CN114314639A - Preparation method of two-dimensional material layered zinc oxide nanosheet - Google Patents

Preparation method of two-dimensional material layered zinc oxide nanosheet Download PDF

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CN114314639A
CN114314639A CN202111643195.8A CN202111643195A CN114314639A CN 114314639 A CN114314639 A CN 114314639A CN 202111643195 A CN202111643195 A CN 202111643195A CN 114314639 A CN114314639 A CN 114314639A
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zinc oxide
dimensional material
ultrasonic oscillation
solution
container
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彭金峰
王鹏
郑学军
苏亮
周春德
刘鸿凯
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Xiangtan University
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Xiangtan University
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Abstract

The invention discloses a preparation method of two-dimensional material layered zinc oxide, which comprises the steps of packaging zinc oxide powder, graphite powder and tin dioxide powder in a quartz tube, controlling the temperature and time by a program in a chemical vapor deposition tube furnace, introducing oxygen simultaneously to prepare a zinc oxide micron rod, putting the zinc oxide micron rod into an acetone or absolute ethyl alcohol solution, carrying out three-time ultrasonic oscillation on the zinc oxide micron rod by an ultrasonic instrument, removing two thirds of the volume of the solution after the first and second ultrasonic oscillations, and adding acetone or absolute ethyl alcohol solution with the same volume as the removed volume. The power of the three-time ultrasonic oscillation is 60KHz, the time is 30 minutes, the two-dimensional material layered zinc oxide nanosheet can be obtained after the three-time ultrasonic oscillation is finished, the two-dimensional material layered zinc oxide nanosheet is well applied to the aspects of electro-catalysis, photocatalysis, photovoltaics and optics, and the two-dimensional material layered zinc oxide nanosheet becomes an important research field which is not negligible in optics and photocatalysis.

