CN110980659A - Tungsten ditelluride grown by using new raw material and preparation method thereof - Google Patents

Tungsten ditelluride grown by using new raw material and preparation method thereof Download PDF

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Publication number
CN110980659A
CN110980659A CN201911378633.5A CN201911378633A CN110980659A CN 110980659 A CN110980659 A CN 110980659A CN 201911378633 A CN201911378633 A CN 201911378633A CN 110980659 A CN110980659 A CN 110980659A
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tungsten
quartz tube
silicon
placing
ditelluride
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陈莹
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Hubei University of Technology
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Hubei University of Technology
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00Selenium; Tellurium; Compounds thereof
    • C01B19/007Tellurides or selenides of metals
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/80Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/04Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM

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Abstract

The invention belongs to the technical field of non-magnetic semi-metal materials, and discloses a method for growing tungsten ditelluride by using a new raw material, which comprises the steps of spin-coating a sodium tungstate aqueous solution on a silicon dioxide sheet, evaporating the solution in the air to obtain a tungsten oxide film, and placing a silicon wafer containing the tungsten oxide film with the front side facing upwards; covering another silicon oxide wafer on the silicon wafer; placing two silicon chips clamped together at the closed end of a large quartz tube; placing tellurium powder at the closed end of a small quartz tube; inserting a small quartz tube into a large quartz tube; and placing the combined quartz tube in a chemical vapor deposition tube furnace, and growing the tungsten ditelluride layered material in a vapor phase. The raw material sodium tungstate or tungsten oxide is low in price, the growth process is short, the repeatability is high, the defects of high energy consumption and long time of the preparation method in the prior art are effectively overcome, and the preparation method has the advantages of simple required equipment and high popularization value.

