CN110734092B - Tungsten disulfide two-dimensional material with monoatomic layer, preparation method and application of tungsten disulfide two-dimensional material by reverse physical vapor deposition - Google Patents

Tungsten disulfide two-dimensional material with monoatomic layer, preparation method and application of tungsten disulfide two-dimensional material by reverse physical vapor deposition Download PDF

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CN110734092B
CN110734092B CN201911032943.1A CN201911032943A CN110734092B CN 110734092 B CN110734092 B CN 110734092B CN 201911032943 A CN201911032943 A CN 201911032943A CN 110734092 B CN110734092 B CN 110734092B
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dimensional material
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tungsten disulfide
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李京波
徐志军
李翎
霍能杰
赵艳
魏钟鸣
陈洪宇
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South China Normal University
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    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G41/00—Compounds of tungsten
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    • 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
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    • 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
    • C23C14/0623—Sulfides, selenides or tellurides
    • 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
    • C23C14/54—Controlling or regulating the coating process
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer

Abstract

The invention belongs to the technical field of piezoelectrics and discloses a WS2Two-dimensional material and preparation method and application thereof. The WS2The two-dimensional material is to be loaded with WS separately2Powder and cleaned SiO2The center and the edge of the heating zone where the/Si substrate is placed; introducing inert gas in the direction from the substrate to WS2Ventilating the powder in the direction of 55-60 ml/min to exhaust air, and changing the flow direction of inert gas when the temperature reaches 1080-1090 ℃; when the temperature is 1000-1200 ℃, the flow rate is 30-100 ml/min; cooling to 900-1000 deg.C at a flow rate of 20-80 ml/min to 800-900 deg.C at a flow rate of 5-50 ml/min, cooling to room temperature at SiO2Is prepared on the surface of the layer. WS of the invention2The prepared piezoelectric device has excellent piezoelectric performance and stable dynamic piezoelectric signals, and the piezoelectric output current reaches 100-800 pA.