Description

Preparation method of two-dimensional material layered zinc oxide nanosheet
Technical Field
The invention belongs to the field of preparation of novel two-dimensional materials, and particularly relates to a method for obtaining a two-dimensional material layered zinc oxide nano-sheet after a zinc oxide micro-rod is subjected to ultrasonic oscillation.
Background
The two-dimensional material has the advantages of ultrahigh carrier mobility, linear dispersion relation of the Dirac cone and the like, has very wide application prospect in the fields of optics, electrics, catalysis and the like, and is favored by extensive researchers. The zinc oxide (ZnO) material has unique optical and electrical properties, has a band gap width of 3.37eV and high exciton binding energy of 60meV at room temperature, and is a II-VI semiconductor material with a wide direct band gap and good performance. And the ZnO nano material can also be used as a gas sensor, fluorescent powder, an energy storage device, a rheostat and the like, and has attracted great interest of researchers. The material has the characteristics of material and shape, has wide application prospect in the aspects of photoelectronic devices and spin memory devices, and has great theoretical research value and practical application value for the development and application of the material through the research on the material and the research on the doping of other ions into the material to achieve the optimization or endow new optical and magnetic properties.
The current methods for preparing two-dimensional materials mainly include ultrasonic stripping, mechanical stripping, physical deposition (PVD), and Chemical Vapor Deposition (CVD). Although the mechanical stripping method is simple to operate, the obtained sample is irregular in shape and multi-layer, a single-layer sample is extremely difficult to obtain, and the stripping method is also influenced by the adhesive tape; the size of the growth in PVD methods is generally small and the thickness of the samples is also inconsistent. In contrast, chemical vapor deposition methods and ultrasonic lift-off methods are the best methods for producing two-dimensional materials. Therefore, the invention adopts a chemical vapor deposition method and ultrasonic stripping to prepare the zinc oxide nano-sheet.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of a two-dimensional material layered zinc oxide nano-sheet.
In order to realize the above-mentioned mode, the present invention is realized by providing one of the following technical solutions.
The invention provides a preparation method of a two-dimensional material layered zinc oxide nano-sheet, which comprises the following steps:
(1) preparing zinc oxide micron rods: mixing zinc oxide powder, graphite powder and tin dioxide powder according to the mass ratio of 1:1:0.025, putting the mixture into a mortar, grinding the mixture to be fine and stirring the mixture uniformly, putting the mixture into an alumina burning boat, putting the alumina burning boat into the middle position of a quartz tube, and conveying the quartz tube and the alumina burning boat to a heating part of a furnace; heating the furnace to 1000 ℃, preserving the heat for 30 minutes, and then cooling to room temperature, wherein substances in the alumina burning boat are flocculent, namely the zinc oxide micron rods;
(2) preparing a solution in a container;
(3) ultrasonic oscillation treatment: taking a single zinc oxide micron rod from the alumina burning boat, putting the single zinc oxide micron rod into the container, and carrying out first ultrasonic oscillation; after ultrasonic oscillation, removing two thirds of volume of solution in the container, adding the prepared solution in the step (2) with the same volume as the removed volume into the container, and carrying out second ultrasonic oscillation; and (3) after ultrasonic oscillation, removing two thirds of volume of the solution in the container, adding the prepared solution in the step (2) with the same volume as the removed volume into the container, and performing third ultrasonic oscillation to obtain the two-dimensional material layered zinc oxide nanosheet.
Preferably, in the step (1), the preparation of the zinc oxide micron rods is carried out by selecting a chemical vapor deposition tube furnace for program temperature control and time control.
Preferably, the solution prepared in the step (2) does not chemically react with the zinc oxide micro-rods, and the solution prepared in the step (2) is acetone or absolute ethyl alcohol solution.
Preferably, the acetone or absolute ethyl alcohol solution in the step (3) completely immerses the zinc oxide micro-rods.
Preferably, the zinc oxide micro-rods in the step (3) are subjected to three ultrasonic vibration treatments.
Preferably, in the step (3), the time for performing the ultrasonic oscillation treatment by using the ultrasonic device for three times is 30 minutes, and the power is 60 KHz.
The invention provides a two-dimensional material layered zinc oxide nano-sheet obtained by the preparation method. The invention adopts a chemical vapor deposition method to prepare the zinc oxide micron rod, and then the zinc oxide micron rod is put into a solution for ultrasonic oscillation treatment. Simple equipment, controllable reaction conditions and the like.
Compared with the prior art, the invention has the following advantages and beneficial effects: the invention provides a preparation method of zinc oxide nano-sheets, which adopts a chemical vapor deposition method, has less equipment and simple operation, can change growth conditions, can prepare the size of a micro-rod, can obtain two-dimensional material layered zinc oxide by ultrasonic oscillation treatment in a prepared solution, and has easily controlled operation process.
Drawings
FIG. 1 is a flow chart of the present invention;
FIG. 2 is a diagram of a CVD prepared zinc oxide micron rod;
FIG. 3 is the appearance of an original zinc oxide single micron rod under SEM observation;
FIG. 4 is the size of a single micron rod of original zinc oxide under SEM observation;
FIG. 5 is an AFM topography of a two-dimensional layered material zinc oxide nanoplate obtained by ultrasonic post-treatment;
FIG. 6 is an AFM height diagram of a two-dimensional layered material zinc oxide nano-sheet obtained by ultrasonic post-treatment;
FIG. 7 is a table of data according to an embodiment of the present invention.
Detailed Description
The following detailed description of specific embodiments of the present invention is provided in connection with the accompanying drawings and examples, but the present invention is not limited thereto.
Example 1
Mixing zinc oxide powder, graphite powder and tin dioxide powder according to the mass ratio of 1:1:0.025, then putting the mixture into a mortar, grinding the mixture to be fine and stirring the mixture evenly, and then filling the mixed powder into an alumina burning boat. The alumina burning boat is put into a large quartz tube in the middle of the quartz tube so as to be convenient for conveying the boat to a heating part of the furnace. The mouth valve and the pressure valve of the gas storage tank are opened, and the flow rate of the carrier gas is set. The furnace was heated to 1000 ℃ at a rate of 50 ℃/min and held at that temperature for at least 30 minutes, and oxygen was continuously fed through the furnace at that temperature at an oxygen flow rate of 10 sccm. The furnace was turned off and after waiting for the furnace to cool to room temperature, white flocculent material was observed to grow inside the boat. The white floccule is a zinc oxide micron rod, and then a single zinc oxide micron rod is put into 1ml of acetone or absolute ethyl alcohol solution prepared in a container for three times of ultrasonic oscillation treatment, wherein the time and power of each ultrasonic oscillation are both 30 minutes and 60 KHz; after the first ultrasonic oscillation, 2/3ml of solution in the container is removed, 2/3ml of acetone or absolute ethyl alcohol solution is added, and the second ultrasonic oscillation is carried out; and after ultrasonic oscillation, removing 2/3ml of solution in the container again, adding 2/3ml of acetone or absolute ethyl alcohol solution, carrying out third ultrasonic oscillation, and obtaining the 4nm two-dimensional material layered zinc oxide nano-sheet after the ultrasonic oscillation is finished.
Example 2
Mixing zinc oxide powder, graphite powder and tin dioxide powder according to the mass ratio of 1:1:0.025, then putting the mixture into a mortar, grinding the mixture to be fine and stirring the mixture evenly, and then filling the mixed powder into an alumina burning boat. The alumina burning boat is put into the quartz tube in the middle of the quartz tube so as to be convenient for conveying the boat to the heating part of the furnace. The mouth valve and the pressure valve of the gas storage tank are opened, and the flow rate of the carrier gas is set. The furnace was heated to 1000 ℃ at a rate of 50 ℃/min and held at that temperature for at least 30 minutes, and oxygen was continuously fed through the furnace at that temperature at an oxygen flow rate of 15 sccm. The furnace was turned off and after waiting for the furnace to cool to room temperature, white flocculent material was observed to grow inside the boat. The white floccule is a zinc oxide micron rod, and then a single zinc oxide micron rod is put into 1ml of acetone or absolute ethyl alcohol solution prepared in a container for three times of ultrasonic oscillation treatment, wherein the time and power of each ultrasonic oscillation are both 30 minutes and 60 KHz; after the first ultrasonic oscillation, 2/3ml of solution in the container is removed, 2/3ml of acetone or absolute ethyl alcohol solution is added, and the second ultrasonic oscillation is carried out; and after ultrasonic oscillation, removing 2/3ml of solution in the container again, adding 2/3ml of acetone or absolute ethyl alcohol solution, carrying out third ultrasonic oscillation, and obtaining the 5nm two-dimensional material layered zinc oxide nano-sheet after the ultrasonic oscillation is finished.
Taking the preparation of the material in the embodiment as an example, as shown in the attached figures 2-7, the technical scheme of the invention is adopted to successfully prepare the material of the two-dimensional layered zinc oxide nano-sheet prepared by carrying out ultrasonic oscillation on the zinc oxide micro-rod material.
The preparation of the zinc oxide nano-sheet of the two-dimensional layered material can be realized by adjusting the process parameters according to the content of the invention, and the performance of the zinc oxide nano-sheet is basically consistent with that of the embodiment. The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.