Description

Tungsten ditelluride grown by using new raw material and preparation method thereof
Technical Field
The invention belongs to the technical field of non-magnetic semi-metal materials, and particularly relates to a method for growing tungsten ditelluride by using a new raw material and a preparation method thereof.
Background
Currently, the closest prior art: tungsten ditelluride (WTE)2) The chalcogenide material is a transition metal chalcogenide compound with a layered structure, tungsten chains in orthogonal unit cells of the chalcogenide material are distributed in one dimension along the a-axis direction of a tellurium layer, and the chalcogenide material is a non-magnetic semi-metal material.
The methods for preparing tungsten ditelluride with different morphologies reported at present mainly comprise the following methods:
the mechanical lift-off method is the most basic method for obtaining tungsten ditelluride with few layers and even a single layer, but the method is difficult to obtain tungsten ditelluride with large area, and the method has limitation because the tungsten ditelluride is easy to degrade in air.
The solid phase reaction method is mainly used for preparing tungsten ditelluride single crystals, requires high temperature and high pressure, and has strict requirement on temperature gradient control during the solid phase reaction.
The chemical vapor transport method and the chemical vapor deposition method have small samples and long reaction time, generally require one to two weeks or even several months to grow tungsten ditelluride, mostly adopt tellurium tetrachloride as raw materials, are easy to mix with tellurium tetrachloride impurities, and subsequently need to be treated in purification and the like.
In summary, the problems of the prior art are as follows: (1) in the prior art for preparing tungsten ditelluride, the cost is high, the growth process is long, the repeatability is poor, and the required equipment in the preparation method is complex and the popularization is limited.
(2) In the prior art, the prepared tungsten ditelluride has poor crystallization property, low yield, difficult transfer and can not be produced in large batch.
The difficulty of solving the technical problems is as follows: two-dimensional transition metal chalcogenides have attracted attention because of their tunable bandgap characteristics (from zero to the visible region). Since graphene has no band gap, the two-dimensional transition metal chalcogenide can replace graphene in many applications, such as field effect transistors, photoelectric devices, integrated logic circuits, biological systems, humidity sensors, electrocatalytic hydrogen production, and the like.
It is well known that large-scale homogeneous semiconductor thin film materials are the cornerstone of future integrated electronic and optoelectronic applications. Although it is easier to prepare large-area high-quality graphene, it is still difficult to prepare large-area two-dimensional metal chalcogenide. The main reason for this is that the precursor is difficult to uniformly disperse on the substrate, so the sample size of the deposited two-dimensional transition metal chalcogenide is small. If the atomic layer deposition and the pulse laser deposition are adopted to prepare the precursor or the noble metal is used as the substrate, the two-dimensional transition metal chalcogenide with larger area, continuity and uniformity can be obtained, but the cost is high, the preparation process is complex, and the crystallinity of the obtained sample is not high. In addition to the above problems, the conventional synthesis technology of tungsten telluride, which is one of two-dimensional transition metal chalcogenide compounds, often uses tellurium tetrachloride as a raw material, and thus the obtained product is easily mixed with impurities of tellurium tetrachloride and has low crystallinity.
The significance of solving the technical problems is as follows: the invention adopts sodium tungstate aqueous solution as tungsten source, can make the tungsten source distribute on the substrate evenly by spin coating method, and has simple operation and low cost. When tungsten oxide is used as a tungsten source, the size of the single tungsten ditelluride film can be regulated and controlled by controlling the dosage of the tungsten oxide. The technology adopts tellurium powder as a tellurium source, and other impurities cannot be introduced.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for growing tungsten ditelluride by using a new raw material and a preparation method thereof.
The invention is realized in such a way that a preparation method for growing tungsten ditelluride by adopting a new raw material comprises the following steps:
step one, spin-coating sodium tungstate aqueous solution on a silicon chip, and heating in air to remove a solvent to obtain WO3Film of which WO is to be contained3The silicon-oxygen sheet of the film is placed with the right side facing upwards;
secondly, covering another silicon oxide sheet on the side cover of the silicon oxide sheet;
placing the two clamped silicon oxygen sheets at the closed end of the large quartz tube;
fourthly, placing the tellurium powder at the closed end of the small quartz tube;
inserting the opening end of the small quartz tube into the large quartz tube;
and sixthly, placing the combined quartz tube in a chemical vapor deposition tube furnace to grow the tungsten ditelluride layered material.
Further, in the second step, the other silicon wafer faces downwards.
Further, in step three, or directly using two silicon sheets to face each other and clamping WO3Powder, placed at the closed end of the large quartz tube.
Further, in the sixth step, the growth time is 30min, the growth temperature is 800 ℃, and the atmosphere is inert gas (high-purity nitrogen or argon).
The invention also aims to provide the tungsten ditelluride prepared by the preparation method for growing the tungsten ditelluride by adopting the new raw material.
In summary, the advantages and positive effects of the invention are: the invention provides a preparation method for growing tungsten ditelluride by adopting a new raw material, the raw material sodium tungstate or tungsten oxide is low in price, the growth process is short, the repeatability is high, the defects of high energy consumption and long time of the preparation method in the prior art are effectively overcome, and the preparation method has simple required equipment and higher popularization value.
As can be seen from the optical micrograph in FIG. 3(a), a tungsten ditelluride thin film having a large area was obtained, and FIG. 3(b) is a Raman spectrum (wavelength: 532nm) of the obtained thin film material, in which 109,117,134,165 and 214cm were observed-1The peaks of (a) correspond to characteristic peaks of two-dimensional tungsten telluride, respectively, indicating that the obtained material is indeed tungsten ditelluride.
From the TEM characterization results of fig. 4, it can be seen that the obtained tungsten ditelluride film has high crystallinity and uniform distribution of tungsten and tellurium elements.
The tungsten ditelluride prepared by the preparation method provided by the invention has good crystallinity, large yield and easy transfer, and provides theoretical reference for mass production of tungsten ditelluride.
Drawings
FIG. 1 is a flow chart of a preparation method for growing tungsten ditelluride by using a new raw material according to an embodiment of the invention.
FIG. 2 is a schematic diagram of the effect of growing tungsten ditelluride by chemical vapor deposition according to an embodiment of the present invention.
FIG. 3 is an optical micrograph and Raman spectrum of tungsten ditelluride (a) provided by an embodiment of the present invention.
Fig. 4 shows (a) TEM photographs, (b) high-resolution transmission electron microscope (HRTEM) photographs of tungsten ditelluride provided by an embodiment of the present invention, in which Selected Area Electron Diffraction (SAED) mode photographs are shown, and (c) and (d) mapping of (a) box portions of tungsten and tellurium elements.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the prior art for preparing tungsten ditelluride, the cost is high, the growth process is long, the repeatability is poor, and the required equipment in the preparation method is complex and the popularization is limited. In the prior art, the prepared tungsten ditelluride has poor crystallization property, low yield, difficult transfer and can not be produced in large batch.
Aiming at the problems in the prior art, the invention provides a method for growing tungsten ditelluride by using a new raw material and a preparation method thereof, and the invention is described in detail by combining the attached drawings.
As shown in fig. 1 and fig. 2, the preparation method for growing tungsten ditelluride by using new raw materials provided by the embodiment of the invention comprises the following steps:
s101, 3.7g of sodium tungstate dihydrate powder is dissolved in 100mL of ultrapure water to obtain a clear and transparent solution for later use. Hydrochloric acid is added dropwise into the sodium tungstate aqueous solution while stirring to adjust the pH value to about 1. The solution was then aged for 24h to give a white flocculent precipitate. The precipitate was heated properly and redissolved in prepared oxalic acid solution (2.8g oxalic acid in 20mL ultrapure water), and finally the solution was diluted to 200mL to obtain clear and transparent tungstic acid colloidal solution.
S102, spin-coating the tungstic acid colloidal solution in the step S101 on a cleaned silicon dioxide Sheet (SiO)2on/Si) and then heating in air (120 ℃ C.) to remove the solvent to give WO3Film of which WO is to be contained3The silicon sheet of the film is placed with the right side up for standby.
S103, another silicon oxygen piece is covered on the upper side of the silicon oxygen piece (the front side faces downwards) in the step S102.
S104, and then placing the two sandwiched silicon wafers at the closed end of the larger quartz tube. Or directly using two silicon sheets with their front faces opposite to each other and sandwiching 0.1g of WO3Powder, placed at the closed end of a larger quartz tube.
S105, placing 0.1g of tellurium powder at the closed end of the smaller quartz tube.
And S106, inserting the opening end of the small quartz tube into the large quartz tube.
S107, finally, placing the combined quartz tube in a 1-inch chemical vapor deposition tube furnace, and growing a few-layer tungsten ditelluride film for 30min at the growth temperature of 800 ℃ in the atmosphere of inert gas (high-purity nitrogen or argon).
The tungsten source provided by the invention is sodium tungstate aqueous solution or tungsten oxide powder, the tellurium source is tellurium powder, the substrate is a silicon-oxygen sheet or a mica sheet, and the placement method and the position are shown in the schematic diagram of figure 2.
The invention is further described below in connection with specific experiments.
As can be seen from the optical micrograph in FIG. 3(a), a tungsten ditelluride thin film having a large area was obtained, and FIG. 3(b) is a Raman spectrum (wavelength: 532nm) of the obtained thin film material, in which 109,117,134,165 and 214cm were observed-1The peaks of (a) correspond to characteristic peaks of two-dimensional tungsten telluride, respectively, indicating that the obtained material is indeed tungsten ditelluride.
From the TEM characterization results of fig. 4, it can be seen that the obtained tungsten ditelluride film has high crystallinity and uniform distribution of tungsten and tellurium elements.
FIG. 3 is an optical micrograph and Raman spectrum of tungsten ditelluride (a) provided by an embodiment of the present invention.
Fig. 4 shows (a) TEM photographs, (b) high-resolution transmission electron microscope (HRTEM) photographs of tungsten ditelluride provided by an embodiment of the present invention, in which Selected Area Electron Diffraction (SAED) mode photographs are shown, and (c) and (d) mapping of (a) box portions of tungsten and tellurium elements.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (5)

