CN109267036B - Preparation of tungsten ditelluride nanowire material and tungsten ditelluride nanowire material - Google Patents
Preparation of tungsten ditelluride nanowire material and tungsten ditelluride nanowire material Download PDFInfo
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- CN109267036B CN109267036B CN201811292951.5A CN201811292951A CN109267036B CN 109267036 B CN109267036 B CN 109267036B CN 201811292951 A CN201811292951 A CN 201811292951A CN 109267036 B CN109267036 B CN 109267036B
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Abstract
The invention discloses a preparation method of a tungsten ditelluride nanowire material and the tungsten ditelluride nanowire material, wherein a silicon dioxide/silicon wafer is used as a substrate, tungsten powder and tellurium powder are used as raw materials, and the growth of a tungsten ditelluride nanowire is carried out on the silicon dioxide surface of the substrate by adopting a chemical vapor deposition method; the growth container of the tungsten ditelluride nanowire is a quartz tube, and mixed gas of argon and hydrogen is introduced into the quartz tube; a quartz test tube is arranged in the quartz tube, the sealing end of the quartz test tube is opposite to the flowing direction of the mixed gas, and the quartz test tube is used for placing a substrate for chemical vapor deposition; the flow rate of argon is 100 sccm; the flow rate of the hydrogen is 10-40 sccm; the reaction temperature of the chemical vapor deposition is 600-800 ℃. The experimental preparation method has the advantages of simple process and low cost, and the prepared tungsten ditelluride nanowires have high quality. The tungsten ditelluride has physical properties such as super-large magnetoresistance effect, superconductivity and the like, and has higher research significance and application value.
Description
Technical Field
The invention belongs to the field of nano materials, and relates to a preparation method of a tungsten ditelluride nanowire material and the tungsten ditelluride nanowire material.
Background
Tungsten ditelluride is a transition metal chalcogenide compound with a layered structure, a tungsten atomic layer is arranged between an upper tellurium atomic layer and a lower tellurium atomic layer in the layer, tungsten atoms are in covalent bond connection with tellurium atoms, and one tungsten atom is surrounded by 6 tellurium atoms and two tungsten atoms. The layers are coupled by van der waals interactions, each stacked along the c-axis. Tungsten ditelluride has a very high unsaturated magnetoresistance, and thus has received much attention, and the physical mechanism of its giant magnetoresistance effect has been widely studied. Tungsten ditelluride is a unique layered material belonging to transition metal chalcogenide, and the preparation of tungsten ditelluride is divided into physical and chemical methods, such as: mechanical stripping, chemical vapor transport, and the like. The chemical vapor deposition method has great significance for the application of the tungsten ditelluride in the aspect of giant magnetoresistance effect, and is the most promising preparation method of the tungsten ditelluride which is accepted at present. At present, researchers have engaged in the preparation of two-dimensional tungsten ditelluride materials and achieved certain results, but the one-dimensional tungsten ditelluride nanowires are not synthesized.
Disclosure of Invention
The invention provides a preparation method of a tungsten ditelluride nanowire material and the tungsten ditelluride nanowire material.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
a preparation method of a tungsten ditelluride nanowire material comprises the following steps of taking silicon dioxide/silicon wafers as substrates, taking tungsten powder and tellurium powder as raw materials, and growing tungsten ditelluride nanowires on the silicon dioxide surfaces of the substrates by adopting a chemical vapor deposition method;
the growth container of the tungsten ditelluride nanowire is a quartz tube, and mixed gas of argon and hydrogen is introduced into the quartz tube;
a quartz test tube is arranged in the quartz tube, the sealing end of the quartz test tube is opposite to the flowing direction of the mixed gas, and the quartz test tube is used for placing a substrate for chemical vapor deposition;
the flow rate of argon is 100 sccm; the flow rate of the hydrogen is 10-40 sccm; the reaction temperature of the chemical vapor deposition is 600-800 ℃.
Optionally, the silicon dioxide/silicon wafer substrates are provided with two silicon dioxide/silicon wafer substrates, the silicon dioxide surfaces of the two silicon dioxide/silicon wafer substrates are oppositely stacked, and tungsten powder and tellurium powder are sandwiched between the stacked layers.
Optionally, the molar ratio of the tungsten powder to the tellurium powder is 1: 1-20, and the total mass of the tungsten powder and the tellurium powder is 1 mg-4 mg.
Optionally, NaCl is doped between the tungsten powder and the tellurium powder, wherein the doping amount of the NaCl is 0.1-0.5 mg.
Optionally, the heating rate of the hydrogen is 20-50 ℃/min.
Optionally, the mixing molar ratio of the tungsten powder to the tellurium powder is 1: 1-20.
Optionally, the growth time of the tungsten ditelluride nanowire is 4-30 min.
