CN108766864B - Method for preparing two-dimensional tungsten selenide regular layered slice on quartz wafer substrate - Google Patents
Method for preparing two-dimensional tungsten selenide regular layered slice on quartz wafer substrate Download PDFInfo
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- CN108766864B CN108766864B CN201810265876.7A CN201810265876A CN108766864B CN 108766864 B CN108766864 B CN 108766864B CN 201810265876 A CN201810265876 A CN 201810265876A CN 108766864 B CN108766864 B CN 108766864B
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Abstract
The invention discloses a method for preparing a tungsten selenide regular layered slice on a quartz wafer substrate, which comprises the following steps: s1: carrying out early-stage surface cleaning treatment on the quartz wafer; s2: uniformly mixing a solvent, a selenium source, a tungsten source and a reducing reagent to prepare a reaction precursor solution; s3: and (4) fully contacting the quartz plate cleaned in the step (S1) with the reaction precursor liquid in the step (S2), and preparing the two-dimensional tungsten selenide regular layered sheet on the quartz plate after fully reacting under the conditions of high temperature and high pressure. The preparation method of the tungsten selenide regular lamellar thin slice has the advantages of simple preparation process, low cost, capability of directly obtaining the tungsten selenide regular lamellar thin slice with higher purity and smaller thickness and the like, and the tungsten selenide regular lamellar thin slice prepared by the invention has good application in a photodetector and a field effect transistor.
Description
Technical Field
The invention relates to the technical field of preparation of regular layered slices of semiconductors, in particular to a method for directly preparing a two-dimensional regular layered slice of tungsten selenide on a quartz plate based on a solvothermal synthesis technology and application thereof.
Background
The quartz plate has silicon dioxide (SiO)2) The content can reach more than 99.99 percent, and the composite material has the characteristics of high temperature resistance, good electrical insulation performance and the like. For tungsten selenide (WSe)2) The material has the advantages of unique energy band structure (the forbidden band width is about 1.66eV), good electron transport property, low cost, no toxic elements, stable performance and the like. Therefore, it is considered as a material for developing an excellent photoelectric device.
Currently, WSe is common2The method for preparing the regular layered structure is generally a mechanical lift-off method, a Chemical Vapor Deposition (CVD) method, or the like. Compared with chemical vapor deposition, the solvothermal synthesis method has the advantages of simple process, low production cost, low energy consumption, capability of directly obtaining products with uniform phase, higher purity and smaller thickness and the like. By passing through a solventThermal or hydrothermal methods are less reported for the preparation of two-dimensional regular lamellar structures.
Disclosure of Invention
In order to solve the above problems, the present invention provides a method for preparing a two-dimensional tungsten selenide regular layered sheet on a quartz substrate.
The technical scheme adopted by the invention is as follows: a method for preparing a two-dimensional tungsten selenide regular layered slice on a quartz chip substrate comprises the following steps:
s1: carrying out early-stage surface cleaning treatment on the quartz wafer;
s2: uniformly mixing a solvent, a selenium source, a tungsten source and a reducing reagent to prepare a reaction precursor solution;
s3: and (4) fully contacting the quartz plate cleaned in the step (S1) with the reaction precursor liquid in the step (S2), and preparing the two-dimensional tungsten selenide regular layered sheet on the quartz plate after fully reacting under the conditions of high temperature and high pressure. The step S1 specifically includes: putting the quartz plate into a beaker, sequentially performing ultrasonic cleaning for 10min by using acetone and absolute ethyl alcohol respectively, taking the quartz plate out of the beaker by using clean tweezers after cleaning, washing the quartz plate by using deionized water, and finally drying the quartz plate by using a blower.
The step S2 specifically includes: adding a reducing reagent into a solvent, and stirring by using magnetic force; then, after the selenium source and the tungsten source are sequentially added, the mixture is stirred by magnetic force until the selenium source and the tungsten source are fully dissolved, and the mixture is uniformly mixed to obtain reaction precursor liquid.
