CN115287765A - Single crystal copper oxide nanowire and simple preparation method of copper nanowire - Google Patents

Single crystal copper oxide nanowire and simple preparation method of copper nanowire Download PDF

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Publication number
CN115287765A
CN115287765A CN202210813681.8A CN202210813681A CN115287765A CN 115287765 A CN115287765 A CN 115287765A CN 202210813681 A CN202210813681 A CN 202210813681A CN 115287765 A CN115287765 A CN 115287765A
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copper
nanowire
copper oxide
single crystal
nanowires
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CN202210813681.8A
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Inventor
张振宇
***
刘伟
于志斌
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Dalian University of Technology
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Dalian University of Technology
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/16Oxides

Abstract

The invention provides a single crystal copper oxide nanowire and a simple preparation method of the copper nanowire. The invention utilizes a constant temperature heating table to heat a common copper carrying net for a transmission electron microscope, and keeps the temperature for 3 to 5 hours, so as to prepare the monocrystal copper oxide nanowire. And putting the copper net loaded with the copper oxide nanowires into a reducing atmosphere, and heating and preserving heat for 1-3h to obtain the single crystal copper nanowires. The invention is a simple and cheap preparation method of the nano-wire.

Description

Single crystal copper oxide nanowire and simple preparation method of copper nanowire
Technical Field
The invention belongs to the field of nano-structure materials, and relates to a single crystal copper oxide nanowire and a simple preparation method of the copper nanowire.
Background
Metals and metal oxides are the most common materials in life and structural performance materials with a wide range of applications. With the development of precision and ultra-precision processing technologies, nanostructured materials gradually come into the field of vision of people and play an important role. Copper and copper oxide nanowires are taken as examples. The copper nanowire can be used for coating and manufacturing a flexible electrode to replace noble metals of indium and silver. And also in the fields of computer chips and semiconductors. More than that, copper and copper oxide nanowires also play a significant role in electronic, optoelectronic and nanoelectromechanical devices.
The current methods for synthesizing nanowires mainly include hydrothermal chemical synthesis, electrochemical deposition and elemental synthesis. The hydrothermal method for synthesizing the nano wire needs a large amount of chemical reagents and is poor in environmental protection property; the electrochemical deposition method requires the preparation of a template, is time-consuming and has a complex process. The element synthesis method requires a large cost for purchasing equipment, and the above methods have certain disadvantages.
Disclosure of Invention
In order to solve the problems, the invention provides a simple and cheap single crystal copper oxide nanowire and a simple preparation method of the single crystal copper nanowire. The invention utilizes a constant temperature heating table to heat a common copper carrying net for a transmission electron microscope, and keeps the temperature for 3 to 5 hours, so as to prepare the monocrystal copper oxide nanowire. And putting the copper net loaded with the copper oxide nanowires into a reducing atmosphere, and heating and preserving heat for 1-3h to obtain the single crystal copper nanowires.
The technical scheme of the invention is as follows:
a simple preparation method of a single crystal copper oxide nanowire comprises the following specific steps:
and a step a1, selecting a special copper grid with the diameter of 3mm for the transmission electron microscope.
And a step a2, placing the transmission electron microscope copper mesh on a heating table, wherein the heating rate is 120-5 ℃/min. Setting the processing temperature to 350-450 ℃, and keeping the temperature for 3-5h.
And a step a3, waiting for the transmission electron microscope copper mesh to be cooled to room temperature, and obtaining a large number of single crystal copper oxide nanowires. The diameter ranges from 50 nm to 300nm. The length is 2-20 μm. The copper net is placed in a transmission electron microscope to observe a large number of single crystal nanometer copper oxide nanowires.
Further, in the step a1, the copper carrying net of the transmission mirror includes various types of copper carrying nets such as a common carbon film, a micro-grid, an ultra-thin carbon film, and the like, but is not limited to these copper carrying nets. Each through net is provided with 200-400 round holes.
Further, in the step a2, the heating table used is only a heating tool and is not limited to the heating table. The heating stage is located in an atmosphere.
Further, in the step a3, the prepared copper nanowires are numerous, and the single crystal copper oxide nanowires are distributed around each round hole of the copper mesh.
The invention also provides a single crystal copper nanowire prepared by the simple preparation method of the single crystal copper oxide nanowire.
A simple preparation method of a copper nanowire comprises the following specific steps:
and b1, selecting a closed steel pipe or a closed glass pipe, placing the copper mesh loaded with the copper oxide nanowires in the closed glass pipe, and introducing reducing gas. The gas pressure is 10mbar-2bar. Maintaining a closed environment.
And b2, heating the glass tube by using a tube furnace at the temperature of 150-300 ℃ for 1-3h.
And b3, placing the copper mesh into a transmission electron microscope for observation, and finding that a large amount of copper single crystal nanowires are prepared.
Further, in the step b1, the sealed steel tube and the sealed glass tube are only a sealed space and are not limited to the glass tube and the steel tube, for example, a large sealed environment such as a glove box. The reducing gas includes hydrogen, carbon monoxide, etc., but is not limited to these two gases.
Furthermore, in the step b2, the heating mode is not limited to tube furnace heating, and any means capable of heating and holding heat may be used.
The invention has the beneficial effects that: the method can simply, efficiently and cheaply prepare the single crystal copper oxide and the copper nanowire. The prepared diameter ranges from 50 nm to 300nm. The length is 2-20 μm. Each copper mesh contains a large amount of copper oxide and copper nanowires. The prepared nanowires are comparable to commercial nanowires.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 (a) is a TEM photograph of the copper oxide nanowires prepared in the example of the present invention, and fig. 1 (b) is an electron diffraction pattern of an ade selection region in the example of the present invention.
FIG. 2 is a transmission electron microscope image of copper nanowires in an embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The following further describes the specific embodiments of the present invention with reference to the drawings and technical solutions.
Example 1
Selecting a copper mesh (micro-grid) with the diameter of 3mm as a raw material for preparing the copper oxide nanowires, placing the copper mesh on a constant-temperature heating table, wherein the atmosphere of the heating table is an atmospheric environment, the heating rate is set to be 20 ℃/min, heating is carried out to 400 ℃, and heat preservation is carried out for 4 hours. And (3) after the copper mesh is cooled to room temperature, placing the copper mesh on a transmission electron microscope to observe the single-crystal copper oxide nanowires shown in the figure 1.
Example 2
And (3) putting the copper mesh loaded with the copper oxide nanowires on quartz wool in a glass tube, and introducing 1bar of hydrogen into the quartz tube to keep the glass tube in a closed space. And (3) putting the quartz tube on a tube furnace for heating at the heating rate of 10 ℃/min to 150 ℃, and preserving heat for 1h. Then slowly cooling. The single crystal copper nanowire as shown in FIG. 2 was observed by placing the nanowire into a transmission electron microscope.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (6)