Optionally, the method specifically includes:
(1) cutting the silicon dioxide/silicon substrate into a sheet shape of 1cm by 3cm, and uniformly mixing tungsten powder and tellurium powder in proportion to obtain mixed powder;
(2) placing the mixed powder on the silicon dioxide surface of a silicon dioxide/silicon substrate, and adding sodium chloride; the silicon dioxide surface of the other silicon dioxide/silicon substrate is reversely buckled on the silicon dioxide/silicon substrate with the mixed powder;
(3) and moving the two silicon dioxide/silicon substrates into a quartz test tube, placing the quartz test tube into the quartz tube, enabling the sealing end of the quartz test tube to be opposite to the flowing direction of the mixed gas, and heating the quartz test tube in a tubular atmosphere furnace to perform chemical vapor deposition of the tungsten ditelluride nanowires.
The tungsten ditelluride nanowire material comprises a silicon dioxide/silicon substrate, and the growth of the tungsten ditelluride nanowire is carried out on the silicon dioxide/silicon substrate by adopting the method provided by the invention.
The invention successfully prepares the tungsten ditelluride nano-wires with uniform size, and the preparation process is simple.
Drawings
FIG. 1 is a schematic diagram of experimental preparation of examples and comparative examples of the present invention;
FIG. 2 is an optical micrograph of example 1 of the present invention;
FIG. 3 is a Raman spectrum of example 1 of the present invention;
FIG. 4 is an optical micrograph of example 2 of the present invention;
FIG. 5 is a Raman spectrum of example 2 of the present invention;
FIG. 6 is an optical micrograph of comparative example 1 according to the present invention;
the invention is described in detail below with reference to the drawings and the detailed description.
Detailed Description
The tungsten ditelluride nanowire material prepared by the invention directly grows on a silicon dioxide/silicon substrate by adopting a chemical vapor deposition method. The tungsten ditelluride nanowire material obtained by the factors of the proportion of the reaction source, the reaction temperature, the reaction time and the like has simple process and low cost.
In order to make the objects and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings and examples, and the advantages of the present invention are shown by comparative analysis. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The first embodiment is as follows:
this example provides a method for preparing tungsten ditelluride nanowires on a silicon dioxide/silicon substrate, which comprises the following steps:
the method comprises the following steps: cutting the silicon dioxide/silicon substrate into sheets of 1cm by 3cm and blowing the sheets by using an air gun;
step two: grinding tungsten powder and tellurium powder according to the molar ratio of 1:1, uniformly mixing, placing 1mg of mixed powder on a silicon dioxide/silicon substrate, and adding 0.1mg of sodium chloride; another silicon dioxide/silicon substrate, SiO2Face down, and flip-chip on the silicon chip;
step three: two silicon dioxide/silicon substrates are moved and placed in a single-end sealed quartz tube with the inner diameter of 1.2cm, the single-end sealed quartz tube is placed at the heating center of the tubular atmosphere furnace, and the opening of the single-end sealed quartz tube faces to one side of the exhaust port, as shown in fig. 1 a.
Step four: argon gas of 100sccm is introduced for 30min to thoroughly remove the residual oxygen in the tube. Then, continuously introducing 40sccm hydrogen, heating the tubular atmosphere furnace to 750 ℃, wherein the heating rate is 37.5 ℃/min, and keeping the temperature for 7 min. And then the heater is turned off, and the temperature is naturally cooled to room temperature, wherein the obtained tungsten ditelluride nano-wire is shown in figure 2, and the Raman spectrum is shown in figure 3.
The optical photograph of fig. 2 illustrates that the synthesized material is a nanowire structure, and fig. 3 illustrates that the synthesized material has a raman characteristic peak of tungsten ditelluride, indicating that the synthesized material is tungsten ditelluride.
Example two:
this example provides a method for preparing tungsten ditelluride nanowires on a silicon dioxide/silicon substrate, which comprises the following steps:
the method comprises the following steps: cutting the silicon dioxide/silicon substrate into sheets of 1cm by 3cm and blowing the sheets by using an air gun;
step two: grinding tungsten powder and tellurium powder according to the molar ratio of 1:16, uniformly mixing, placing 2mg of mixed powder on a silicon dioxide/silicon substrate, and adding 0.2mg of sodium chloride; another silicon dioxide/silicon substrate, SiO2Face down, and flip-chip on the silicon chip;
step three: two silicon dioxide/silicon substrates are moved and placed in a single-end sealed quartz tube with the inner diameter of 1.2cm, the single-end sealed quartz tube is placed at the heating center of the tubular atmosphere furnace, and the opening of the single-end sealed quartz tube faces to one side of the exhaust port, as shown in fig. 1 a.