Description

Tungsten disulfide two-dimensional material with monoatomic layer, preparation method and application of tungsten disulfide two-dimensional material by reverse physical vapor deposition
Technical Field
The invention belongs to the technical field of growth and piezoelectricity of two-dimensional materials, and particularly relates to tungsten disulfide (WS) with a single atomic layer2) Two-dimensional material and preparation method and application of reverse Physical Vapor Deposition (PVD) thereof.
Background
Due to the unique electrical and optical properties of atom thick two-dimensional transition metal chalcogenides (TMDCs), which have a certain band gap, strong photo-physical interactions and strong mechanical flexibility, which can complement the properties of graphene, there is a strong interest. Unlike multilayer structures, single-layer semiconductor TMDCs have a relatively large direct band gap, which provides possibilities for their application in the fields of transistors, integrated circuits, photodetectors, electroluminescent devices, electronics, and spintronics.
As an important member of two-dimensional TMDCs, WS2Has excellent physical performance and wide application range. And single-layer WS2Also has good softness, can bear larger external stress, and has single-layer WS2Also makes it potentially piezoelectric. The prior physical vapor deposition technology is easily influenced by the outside because the flow velocity of the introduced air flow is low during heat preservation, and the consequences or specific adverse effects are generated. Therefore, how to stably obtain a single-layered WS2Is a key technical problem.
Disclosure of Invention
To overcome the above-mentioned disadvantages and drawbacks of the prior art, the present invention provides a WS layer with a single atomic layer2Two-dimensional material of WS2The grain size of the two-dimensional material is more than 80um, WS2High crystallinity, and good optical, electrical and piezoelectric properties.
Another object of the present invention is to provide WS as a monoatomic layer2The preparation method of two-dimensional material adopts reverse physical vapor deposition method, and controls WS by changing flow direction of inert gas and regulating flow rate2And (4) growing the two-dimensional material. In the heat preservation process, the introduced air flow is large, so that the heat preservation device is not easily influenced by the outside. More stable to WS than previous physical vapor deposition techniques2Plays a key role.
It is another object of the present invention to provide WS as a monoatomic layer2The application of two-dimensional materials in the field of piezoelectrics.
The purpose of the invention is realized by the following technical scheme:
WS of monoatomic layer2Two-dimensional material, said WS2The two-dimensional material is prepared by firstly preparing SiO2the/Si substrate is firstly cleaned by ultrasonic wave and then is respectively loaded with WS2Powder and SiO2The center and the edge of a heating zone where a quartz boat of the/Si substrate is placed; opening the gas cylinder valve, introducing inert gas, wherein the gas flow direction is from the substrate to WS2Exhausting air in the quartz tube in the direction of the powder, then starting to heat up, changing the introduction direction of the inert gas when the temperature is raised to 1000-1200 ℃, and leading the gas flow direction to be from WS2Powder is added to a substrate, the flow rate of air flow is adjusted to be 30-100 ml/min, and heat preservation is carried out for 3-10 minutes within the temperature range; then, the temperature is reduced to 900-1000 ℃, the flow rate of the air flow is adjusted to 20-80 ml/min, when the temperature is reduced to 800-900 ℃, the flow rate of the air flow is adjusted to 5-50 ml/min, the substrate is taken out after the temperature is reduced to room temperature, and the substrate is taken out after SiO2Preparation of a monoatomic layer of WS on a layer surface2A two-dimensional material.
Preferably, said WS2The amount of the powder is 20-100 mg.
Preferably, the inert gas is nitrogen or argon.
Preferably, the gas flow rate during growth is 30-100 ml/min.
Preferably, the heat preservation time is 3-10 min.
Preferably, WS of said monoatomic layer2The grain size of the two-dimensional material is 50-200 μm.
WS of the monoatomic layer2The preparation method of the reverse physical vapor deposition of the two-dimensional material comprises the following specific steps:
s1, mixing SiO2Soaking the/Si substrate in acetone, deionized water and isopropanol, ultrasonically treating, blow-drying with nitrogen, cleaning, and loading WS2Powder and SiO2The center and the edge of a heating zone where a quartz boat of the/Si substrate is placed;
s2, opening a gas cylinder gas valve, introducing inert gas, wherein the direction of the gas flow is from the substrate to WS2Exhausting air in the quartz tube in the direction of the powder, and then starting to heat; when the temperature is raised to 1000-1200 ℃, the inertia is changedThe direction of gas introduction being from WS2Powder to a substrate;
s3, opening an air valve of the air bottle when the temperature is heated to 1000-1200 ℃, adjusting the flow rate of air flow to be 30-100 ml/min, and preserving the heat for 3-10 minutes in the temperature range; then, the temperature is reduced to 900-1000 ℃, the flow rate of the air flow is adjusted to 20-80 ml/min, when the temperature is reduced to 800-900 ℃, the flow rate of the air flow is adjusted to 5-50 ml/min, the substrate is taken out after the temperature is reduced to room temperature, and the substrate is taken out after SiO2Preparation of a monoatomic layer of WS on a layer surface2A two-dimensional material.
Preferably, the soaking time in the step S1 is 5-10 min; the time of the ultrasonic treatment is 4-8 min.
The WS2The application of two-dimensional materials in the field of piezoelectricity.
Preferably, WS is formed from said monoatomic layer2The piezoelectric output current of the piezoelectric device made of the two-dimensional material is 100-800 pA.
The invention first adjusts the direction of the gas flow from the substrate to WS2Powder, then starting to warm up to block WS2The growth is started without reaching the growth temperature; when the temperature is raised to 1000-1200 ℃, the introduction direction of the inert gas is changed to lead the gas flow direction to be from WS2Powder is added to the substrate, the flow rate of air flow is adjusted to be 30-100 ml/min, and heat preservation is carried out within the temperature range to ensure WS2Starting growth on the substrate; then, the temperature is reduced to 900-1000 ℃, and the flow rate of the air flow is adjusted to 20-80 ml/min to reduce WS2The growth rate of (2); when the temperature is reduced to 800-900 ℃, the gas flow rate is adjusted to 5-50 ml/min to further reduce WS2Growth rate of WS to further increase2The grain size of the crystal is not too large; cooling to room temperature, taking out the substrate, and placing the substrate on SiO2Preparation of a monoatomic layer of WS on a layer surface2A two-dimensional material.
Compared with the prior art, the invention has the following beneficial effects:
1. WS of a monoatomic layer of the invention2The grain size of the two-dimensional material is 50-200 μm, WS2High crystallinity, and good optical, electrical and piezoelectric properties. This is due to the use ofReverse physical vapor deposition by changing the flow direction of inert gas and regulating the flow rate2No deposition of WS on the silicon dioxide substrate until the crystal reaches the growth temperature2Crystal nuclei capable of reducing WS2Multiple layers are deposited. And the size of the material growth is made larger by adjusting the flow rate, the produced WS2The grain size is 50-200 μm, the crystallinity is high, and the growth process of the material is also realized in the cooling process.
2. The luminescence peak of the invention in PL test is obviously stronger than WS that is mechanically stripped2The WS is more stable than the conventional physical vapor deposition technology, and the monoatomic layer grown by the method2Having good piezoelectric properties, formerly WS2The piezoelectric test of (2) has no report, and the test finds that the dynamic piezoelectric reaches 100-800 pA.
