFM figures for the two-dimentional tungsten selenide rule laminar sheet that embodiment one is prepared；
Fig. 4 is the Raman spectrogram for the two-dimentional tungsten selenide rule laminar sheet that embodiment one is prepared；
Fig. 5 is the luminescence generated by light spectrogram for the two-dimentional tungsten selenide rule laminar sheet that embodiment one is prepared.
Specific implementation mode
The technical solution further illustrated the present invention with reference to specific embodiment.
A method of it preparing two-dimentional tungsten selenide rule laminar sheet in quartz plate substrate, includes the following steps：
S1：Prior surface cleaning treatment is carried out to quartz plate；
S2：Solvent, selenium source, tungsten source and reproducibility reagent are uniformly mixed obtained reaction precursor liquid；
S3：The reaction precursor liquid of quartz plate and step S2 through step S1 cleaning treatments is come into full contact with, in high temperature and pressure
Under conditions of fully react after, two-dimentional tungsten selenide rule laminar sheet is prepared on quartz plate.The step S1 is specially：
Quartz plate is put into beaker, uses acetone, absolute ethyl alcohol to be respectively cleaned by ultrasonic 10min successively, after cleaning, with clean tweezer
Son rinses quartz plate with deionized water after being taken out in beaker, is finally dried up with hair-dryer.
The step S2 is specially：After reproducibility reagent first is added in a solvent, magnetic agitation is utilized；Then, add successively
After entering selenium source and tungsten source, using magnetic agitation to abundant dissolving, it is uniformly mixed and obtains reaction precursor liquid.
The step S3 is specially：The quartz plate cleaned up is put into the clean inner liner of reaction kettle of 100ml, is leant against
Inner liner of reaction kettle bottom interior wall；Then the reaction precursor liquid of step S2 is poured slowly into the inner liner of reaction kettle, puts on stainless steel
Outer lining, which is put into air blast thermostatic drying chamber, carries out isothermal reaction, and after isothermal reaction, quartz plate is taken out from reactor bottom,
It is finally dried to obtain two-dimentional tungsten selenide rule laminar sheet in a natural environment.
In step S2, the selenium source is selenium powder, and the tungsten source is sodium tungstate, and the reproducibility reagent is sodium borohydride.
In step S2, the tungsten source, selenium source, reproducibility reagent amount ratio be：1mmol：2-2.2mmol：1.3-
1.5mmol。
In step S2, the tungsten source, selenium source, reproducibility reagent amount ratio be：(2-4)mmol：(4-8.8)mmol：
(2.6-6)mmol。
In step S2, magnetic agitation 1-2 hours；In step S3, reaction kettle is put into air blast thermostatic drying chamber and carries out perseverance
When temperature reaction, setting condition is：Reaction temperature is 200 DEG C -220 DEG C, reaction time 24-48h.
Application of the prepared two-dimentional tungsten selenide rule laminar sheet in making optical detector.
Application of the prepared two-dimentional tungsten selenide rule laminar sheet in making field-effect transistor.
Embodiment one
A method of it preparing two-dimentional tungsten selenide rule laminar sheet in quartz plate substrate, specifically includes：
S1：Prior surface cleaning treatment is carried out to quartz plate：Quartzy sheet glass is put into beaker, successively use acetone,
Absolute ethyl alcohol is respectively cleaned by ultrasonic 10min, after cleaning, with clean tweezers sheet glass the taking-up deionized water from beaker
It rinses, is finally dried up with hair-dryer.
S2：After 5.3mmol sodium borohydrides are added in the DMF of 60ml, it is sufficiently stirred using magnetic force；Then, it sequentially adds
After 8.2mmol selenium powders and 4mmol sodium tungstates, using magnetic agitation 1-2 hours, until fully dissolving, is uniformly mixed before obtaining reaction
Drive liquid；
S3：The quartz plate cleaned up is put into the clean inner liner of reaction kettle of 100ml, inner liner of reaction kettle bottom is leant against
Inner wall；Then the reaction precursor liquid being prepared is poured slowly into the inner liner of reaction kettle, puts on stainless steel outer lining and is put into air blast
Isothermal reaction is carried out in thermostatic drying chamber.Wherein, reaction temperature is set as 200 DEG C, and the reaction time is set as reaction 48h；Isothermal reaction
After, quartz plate is taken out from reactor bottom, is finally dried in a natural environment.
Embodiment two
A method of it preparing two-dimentional tungsten selenide rule laminar sheet in quartz plate substrate, specifically includes：
S1：Prior surface cleaning treatment is carried out to quartz plate：Quartzy sheet glass is put into beaker, successively use acetone,
Absolute ethyl alcohol is respectively cleaned by ultrasonic 10min, after cleaning, with clean tweezers sheet glass the taking-up deionized water from beaker
It rinses, is finally dried up with hair-dryer.