The step S3 specifically includes: putting the cleaned quartz plate into a 100ml clean reaction kettle lining, and leaning against the inner wall of the bottom of the reaction kettle lining; and slowly pouring the reaction precursor liquid obtained in the step S2 into the inner liner of the reaction kettle, sleeving the stainless steel outer liner, putting the stainless steel outer liner into an air-blowing constant-temperature drying box for constant-temperature reaction, taking out the quartz plate from the bottom of the reaction kettle after the constant-temperature reaction is finished, and finally drying the quartz plate in a natural environment to obtain the two-dimensional tungsten selenide regular layered sheet.
In step S2, the selenium source is selenium powder, the tungsten source is sodium tungstate, and the reducing agent is sodium borohydride.
In step S2, the dosage ratio of the tungsten source, the selenium source, and the reducing agent is: 1 mmol: 2-2.2 mmol: 1.3-1.5 mmol.
In step S2, the dosage ratio of the tungsten source, the selenium source, and the reducing agent is: (2-4) mmol: (4-8.8) mmol: (2.6-6) mmol.
In step S2, stirring for 1-2 hours by magnetic force; in step S3, the reaction kettle is placed in an air-blowing constant-temperature drying oven to perform a constant-temperature reaction, and the setting conditions are as follows: the reaction temperature is 200-220 ℃, and the reaction time is 24-48 h.
The prepared two-dimensional tungsten selenide regular layered slice is applied to the manufacture of a light detector.
The prepared two-dimensional tungsten selenide regular layered slice is applied to the preparation of a field effect transistor.
Compared with the prior art, the invention has the beneficial effects that: the preparation method of the two-dimensional tungsten selenide regular lamellar slice has the advantages of simple preparation process, low production cost, capability of directly obtaining the tungsten selenide regular lamellar slice with uniform phase, higher purity and smaller thickness, and the like.
The two-dimensional tungsten selenide regular layered slice prepared by the method can be used for manufacturing a light detector and a field effect transistor, obtains good photoelectric property and reduces the manufacturing cost of a tungsten selenide photoelectric device to a certain extent.
Drawings
FIG. 1 is an optical microscope image of a two-dimensional regular lamellar sheet of tungsten selenide prepared according to example one;
FIG. 2 is a surface SEM image of a two-dimensional regular layered sheet of tungsten selenide obtained in the first preparation;
FIG. 3 is an AFM image of a two-dimensional regular layered sheet of tungsten selenide prepared in the first example;
FIG. 4 is a Raman spectrum of a two-dimensional tungsten selenide regular lamellar sheet prepared in the first example;
fig. 5 is a photoluminescence spectrum of the two-dimensional tungsten selenide regular layered sheet prepared in the first example.
Detailed Description
The technical scheme of the invention is further explained by combining specific examples.
A method for preparing a two-dimensional tungsten selenide regular layered slice on a quartz chip substrate comprises the following steps:
s1: carrying out early-stage surface cleaning treatment on the quartz wafer;
s2: uniformly mixing a solvent, a selenium source, a tungsten source and a reducing reagent to prepare a reaction precursor solution;
s3: and (4) fully contacting the quartz plate cleaned in the step (S1) with the reaction precursor liquid in the step (S2), and preparing the two-dimensional tungsten selenide regular layered sheet on the quartz plate after fully reacting under the conditions of high temperature and high pressure. The step S1 specifically includes: putting the quartz plate into a beaker, sequentially performing ultrasonic cleaning for 10min by using acetone and absolute ethyl alcohol respectively, taking the quartz plate out of the beaker by using clean tweezers after cleaning, washing the quartz plate by using deionized water, and finally drying the quartz plate by using a blower.
The step S2 specifically includes: adding a reducing reagent into a solvent, and stirring by using magnetic force; then, after the selenium source and the tungsten source are sequentially added, the mixture is stirred by magnetic force until the selenium source and the tungsten source are fully dissolved, and the mixture is uniformly mixed to obtain reaction precursor liquid.