1. A preparation method for growing tungsten ditelluride by using a new raw material is characterized by comprising the following steps:
step one, spin-coating a sodium tungstate aqueous solution on a silicon dioxide wafer, evaporating the solution in air to obtain a tungsten oxide film, and placing the silicon wafer containing the tungsten oxide film with the front side facing upwards;
covering another silicon-oxygen piece on the silicon chip;
placing the two silicon chips clamped together at the closed end of the large quartz tube;
fourthly, placing the tellurium powder at the closed end of the small quartz tube;
inserting the small quartz tube into the large quartz tube;
and sixthly, placing the combined quartz tube in a CVD tube, and growing the tungsten ditelluride layered material by a chemical vapor deposition method.
2. The method of claim 1, wherein in step two, the other silicon wafer is facing down.
3. The method of claim 1, wherein in step three, or directly using two silicon wafers with their front faces facing each other, the tungsten oxide powder is sandwiched and placed at the closed end of the large quartz tube.
4. The method according to claim 1, wherein in the sixth step, the growth time is 30min, the growth temperature is 800 ℃, and the atmosphere is inert gas (high purity nitrogen or argon).
5. A tungsten ditelluride produced by the method of claim 1 using a novel starting material for the production of tungsten ditelluride.
CN201911378633.5A 2019-12-27 2019-12-27 Tungsten ditelluride grown by using new raw material and preparation method thereof Pending CN110980659A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111437841A (en) * 2020-05-15 2020-07-24 山西大学 Tungsten telluride-tungsten boride heterojunction electrocatalyst and preparation method and application thereof
CN111874876A (en) * 2020-08-12 2020-11-03 湖北工业大学 Method for growing copper telluride by adopting new raw material, copper telluride and application
CN112938909A (en) * 2021-03-29 2021-06-11 湘潭大学 Preparation method of tungsten ditelluride nanoribbon
CN113501505A (en) * 2021-08-19 2021-10-15 河北大学 Two-dimensional tungsten selenide nano material and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110262660A1 (en) * 2010-04-22 2011-10-27 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Chalcogenide-containing precursors, methods of making, and methods of using the same for thin film deposition
CN104218114A (en) * 2014-08-28 2014-12-17 太原理工大学 Two-dimensional heterojunction solar cell and manufacturing method thereof
CN104894530A (en) * 2015-06-09 2015-09-09 国家纳米科学中心 Two-dimensional transition metal sulfur compound film and preparation method and application thereof
CN109267036A (en) * 2018-11-01 2019-01-25 西北大学 A kind of preparation of two telluride tungsten nanowires material and two telluride tungsten nanowires materials
CN110155959A (en) * 2019-05-31 2019-08-23 西北工业大学 The confinement chemical gas-phase deposition process for preparing of two-dimentional transition metal alloy chalcogenide