S2：After 2.65mmol sodium borohydrides are added in the DMF of 60ml, it is sufficiently stirred using magnetic force；Then, it sequentially adds
After 4.1mmol selenium powders and 2mmol sodium tungstates, using magnetic agitation 1-2 hours, until fully dissolving, is uniformly mixed before obtaining reaction
Drive liquid；
S3：The quartz plate cleaned up is put into the clean inner liner of reaction kettle of 100ml, inner liner of reaction kettle bottom is leant against
Inner wall；Then the reaction precursor liquid being prepared is poured slowly into the inner liner of reaction kettle, puts on stainless steel outer lining and is put into air blast
Isothermal reaction is carried out in thermostatic drying chamber.Wherein, reaction temperature is set as 200 DEG C, and the reaction time is set as reaction 48h；Isothermal reaction
After, quartz plate is taken out from reactor bottom, is finally dried in a natural environment.
Embodiment three
A method of it preparing two-dimentional tungsten selenide rule laminar sheet in quartz plate substrate, specifically includes：
S1：Prior surface cleaning treatment is carried out to quartz plate：Quartzy sheet glass is put into beaker, successively use acetone,
Absolute ethyl alcohol is respectively cleaned by ultrasonic 10min, after cleaning, with clean tweezers sheet glass the taking-up deionized water from beaker
It rinses, is finally dried up with hair-dryer.
S2：After 5.3mmol sodium borohydrides are added in the DMF of 60ml, it is sufficiently stirred using magnetic force；Then, it sequentially adds
After 8.2mmol selenium powders and 4mmol sodium tungstates, using magnetic agitation 1-2 hours, until fully dissolving, is uniformly mixed before obtaining reaction
Drive liquid；
S3：The quartz plate cleaned up is put into the clean inner liner of reaction kettle of 100ml, inner liner of reaction kettle bottom is leant against
Inner wall；Then the reaction precursor liquid being prepared is poured slowly into the inner liner of reaction kettle, puts on stainless steel outer lining and is put into air blast
Isothermal reaction is carried out in thermostatic drying chamber.Wherein, reaction temperature is set as 220 DEG C, and the reaction time is set as reaction for 24 hours；Isothermal reaction
After, quartz plate is taken out from reactor bottom, is finally dried in a natural environment.
Example IV
A method of it preparing two-dimentional tungsten selenide rule laminar sheet in quartz plate substrate, specifically includes：
S1：Prior surface cleaning treatment is carried out to quartz plate：Quartzy sheet glass is put into beaker, successively use acetone,
Absolute ethyl alcohol is respectively cleaned by ultrasonic 10min, after cleaning, with clean tweezers sheet glass the taking-up deionized water from beaker
It rinses, is finally dried up with hair-dryer.
S2：After 5.3mmol sodium borohydrides are added in the DMF of 60ml, it is sufficiently stirred using magnetic force；Then, it sequentially adds
After 8.2mmol selenium powders and 4mmol sodium tungstates, using magnetic agitation 1-2 hours, until fully dissolving, is uniformly mixed before obtaining reaction
Drive liquid；
S3：The quartz plate cleaned up is put into the clean inner liner of reaction kettle of 100ml, inner liner of reaction kettle bottom is leant against
Inner wall；Then the reaction precursor liquid being prepared is poured slowly into the inner liner of reaction kettle, puts on stainless steel outer lining and is put into air blast
Isothermal reaction is carried out in thermostatic drying chamber.Wherein, reaction temperature is set as 220 DEG C, and the reaction time is set as reaction 48h；Isothermal reaction
After, quartz plate is taken out from reactor bottom, is finally dried in a natural environment.
It is obtained by above-mentioned, advantages of the present invention includes：
1, the stability of quartz plate, profile pattern and quartz plate and WSe2Similar lattice structure is to two-dimentional WSe2Rule
Then the growth of laminar sheet plays an important roll.
2, the two-dimentional WSe prepared on quartz plate2Regular laminar sheet can be used for making optical detector, obtain higher
Photoelectric properties.
4, the two-dimentional WSe prepared on quartz plate2Regular laminar sheet can be used for making field-effect transistor, obtain
Higher photoelectric properties.To replace other materials, the photoelectric device of function admirable is developed, while greatly reducing and being produced into
This.
5, preparation process is simple, low production cost, can directly obtain object mutually uniformly, purity is higher, the lower production of thickness
Object.
For those skilled in the art, technical solution that can be as described above and design are made other each
Kind is corresponding to be changed and deforms, and all these change and deform the protection model that should all belong to the claims in the present invention
Within enclosing.
Claims (10)
1. a kind of method preparing two-dimentional tungsten selenide rule laminar sheet in quartz plate substrate, it is characterised in that：Including as follows
Step：
S1：Prior surface cleaning treatment is carried out to quartz plate；
S2：Solvent, selenium source, tungsten source and reproducibility reagent are uniformly mixed obtained reaction precursor liquid；
S3：The reaction precursor liquid of quartz plate and step S2 through step S1 cleaning treatments is come into full contact with, in the item of high temperature and pressure
After fully being reacted under part, two-dimentional tungsten selenide rule laminar sheet is prepared on quartz plate.