The step S3 specifically includes: putting the cleaned quartz plate into a 100ml clean reaction kettle lining, and leaning against the inner wall of the bottom of the reaction kettle lining; and slowly pouring the reaction precursor liquid obtained in the step S2 into the inner liner of the reaction kettle, sleeving the stainless steel outer liner, putting the stainless steel outer liner into an air-blowing constant-temperature drying box for constant-temperature reaction, taking out the quartz plate from the bottom of the reaction kettle after the constant-temperature reaction is finished, and finally drying the quartz plate in a natural environment to obtain the two-dimensional tungsten selenide regular layered sheet.
In step S2, the selenium source is selenium powder, the tungsten source is sodium tungstate, and the reducing agent is sodium borohydride.
In step S2, the dosage ratio of the tungsten source, the selenium source, and the reducing agent is: 1 mmol: 2-2.2 mmol: 1.3-1.5 mmol.
In step S2, the dosage ratio of the tungsten source, the selenium source, and the reducing agent is: (2-4) mmol: (4-8.8) mmol: (2.6-6) mmol.
In step S2, stirring for 1-2 hours by magnetic force; in step S3, the reaction kettle is placed in an air-blowing constant-temperature drying oven to perform a constant-temperature reaction, and the setting conditions are as follows: the reaction temperature is 200-220 ℃, and the reaction time is 24-48 h.
The prepared two-dimensional tungsten selenide regular layered slice is applied to the manufacture of a light detector.
The prepared two-dimensional tungsten selenide regular layered slice is applied to the preparation of a field effect transistor.
Example one
A method for preparing a two-dimensional tungsten selenide regular layered slice on a quartz chip substrate specifically comprises the following steps:
s1: carrying out early-stage surface cleaning treatment on the quartz wafer: putting quartz plate glass into a beaker, sequentially performing ultrasonic cleaning for 10min by using acetone and absolute ethyl alcohol respectively, taking out the glass plate from the beaker by using clean tweezers after the cleaning is finished, washing the glass plate by using deionized water, and finally drying the glass plate by using a blower.
S2: adding 5.3mmol of sodium borohydride into 60ml of DMF, and fully stirring by using magnetic force; then, after sequentially adding 8.2mmol of selenium powder and 4mmol of sodium tungstate, stirring for 1-2 hours by using magnetic force until the selenium powder and the sodium tungstate are fully dissolved, and uniformly mixing to obtain reaction precursor liquid;
s3: putting the cleaned quartz plate into a 100ml clean reaction kettle lining, and leaning against the inner wall of the bottom of the reaction kettle lining; and slowly pouring the prepared reaction precursor liquid into the inner liner of the reaction kettle, sleeving the stainless steel outer liner, and putting the stainless steel outer liner into an air-blast constant-temperature drying oven for constant-temperature reaction. Wherein the reaction temperature is set as 200 ℃, and the reaction time is set as 48 hours; and after the constant-temperature reaction is finished, taking out the quartz plate from the bottom of the reaction kettle, and finally drying in a natural environment.
Example two
A method for preparing a two-dimensional tungsten selenide regular layered slice on a quartz chip substrate specifically comprises the following steps:
s1: carrying out early-stage surface cleaning treatment on the quartz wafer: putting quartz plate glass into a beaker, sequentially performing ultrasonic cleaning for 10min by using acetone and absolute ethyl alcohol respectively, taking out the glass plate from the beaker by using clean tweezers after the cleaning is finished, washing the glass plate by using deionized water, and finally drying the glass plate by using a blower.