1. A simple preparation method of a single crystal copper oxide nanowire is characterized by comprising the following specific steps:
step a1, selecting a special copper grid for a transmission electron microscope;
step a2, placing the transmission electron microscope copper mesh on a heating device, wherein the heating rate is 120-5 ℃/min, the processing temperature is set to be 350-450 ℃, and the temperature is kept for 3-5h;
and a step a3, waiting for the temperature of the transmission electron microscope copper mesh to be reduced to room temperature, and obtaining a large number of single crystal copper oxide nanowires with the diameter range of 50-300nm and the length of 2-20 mu m.
2. The simple preparation method of single-crystal copper oxide nanowires of claim 1, wherein in the step a1, the transmission electron mirror copper grid comprises a common carbon film, a micro-grid, or an ultra-thin carbon film.
3. The method for simply preparing single-crystal copper oxide nanowires of claim 1, wherein in the step a1, 200-400 round holes are formed in each copper grid.
4. The method of simply manufacturing a single-crystal copper oxide nanowire according to claim 1, wherein the heating device comprises a heating stage, and an atmosphere in which the heating stage is located is an atmospheric atmosphere.
5. A simple preparation method of a single crystal copper nanowire is characterized in that the single crystal copper nanowire is prepared by the simple preparation method of the single crystal copper oxide nanowire according to any one of claims 1 to 4, and the method comprises the following specific steps:
b1, placing the copper net loaded with the copper oxide nanowires in a closed container, and introducing reducing gas, wherein the gas pressure is 10mbar-2bar;
and b2, heating the closed container at the temperature of 150-300 ℃ for 1-3h.
6. The method for simply preparing single-crystal copper nanowires as claimed in claim 5, wherein in the step b1, the closed container comprises a closed steel tube, a closed glass tube and a glove box, and the reducing gas comprises hydrogen and carbon monoxide.
CN202210813681.8A 2022-07-11 2022-07-11 Single crystal copper oxide nanowire and simple preparation method of copper nanowire Pending CN115287765A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040147049A1 (en) * 2002-12-26 2004-07-29 Seoul National University Industry Foundation Low-temperature formation method for emitter tip including copper oxide nanowire or copper nanowire and display device or light source having emitter tip manufactured using the same
US20050064158A1 (en) * 2003-09-19 2005-03-24 Hyungsoo Choi Nanostructures including a metal
CN1843932A (en) * 2006-03-03 2006-10-11 中山大学 Localized growth method of nanowire array of copper oxide
CN102051675A (en) * 2010-10-28 2011-05-11 中山大学 Method for manufacturing CuO nanowire
CN102776469A (en) * 2012-07-27 2012-11-14 中山大学 Method for preparing copper nanowires and copper nano pointed cones
CN104637831A (en) * 2015-02-12 2015-05-20 华中科技大学 Copper nanometer wire-based copper-copper bonding process
CN106424750A (en) * 2016-09-21 2017-02-22 见嘉环境科技(苏州)有限公司 Preparation method for multi-dimensional copper nanowire material

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040147049A1 (en) * 2002-12-26 2004-07-29 Seoul National University Industry Foundation Low-temperature formation method for emitter tip including copper oxide nanowire or copper nanowire and display device or light source having emitter tip manufactured using the same
US20050064158A1 (en) * 2003-09-19 2005-03-24 Hyungsoo Choi Nanostructures including a metal
CN1843932A (en) * 2006-03-03 2006-10-11 中山大学 Localized growth method of nanowire array of copper oxide
CN102051675A (en) * 2010-10-28 2011-05-11 中山大学 Method for manufacturing CuO nanowire
CN102776469A (en) * 2012-07-27 2012-11-14 中山大学 Method for preparing copper nanowires and copper nano pointed cones
CN104637831A (en) * 2015-02-12 2015-05-20 华中科技大学 Copper nanometer wire-based copper-copper bonding process
CN106424750A (en) * 2016-09-21 2017-02-22 见嘉环境科技(苏州)有限公司 Preparation method for multi-dimensional copper nanowire material

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