2. a kind of method preparing two-dimentional tungsten selenide rule laminar sheet in quartz plate substrate according to claim 1,
It is characterized in that：The step S1 is specially：Quartz plate is put into beaker, uses each ultrasound of acetone, absolute ethyl alcohol clear successively
10min is washed, after cleaning, quartz plate is rinsed with deionized water after being taken out in beaker with clean tweezers, finally with blowing
Wind turbine dries up.
3. a kind of method preparing two-dimentional tungsten selenide rule laminar sheet in quartz plate substrate according to claim 1,
It is characterized in that：The step S2 is specially：After reproducibility reagent first is added in a solvent, magnetic agitation is utilized；Then, successively
After selenium source and tungsten source is added, using magnetic agitation to abundant dissolving, it is uniformly mixed and obtains reaction precursor liquid.
4. a kind of method preparing two-dimentional tungsten selenide rule laminar sheet in quartz plate substrate according to claim 1,
It is characterized in that：The step S3 is specially：The quartz plate cleaned up is put into the clean inner liner of reaction kettle of 100ml, tiltedly
Lean against inner liner of reaction kettle bottom interior wall；Then the reaction precursor liquid of step S2 is poured slowly into the inner liner of reaction kettle, is put on not
Rust steel outer lining is put into air blast thermostatic drying chamber and carries out isothermal reaction, after isothermal reaction, by quartz plate from reactor bottom
It takes out, is finally dried to obtain two-dimentional tungsten selenide rule laminar sheet in a natural environment.
5. a kind of method preparing two-dimentional tungsten selenide rule laminar sheet in quartz plate substrate according to claim 1,
It is characterized in that：In step S2, the selenium source is selenium powder, and the tungsten source is sodium tungstate, and the reproducibility reagent is sodium borohydride.
6. a kind of method preparing two-dimentional tungsten selenide rule laminar sheet in quartz plate substrate according to claim 1,
It is characterized in that：In step S2, the tungsten source, selenium source, reproducibility reagent amount ratio be：1mmol：2-2.2mmol：1.3-
1.5mmol。
7. a kind of method preparing two-dimentional tungsten selenide rule laminar sheet in quartz plate substrate according to claim 1,
It is characterized in that：In step S2, the tungsten source, selenium source, reproducibility reagent amount ratio be：(2-4)mmol：(4-8.8)mmol：
(2.6-6)mmol。
8. a kind of method preparing two-dimentional tungsten selenide rule laminar sheet in quartz plate substrate according to claim 1,
It is characterized in that：In step S2, magnetic agitation 1-2 hours；In step S3, reaction kettle is put into air blast thermostatic drying chamber and is carried out
When isothermal reaction, setting condition is：Reaction temperature is 200 DEG C -220 DEG C, reaction time 24-48h.
9. the two-dimentional tungsten selenide rule laminar sheet prepared according to claim 1-8 either method, it is characterised in that：Prepared
Application of the two-dimentional tungsten selenide rule laminar sheet in making optical detector.
10. the two-dimentional tungsten selenide rule laminar sheet prepared according to claim 1-8 either method, it is characterised in that：It is prepared
Application of the two-dimentional tungsten selenide rule laminar sheet in making field-effect transistor.
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| CN201810265876.7A CN108766864B (en) | 2018-03-28 | 2018-03-28 | Method for preparing two-dimensional tungsten selenide regular layered slice on quartz wafer substrate |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105967155A (en) * | 2016-05-10 | 2016-09-28 | 电子科技大学 | Method for preparing tungsten diselenide nanoflower |
| CN107475694A (en) * | 2017-06-20 | 2017-12-15 | 广东工业大学 | A kind of method and its application that two tungsten selenide semiconductive thin films are prepared on FTO substrates |
| CN107601443A (en) * | 2017-11-09 | 2018-01-19 | 安徽大学 | A kind of preparation method of ultra-thin tungsten selenide nanometer sheet |
-
2018
- 2018-03-28 CN CN201810265876.7A patent/CN108766864B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105967155A (en) * | 2016-05-10 | 2016-09-28 | 电子科技大学 | Method for preparing tungsten diselenide nanoflower |
| CN107475694A (en) * | 2017-06-20 | 2017-12-15 | 广东工业大学 | A kind of method and its application that two tungsten selenide semiconductive thin films are prepared on FTO substrates |
| CN107601443A (en) * | 2017-11-09 | 2018-01-19 | 安徽大学 | A kind of preparation method of ultra-thin tungsten selenide nanometer sheet |
Non-Patent Citations (2)
| Title |
|---|
| SU ET AL: "Deposition of porous few-layer WSe2 flakes with high density of exposed edge sites", 《VACUUN》 * |
| WANG ET AL20160830: "Graphene-like WSe2 nanosheets for efficient and stable hydrogen evoluation", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
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