S2: adding 2.65mmol of sodium borohydride into 60ml of DMF, and fully stirring by using magnetic force; then, sequentially adding 4.1mmol of selenium powder and 2mmol of sodium tungstate, stirring for 1-2 hours by using magnetic force until the selenium powder and the sodium tungstate are fully dissolved, and uniformly mixing to obtain reaction precursor liquid;
s3: putting the cleaned quartz plate into a 100ml clean reaction kettle lining, and leaning against the inner wall of the bottom of the reaction kettle lining; and slowly pouring the prepared reaction precursor liquid into the inner liner of the reaction kettle, sleeving the stainless steel outer liner, and putting the stainless steel outer liner into an air-blast constant-temperature drying oven for constant-temperature reaction. Wherein the reaction temperature is set as 200 ℃, and the reaction time is set as 48 hours; and after the constant-temperature reaction is finished, taking out the quartz plate from the bottom of the reaction kettle, and finally drying in a natural environment.
EXAMPLE III
A method for preparing a two-dimensional tungsten selenide regular layered slice on a quartz chip substrate specifically comprises the following steps:
s1: carrying out early-stage surface cleaning treatment on the quartz wafer: putting quartz plate glass into a beaker, sequentially performing ultrasonic cleaning for 10min by using acetone and absolute ethyl alcohol respectively, taking out the glass plate from the beaker by using clean tweezers after the cleaning is finished, washing the glass plate by using deionized water, and finally drying the glass plate by using a blower.
S2: adding 5.3mmol of sodium borohydride into 60ml of DMF, and fully stirring by using magnetic force; then, after sequentially adding 8.2mmol of selenium powder and 4mmol of sodium tungstate, stirring for 1-2 hours by using magnetic force until the selenium powder and the sodium tungstate are fully dissolved, and uniformly mixing to obtain reaction precursor liquid;
s3: putting the cleaned quartz plate into a 100ml clean reaction kettle lining, and leaning against the inner wall of the bottom of the reaction kettle lining; and slowly pouring the prepared reaction precursor liquid into the inner liner of the reaction kettle, sleeving the stainless steel outer liner, and putting the stainless steel outer liner into an air-blast constant-temperature drying oven for constant-temperature reaction. Wherein the reaction temperature is set as 220 ℃, and the reaction time is set as 24 hours; and after the constant-temperature reaction is finished, taking out the quartz plate from the bottom of the reaction kettle, and finally drying in a natural environment.
Example four
A method for preparing a two-dimensional tungsten selenide regular layered slice on a quartz chip substrate specifically comprises the following steps:
s1: carrying out early-stage surface cleaning treatment on the quartz wafer: putting quartz plate glass into a beaker, sequentially performing ultrasonic cleaning for 10min by using acetone and absolute ethyl alcohol respectively, taking out the glass plate from the beaker by using clean tweezers after the cleaning is finished, washing the glass plate by using deionized water, and finally drying the glass plate by using a blower.
S2: adding 5.3mmol of sodium borohydride into 60ml of DMF, and fully stirring by using magnetic force; then, after sequentially adding 8.2mmol of selenium powder and 4mmol of sodium tungstate, stirring for 1-2 hours by using magnetic force until the selenium powder and the sodium tungstate are fully dissolved, and uniformly mixing to obtain reaction precursor liquid;
s3: putting the cleaned quartz plate into a 100ml clean reaction kettle lining, and leaning against the inner wall of the bottom of the reaction kettle lining; and slowly pouring the prepared reaction precursor liquid into the inner liner of the reaction kettle, sleeving the stainless steel outer liner, and putting the stainless steel outer liner into an air-blast constant-temperature drying oven for constant-temperature reaction. Wherein the reaction temperature is set as 220 ℃, and the reaction time is set as 48 hours; and after the constant-temperature reaction is finished, taking out the quartz plate from the bottom of the reaction kettle, and finally drying in a natural environment.
From the above, the advantages of the present invention include:
1. stability and surface smoothness of quartz plate, and quartz plate and WSe2Similar lattice structure versus two-dimensional WSe2The growth of regular lamellar sheets plays an important role.
2. Two-dimensional WSe prepared on quartz wafer2The regular laminated sheet can be used for manufacturing a light detector to obtain higher photoelectric property.
