KR20170056104A - Manufacturing method of copper 3-demension nanostructure - Google Patents
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- KR20170056104A KR20170056104A KR1020150159214A KR20150159214A KR20170056104A KR 20170056104 A KR20170056104 A KR 20170056104A KR 1020150159214 A KR1020150159214 A KR 1020150159214A KR 20150159214 A KR20150159214 A KR 20150159214A KR 20170056104 A KR20170056104 A KR 20170056104A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
- B82B3/0009—Forming specific nanostructures
- B82B3/0014—Array or network of similar nanostructural elements
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- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
- B82B3/0009—Forming specific nanostructures
- B82B3/0019—Forming specific nanostructures without movable or flexible elements
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- 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
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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
- C23C14/14—Metallic material, boron or silicon
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- 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
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
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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
- 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
- C23C14/34—Sputtering
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The present invention relates to a method for producing a copper three-dimensional nanostructure. A method for manufacturing a copper three-dimensional nanostructure according to an embodiment of the present invention includes growing a copper (II) hydroxide nanostructure on a copper substrate, preparing a copper oxide nanostructure from a copper (II) hydroxide nanostructure, Forming a copper oxide three-dimensional nanostructure using a chemical precipitation method or a hydrothermal synthesis method; and reducing the copper oxide three-dimensional nanostructure to a copper three-dimensional nanostructure.
Description
The present invention relates to a method for producing a copper three-dimensional nanostructure.
Recently, one-dimensional nano-sized materials have been actively studied worldwide due to their new optical, electronic, chemical, mechanical and electrical properties. Nanowires are materials with diameters in nanometers and lengths ranging from a few hundred nanometers to tens of micrometers, much larger than diameters. Among the nanowires of many materials, copper oxide (CuO) nanowires have been actively studied by various properties of copper oxide. Since copper oxide has a bandgap energy of 1.2 eV, it is capable of absorbing light in the near infrared region and consequently absorbing a wide range of light. Copper oxide nanowires have also been studied as photochemical water degradation and cathode materials for electrochemical carbon dioxide reduction. Copper metal, which can be obtained by reducing copper oxide, has also been studied as a cathode material for lithium ion batteries. Copper oxide can be easily prepared by nanowires by various methods such as thermal oxidation, chemical precipitation, and hydrothermal synthesis.
Among the various applications of copper oxide, active research is being conducted on methods for improving the efficiency in the photolysis of water. In order to increase the photodegradation efficiency of water, many studies such as a method of coating a transition metal ditallow cogenide (TMD) material such as molybdenum disulfide or tungsten molybdenum, a method of producing a heteronano structure, a method of producing a three-dimensional nanostructure have.
The present invention provides a method for manufacturing a copper three-dimensional nanostructure that increases the surface area of a substrate by preparing a three-dimensional nanostructure in which a high-density copper oxide branch is grown on a copper oxide nanowire template based on a solution.
A method for manufacturing a copper three-dimensional nanostructure according to an embodiment of the present invention includes growing a copper (II) hydroxide nanostructure on a copper substrate, preparing a copper oxide nanostructure from a copper (II) hydroxide nanostructure, Forming a copper oxide three-dimensional nanostructure using a chemical precipitation method or a hydrothermal synthesis method; and reducing the copper oxide three-dimensional nanostructure to a copper three-dimensional nanostructure.
Here, the copper (II) hydroxide nanostructure can be synthesized by wet chemical oxidation. At this time, the copper (II) hydroxide nanostructure can be synthesized using an aqueous solution for synthesizing a copper (II) hydroxide nanostructure containing sodium hydroxide and ammonium persulfate.
Next, the copper oxide nanostructure can be converted from the copper (II) hydroxide nanostructure through annealing.
Next, a seed layer may be formed using at least one of a thermal deposition method, an electron beam deposition method, and a sputter deposition method. The seed layer may be formed using at least one of Pt, Au, Ag, Cu, Fe, Ni, Al, Ti, Cr and Co.
Next, the copper oxide three-dimensional nanostructure can be formed using an aqueous solution for synthesizing a copper oxide three-dimensional nanostructure containing copper (II) nitrate trihydrate and sodium hydroxide.
Next, the copper three-dimensional nanostructure can be formed by subjecting the copper oxide three-dimensional nanostructure to a hydrogen plasma treatment.
According to the present invention, a copper oxide three-dimensional nanostructure grown on a solution provides an advantage of being able to grow uniformly over a large area to increase the surface area of the substrate. The three-dimensional nanocomposite of copper oxide can be easily grown on the substrate by using the low-temperature chemical precipitation method and the hydrothermal synthesis method, and the nanostructure can be grown by the concentration of the aqueous solution, the reaction time, and the thickness of the seed layer There is an advantage that it can be adjusted easily.