Step four: argon gas of 100sccm is introduced for 30min to thoroughly remove the residual oxygen in the tube. Then, continuously introducing 30sccm hydrogen, heating the tubular atmosphere furnace to 550 ℃, wherein the heating rate is 45.8 ℃/min, and keeping the temperature for 30 min. And then the heater is turned off, and the temperature is naturally cooled to room temperature, wherein the obtained tungsten ditelluride nano-wires are shown in figure 4, and the Raman spectrum is shown in figure 5.
The optical photograph of fig. 4 illustrates that the synthesized material is a nanowire structure, and fig. 5 illustrates that the synthesized material has a raman characteristic peak of tungsten ditelluride, indicating that the synthesized material is tungsten ditelluride.
Comparative example:
this comparative example shows a method of preparing a material without using a single-ended sealed quartz tube, comprising the steps of,
the method comprises the following steps: same as example 1;
step two: same as example 1;
step three: two silica/silicon substrates were placed directly in the position of the heating center of the tube-type atmosphere furnace as shown in FIG. 1 b.
Step four: the results obtained at this time are shown in FIG. 6, as in example 1.
The comparison shows that the single-end sealed quartz tube is not used as the cavity, and under the condition that other conditions are not changed, the material synthesized on the substrate is microparticles and a nanowire structure is not formed.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (4)
1. A preparation method of a tungsten ditelluride nanowire material is characterized in that a silicon dioxide/silicon wafer is used as a substrate, tungsten powder and tellurium powder are used as raw materials, and a chemical vapor deposition method is adopted for growing a tungsten ditelluride nanowire on the silicon dioxide surface of the substrate;
the growth container of the tungsten ditelluride nanowire is a quartz tube, and mixed gas of argon and hydrogen is introduced into the quartz tube;
a quartz test tube is arranged in the quartz tube, the sealing end of the quartz test tube is opposite to the flowing direction of the mixed gas, and the quartz test tube is used for placing a substrate for chemical vapor deposition;
the flow rate of argon is 100 sccm; the flow rate of the hydrogen is 10-40 sccm; the reaction temperature of the chemical vapor deposition is 600-800 ℃;
the molar ratio of the tungsten powder to the tellurium powder is 1: 1-20, and the total mass of the tungsten powder and the tellurium powder is 1 mg-4 mg;
doping NaCl between the tungsten powder and the tellurium powder, wherein the doping amount of the NaCl is 0.1-0.5 mg;
the temperature rise rate of the hydrogen is 20-50 ℃/min;
the growth time of the tungsten ditelluride nanowire is 4-30 min.
2. The method of claim 1, wherein the two silicon dioxide/silicon wafer substrates are stacked with their silicon dioxide surfaces facing each other, and tungsten powder and tellurium powder are interposed between the stacked layers.
3. The method for preparing a tungsten ditelluride nanowire material as claimed in claim 1 or 2, which specifically comprises:
(1) cutting the silicon dioxide/silicon substrate into a sheet shape of 1cm by 3cm, and uniformly mixing tungsten powder and tellurium powder in proportion to obtain mixed powder;
(2) placing the mixed powder on the silicon dioxide surface of a silicon dioxide/silicon substrate, and adding sodium chloride; the silicon dioxide surface of the other silicon dioxide/silicon substrate is reversely buckled on the silicon dioxide/silicon substrate with the mixed powder;
(3) and moving the two silicon dioxide/silicon substrates into a quartz test tube, placing the quartz test tube into the quartz tube, enabling the sealing end of the quartz test tube to be opposite to the flowing direction of the mixed gas, and heating the quartz test tube in a tubular atmosphere furnace to perform chemical vapor deposition of the tungsten ditelluride nanowires.
4. A tungsten ditelluride nanowire material comprising a silica/silicon substrate on which tungsten ditelluride nanowires are grown using a method as claimed in any one of claims 1 to 3.
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| CN110510585B (en) * | 2019-09-30 | 2022-09-06 | 福州大学 | Preparation method of large-area thin-layer two-dimensional telluroene |
| CN110980659A (en) * | 2019-12-27 | 2020-04-10 | 湖北工业大学 | Tungsten ditelluride grown by using new raw material and preparation method thereof |
| CN111613522A (en) * | 2020-05-08 | 2020-09-01 | 西北工业大学 | Method for integrating transition metal chalcogenide and micro-nano photonic device |
| CN111874876B (en) * | 2020-08-12 | 2022-02-22 | 湖北工业大学 | Method for growing copper telluride, copper telluride and application |
| CN112938909B (en) * | 2021-03-29 | 2022-09-09 | 湘潭大学 | Preparation method of tungsten ditelluride nanoribbon |
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| CN105301909B (en) * | 2015-09-22 | 2019-07-19 | 北京大学 | A method of preparing the micro belt or nanobelt of two-dimension nano materials |
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