4. Two-dimensional WSe prepared on quartz wafer2The regular laminated sheet can be used for manufacturing a field effect transistor to obtain higher photoelectric property. Therefore, the photoelectric device with excellent performance is developed by replacing other materials, and meanwhile, the production cost is greatly reduced.
5. The preparation process is simple, the production cost is low, and products with uniform phases, higher purity and lower thickness can be directly obtained.
Various other changes and modifications to the above-described embodiments and concepts will become apparent to those skilled in the art from the above description, and all such changes and modifications are intended to be included within the scope of the present invention as defined in the appended claims.
Claims (6)
1. A method for preparing two-dimensional tungsten selenide regular layered slice on a quartz chip substrate is characterized in that
In the following steps: the method comprises the following steps:
s1: carrying out early-stage surface cleaning treatment on the quartz wafer;
s2: adding a reducing reagent into a solvent, and then fully stirring by using magnetic force; then, after sequentially adding a selenium source and a tungsten source, stirring for 1-2 hours by using magnetic force until the selenium source and the tungsten source are fully dissolved, and uniformly mixing to obtain a reaction precursor solution;
s3: fully contacting the quartz plate cleaned in the step S1 with the reaction precursor liquid in the step S2, and then reacting at the constant temperature of 200-220 ℃ for 24-48h to prepare a two-dimensional tungsten selenide regular layered sheet on the quartz plate;
in step S2, the selenium source is selenium powder, the tungsten source is sodium tungstate, and the reducing agent is sodium borohydride;
in step S2, the dosage ratio of the tungsten source, the selenium source, and the reducing agent is: (2-4) mmol: (4-8.8) mmol: (2.6-6) mmol.
2. The method for preparing the two-dimensional tungsten selenide regular layered sheet on the quartz substrate according to claim 1, wherein the method comprises the following steps: the step S1 specifically includes: putting the quartz plate into a beaker, sequentially performing ultrasonic cleaning for 10min by using acetone and absolute ethyl alcohol respectively, taking the quartz plate out of the beaker by using clean tweezers after cleaning, washing the quartz plate by using deionized water, and finally drying the quartz plate by using a blower.
3. The method for preparing the two-dimensional tungsten selenide regular layered sheet on the quartz substrate according to claim 1, wherein the method comprises the following steps: the step S3 specifically includes: putting the cleaned quartz plate into a 100ml clean reaction kettle lining, and leaning against the inner wall of the bottom of the reaction kettle lining; and slowly pouring the reaction precursor liquid obtained in the step S2 into the inner liner of the reaction kettle, sleeving the stainless steel outer liner, putting the stainless steel outer liner into an air-blowing constant-temperature drying box for constant-temperature reaction, taking out the quartz plate from the bottom of the reaction kettle after the constant-temperature reaction is finished, and finally drying the quartz plate in a natural environment to obtain the two-dimensional tungsten selenide regular layered sheet.
4. The method for preparing the two-dimensional tungsten selenide regular layered sheet on the quartz substrate according to claim 1, wherein the method comprises the following steps: in step S2, the dosage ratio of the tungsten source, the selenium source, and the reducing agent is: 1 mmol: 2-2.2 mmol: 1.3-1.5 mmol.
5. The two-dimensional tungsten selenide regular layered sheet prepared by the method according to any one of claims 1 to 4, wherein: the prepared two-dimensional tungsten selenide regular layered slice is applied to the manufacture of a light detector.
6. The two-dimensional tungsten selenide regular layered sheet prepared by the method according to any one of claims 1 to 4, wherein: the prepared two-dimensional tungsten selenide regular layered slice is applied to the preparation of a field effect transistor.
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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 |
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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 |
|---|
| Deposition of porous few-layer WSe2 flakes with high density of exposed edge sites;Su et al;《vacuun》;20170816;Introduction部分，文章第2页实验部分，WSe2生长部分，图1 * |
| Graphene-like WSe2 nanosheets for efficient and stable hydrogen evoluation;wang et al20160830;《Journal of Alloys and Compounds》;20160830;文章第2页实验部分，图1，4-5 * |
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