Claims (4)

1. A preparation method of a two-dimensional material layered zinc oxide nano-sheet is characterized by comprising the following steps:
step 1, mixing zinc oxide powder, graphite powder and tin dioxide powder according to the mass ratio of 1:1:0.025, putting the mixture into a mortar, grinding the mixture to be fine and stirring the mixture uniformly, putting the mixture into an alumina burning boat, putting the alumina burning boat into the middle position of a quartz tube, and conveying the quartz tube and the alumina burning boat to a heating part of a furnace; heating the furnace to 1000 ℃, preserving the heat for 30 minutes, and then cooling to room temperature, wherein substances in the alumina burning boat are flocculent, namely the zinc oxide micron rods;
step 2, preparing a solution in a container;
step 3, taking a single zinc oxide micron rod from the alumina burning boat, putting the zinc oxide micron rod into the container, and performing first ultrasonic oscillation; after ultrasonic oscillation, removing two thirds of the volume of the solution from the container, adding the prepared solution in the step 2 with the same volume as the removed volume into the container, and carrying out second ultrasonic oscillation; and (3) after ultrasonic oscillation, removing two thirds of volume of the solution in the container, adding the prepared solution in the step (2) with the same volume as the removed volume into the container, and performing third ultrasonic oscillation to obtain the two-dimensional material layered zinc oxide nanosheet.
2. The method for preparing the two-dimensional material layered zinc oxide nano-sheet according to claim 1, wherein in step 1, the temperature control is performed by selecting a chemical vapor deposition tube furnace.
3. The method for preparing the layered zinc oxide nanosheet of the two-dimensional material as defined in claim 1, wherein in step 2, the prepared solution does not chemically react with the zinc oxide nanorod itself, and the prepared solution is acetone or absolute ethyl alcohol solution.
4. The method for preparing the two-dimensional material layered zinc oxide nanosheet according to claim 1, wherein in step 3, the time for the three ultrasonic vibration treatments is 30 minutes, and the power is 60 KHz.
CN202111643195.8A 2021-12-30 2021-12-30 Preparation method of two-dimensional material layered zinc oxide nanosheet Pending CN114314639A (en)

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CN102942209A (en) * 2012-11-07 2013-02-27 上海大学 Method for preparing one-dimensional nanostructure zinc oxides through changing tin doping ratio
CN103303967A (en) * 2012-03-08 2013-09-18 国家纳米科学中心 Tower-shaped layered zinc oxide nanometer rod, and preparation method and application thereof
US20140065766A1 (en) * 2012-08-30 2014-03-06 National Taiwan University Method for fabricating well-aligned zinc oxide microrods and nanorods and application thereof
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* Cited by examiner, † Cited by third party
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JP2006199552A (en) * 2005-01-24 2006-08-03 National Institute For Materials Science Zinc oxide nanoplate-nanorod bonded article and method for producing the same
CN1789137A (en) * 2005-12-07 2006-06-21 天津大学 Method for preparing nano-rod of zinc oxide or its ordered structure
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CN102912436A (en) * 2011-08-05 2013-02-06 国家纳米科学中心 Preparation method of conical zinc oxide sub-micron rods and array thereof
CN103303967A (en) * 2012-03-08 2013-09-18 国家纳米科学中心 Tower-shaped layered zinc oxide nanometer rod, and preparation method and application thereof
US20140065766A1 (en) * 2012-08-30 2014-03-06 National Taiwan University Method for fabricating well-aligned zinc oxide microrods and nanorods and application thereof
CN102942209A (en) * 2012-11-07 2013-02-27 上海大学 Method for preparing one-dimensional nanostructure zinc oxides through changing tin doping ratio
CN102910668A (en) * 2012-11-08 2013-02-06 中国科学院上海光学精密机械研究所 Preparation method of ZnO (zinc oxide) nanometer-micrometer rod with parallelogram cross section
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