3. In the invention, the flow velocity of the air flow is gradually reduced in the cooling process, if the flow velocity is changed too much at one time, the growth of the material is seriously unfavorable, and the grown material has smaller size and poorer quality. Therefore, the flow rate is gradually reduced in the cooling process, and the WS in a monoatomic layer is favorably realized at low flow rate2And (4) growing the two-dimensional material.
4. The method adopts a reverse physical vapor deposition method, and controls WS of the monoatomic layer by changing the flow direction and regulating and controlling the flow rate of inert gas2And (4) growing the two-dimensional material. In the heat preservation process, the introduced air flow is large, so that the heat preservation device is not easily influenced by the outside. Compared with the prior physical vapor deposition technology, the method is more stable to WS of a monoatomic layer2Plays a key role.
Drawings
FIG. 1 shows WS as a monoatomic layer formed by reversed physical vapor deposition in example 12An optical microscopy image of a two-dimensional material;
FIG. 2 shows WS in example 42Dynamic piezoelectric diagram of flexible electronic devices.
Detailed Description
The following examples are presented to further illustrate the present invention and should not be construed as limiting the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Example 1
1. Preparation: mixing SiO2Firstly, ultrasonically cleaning a Si substrate by using acetone, deionized water and isopropanol; loading 50mg of WS in boat in single temperature zone tube furnace2Placing the powder in the middle of the heating zone, and adding SiO2The Si substrate is placed at the mouth of the tube furnace, and the gas flow direction is from the substrate to WS2Powder, then starting to warm up to block WS2The growth is started without reaching the growth temperature; when the temperature is raised to 1100 ℃, the direction of the inert gas is changed to lead the gas flow direction to be from WS2Powder is applied to the substrate, then the gas flow rate is adjusted to 100ml/min, and the temperature is kept in this temperature range for 7 minutes to make WS2Starting growth on the substrate; then the temperature is reduced to 1000 ℃, and the flow rate of the air flow is adjusted to 80ml/min to reduce WS2The growth rate of (2); when the temperature is reduced to 900 ℃, the gas flow rate is adjusted to 5ml/min to further reduce WS2Growth rate of WS to further increase2The size of the steel plate is not too long and thick; cooling to room temperature, taking out the substrate, and placing the substrate on SiO2SiO on/Si substrate2Preparation of a monoatomic layer of WS on a layer surface2A two-dimensional material.
2. And (3) performance testing: FIG. 1 shows WS in example 1, in which a monoatomic layer was formed by reverse PVD2An optical microscopy image of a two-dimensional material; from FIG. 1, it can be seen that WS was obtained by growth2The crystallinity is high and the size reaches 80 μm.
Example 2
1. Preparation: mixing SiO2Firstly, ultrasonically cleaning a Si substrate by using acetone, deionized water and isopropanol; loading 20mg of WS in boat in single temperature zone tube furnace2Placing the powder in the middle of the heating zone, and adding 0.5cm2SiO of (2)2The Si substrate is placed at the mouth of the tube furnace, and the gas flow direction is from the substrate to WS2Powder, then starting to warm up to block WS2Not reached to growthThe growth starts at temperature; when the temperature is raised to 1000 ℃, the direction of the inert gas is changed to lead the gas flow direction to be from WS2Powder is applied to the substrate, then the gas flow rate is adjusted to 50ml/min, and the temperature is kept in this temperature range for 8 minutes to make WS2Starting growth on the substrate; then the temperature is reduced to 900 ℃, and the flow rate of the air flow is adjusted to 50ml/min to reduce WS2The growth rate of (2); when the temperature is reduced to 800 ℃, the gas flow rate is adjusted to be 50ml/min so as to further reduce WS2Growth rate of WS to further increase2The size of the steel plate is not too long and thick; cooling to room temperature, taking out the substrate, and placing the substrate on SiO2SiO on/Si substrate2Preparation of a monoatomic layer of WS on a layer surface2A two-dimensional material.
2. And (3) performance testing: growth of the resulting monoatomic layer of WS2The crystallinity is high and the size reaches 50 μm.
Example 3
1. Preparation: mixing SiO2Firstly, ultrasonically cleaning a Si substrate by using acetone, deionized water and isopropanol; loading 60mg of WS in boat in single temperature zone tube furnace2Placing the powder in the middle of the heating zone, and adding 0.5cm2SiO of (2)2The Si substrate is placed at the mouth of the tube furnace, and the gas flow direction is from the substrate to WS2Powder, then starting to warm up to block WS2The growth is started without reaching the growth temperature; when the temperature is raised to 1200 ℃, the direction of the inert gas is changed to lead the gas flow direction to be from WS2Powder is applied to the substrate, then the gas flow rate is adjusted to 30ml/min, and the temperature is kept in the temperature range for 10 minutes to ensure that WS is2Starting growth on the substrate; then, the temperature was initially decreased to 950 ℃ and the gas flow rate was adjusted to 50ml/min to decrease WS2The growth rate of (2); when the temperature is reduced to 800 ℃, the gas flow rate is adjusted to be 20ml/min so as to further reduce WS2Growth rate of WS to further increase2The size of the steel plate is not too long and thick; cooling to room temperature, taking out the substrate, and placing the substrate on SiO2SiO on/Si substrate2Preparation of a monoatomic layer of WS on a layer surface2A two-dimensional material.
2. And (3) performance testing: growing the resulting monoatomicWS of a layer2The crystallinity is high and the size reaches 200 mu m.
Example 4
Will grow on SiO2WS (A) of2PMMA was spin-coated on a spin coater at 7000 rpm for 60 s. Then heated in a hot plate for 30 minutes at 150 ℃. After heating, soaking KOH solution for 20 minutes, waiting for the PMMA film to be separated from the Si substrate, soaking the separated PMMA film in deionized water for 45 minutes, finally placing the PMMA film on a flexible substrate, heating the flexible substrate in a heating plate for 30 minutes at 120 ℃, finally soaking acetone for 20 minutes, drying by using a nitrogen gun, and preparing the flexible electronic device, namely WS, the flexible electronic device2The piezoelectric device of (1).
FIG. 2 depicts WS using a single atomic layer of example 12Flexible electronic devices made of two-dimensional materials. From FIG. 2, WS2Large dynamic piezoelectric current of, indicates WS2The piezoelectric signal is good, and the piezoelectric performance is stable. Compared with WS prepared by conventional physical vapor deposition method2WS of the present invention2The number of the layers is single layer, the crystallinity is high, and the single layer WS can be prepared more stably2. By WS of the present invention2The flexible electronic device made of two-dimensional material is found to have excellent piezoelectric performance for the first time, and obtains higher and stable dynamic piezoelectric signal, WS2The piezoelectric output current of the piezoelectric device of (1) reached 400 pA.
Example 5
Will grow on SiO2WS (A) of2PMMA was spin-coated on a spin coater at 8000 rpm for 60 s. Then heated in a hot plate for 25 minutes at 140 ℃. After heating, soaking KOH solution for 20 minutes, waiting for the PMMA film to be separated from the Si substrate, soaking the separated PMMA film in deionized water for 45 minutes, finally placing the PMMA film on a flexible substrate, heating the flexible substrate in a heating plate for 30 minutes at 120 ℃, finally soaking acetone for 20 minutes, drying by using a nitrogen gun, and preparing the flexible electronic device, namely WS, the flexible electronic device2The piezoelectric device of (1). Obtaining a high and stable dynamic piezoelectric signal, WS2The piezoelectric output current of the piezoelectric device of (1) reached 450 pA.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations and simplifications are intended to be included in the scope of the present invention.