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110262660A1 (en) * 2010-04-22 2011-10-27 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Chalcogenide-containing precursors, methods of making, and methods of using the same for thin film deposition
CN104218114A (en) * 2014-08-28 2014-12-17 太原理工大学 Two-dimensional heterojunction solar cell and manufacturing method thereof
CN104894530A (en) * 2015-06-09 2015-09-09 国家纳米科学中心 Two-dimensional transition metal sulfur compound film and preparation method and application thereof
CN109267036A (en) * 2018-11-01 2019-01-25 西北大学 A kind of preparation of two telluride tungsten nanowires material and two telluride tungsten nanowires materials
CN110155959A (en) * 2019-05-31 2019-08-23 西北工业大学 The confinement chemical gas-phase deposition process for preparing of two-dimentional transition metal alloy chalcogenide

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
N.KAISER: "《光学干涉薄膜》", 31 August 2008, 浙江大学出版社 *
王箴: "《化工辞典 第2版》", 30 April 1985 *
黄克靖 等: "《二维过渡金属二硫属化合物的电化学储能应用》", 30 September 2018 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111437841A (en) * 2020-05-15 2020-07-24 山西大学 Tungsten telluride-tungsten boride heterojunction electrocatalyst and preparation method and application thereof
CN111437841B (en) * 2020-05-15 2023-03-24 山西大学 Tungsten telluride-tungsten boride heterojunction electrocatalyst and preparation method and application thereof
CN111874876A (en) * 2020-08-12 2020-11-03 湖北工业大学 Method for growing copper telluride by adopting new raw material, copper telluride and application
CN111874876B (en) * 2020-08-12 2022-02-22 湖北工业大学 Method for growing copper telluride, copper telluride and application
CN112938909A (en) * 2021-03-29 2021-06-11 湘潭大学 Preparation method of tungsten ditelluride nanoribbon
CN113501505A (en) * 2021-08-19 2021-10-15 河北大学 Two-dimensional tungsten selenide nano material and preparation method thereof

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