Claims (4)

1. A preparation method of reverse physical vapor deposition of a tungsten disulfide two-dimensional material with a monoatomic layer is characterized by comprising the following specific steps:
s1, mixing SiO2Soaking the/Si substrate in acetone, deionized water and isopropanol, ultrasonically treating, blow-drying with nitrogen, cleaning, and loading WS2Powder and SiO2The center and the edge of the heating zone where the/Si substrate is placed;
s2, opening the gas cylinder valve, and introducing argon or nitrogen, wherein the gas flow direction is from the substrate to WS2Exhausting air in the quartz tube in the direction of the powder, and then starting to heat; when the temperature is raised to 1000-1200 ℃, the introduction direction of argon or nitrogen is changed to lead the gas flow direction to be from WS2Powder to a substrate;
s3, when the temperature reaches 1000-1200 ℃, opening the gas valve of the gas cylinder, adjusting the flow rate of the gas flow to be 30-100 mL/min, and preserving the heat for 3-10 minutes in the temperature range; then, the temperature is reduced to 900-1000 ℃, the flow rate of the air flow is adjusted to 20-80 mL/min, when the temperature is reduced to 800-900 ℃, the flow rate of the air flow is adjusted to 5-50 mL/min, the substrate is taken out after the temperature is reduced to the room temperature, and the substrate is taken out after SiO2Preparation of a monoatomic layer of WS on a layer surface2A two-dimensional material.
2. The method for preparing the monolayer tungsten disulfide two-dimensional material according to claim 1, wherein the soaking time in step S1 is 5-10 min; the time of the ultrasonic treatment is 4-8 min.
3. The method according to claim 1, wherein the WS 1 is prepared by reverse pvd of a monoatomic layer of tungsten disulfide two-dimensional material2The amount of the powder is 20-100 mg.
4. The method according to claim 1, wherein the WS 3 is prepared by reverse pvd of a monoatomic layer of tungsten disulfide two-dimensional material2The grain size of the two-dimensional material is 50-200 mu m.
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