The copper oxide three-dimensional nanostructures of the present invention are readily applicable as a cathode material in photochemical water decomposition and electrochemical carbon dioxide reduction. Copper nanostructures with reduced copper oxide can also be readily applied as a cathode material in lithium ion batteries. The large surface area of the copper-based three-dimensional nanostructure is expected to have the advantage of greatly increasing the efficiency of the nanodevice.
The renewable energy resources obtained through the nano device to which the present invention is applied is a future-oriented technology that can replace a new generation of fuel.
FIG. 1 is a view for explaining a process of forming a copper oxide three-dimensional nanostructure used in the present invention,
2 is a scanning electron microscope (SEM) photograph showing that copper-based nanostructures are grown uniformly and densely,
3 is a graph and a scanning electron microscope (SEM) photograph showing that a copper (II) hydroxide nanostructure grows with time,
4 is an X-ray diffraction (XRD) diagram illustrating the conversion of a copper (II) hydroxide nanocomposite into a copper oxide nanostructure according to heat treatment time and temperature,
5 is a scanning electron microscope (SEM) photograph showing that a copper oxide three-dimensional nanostructure is grown by varying the concentration of the solution and the thickness of the seed layer,
6 is an X-ray diffractometer (XRD) diagram showing the growth of a copper oxide three-dimensional nanostructure,
FIG. 7 is a view for explaining a process for producing a copper nanostructure from a copper oxide nanostructure, and FIG.
8 is a scanning electron microscope (SEM) photograph showing that the copper nanostructure is grown uniformly and densely
9 is an X-ray diffraction (XRD) diagram showing the production of a copper nanostructure from a copper oxide nanostructure according to a hydrogen plasma treatment temperature,
10 is a view for explaining a process for producing a copper nanostructure from a copper hydroxide nanostructure, and FIG.
11 is a scanning electron microscope (SEM) photograph showing that the copper nanostructure is grown uniformly and densely
12 is an X-ray diffractometer (XRD) diagram showing the production of a copper nanostructure from a copper (II) hydroxide nanostructure according to a hydrogen plasma treatment temperature.
Hereinafter, the present invention will be described more specifically based on preferred embodiments of the present invention. However, the following embodiments are merely examples for helping understanding of the present invention, and thus the scope of the present invention is not limited or limited.
Hereinafter, a method for fabricating a copper three-dimensional nanostructure according to an embodiment of the present invention will be described with reference to FIGS. 1 to 9. FIG.
FIG. 1 illustrates a method of fabricating a copper three-dimensional nanostructure according to an embodiment of the present invention.
1 (a) shows a cleaned copper substrate, (b) shows a process of growing a copper (II) hydroxide nanostructure using wet chemical oxidation, and FIG. 1 (D) shows a process of forming a seed layer by using a deposition apparatus, and (e) shows a process of converting a copper hydroxide (II) nanostructure into a copper oxide nanostructure by a chemical precipitation method Chemical Precipitation) to form a copper oxide three-dimensional nanostructure.
2 is an image of a grown nanostructure observed with a scanning electron microscope (SEM). FIG. 2 (a) shows a copper (II) hydroxide nanostructure observed by a scanning electron microscope. Fig. 2 (b) shows the copper oxide nanostructure observed with a scanning electron microscope. FIG. 2 (c) shows a copper oxide nanostructure deposited with a copper seed layer by a scanning electron microscope. 2 (d) shows a copper oxide three-dimensional nanostructure observed with a scanning electron microscope. It can be seen that branches are formed over a large area as in the scanning electron microscope photograph. Branches of several tens of nano-sized branches were formed and the roughness of the nanostructure was increased.
FIG. 3 is a scanning electron microscope (SEM) image of a copper (II) hydroxide nanostructure grown according to a reaction time using a wet chemical oxidation method. 3 (a) to 3 (f) show that the density and length of the nanostructure increase with increasing reaction time.
After a long period of time, the nanowires aggregate and form nanostructures like flowers. The step of growing the copper hydroxide (II) nanostructure proceeds by reacting with a solution containing a copper substrate in a beaker containing a mixed solution of sodium hydroxide and ammonium persulfate. At this time, the copper (II) hydroxide nanostructure can be grown while the reaction represented by the general formula (1) takes place.
[Chemical Formula 1]
Cu + 4NaOH + (NH 4) 2 S 2 O 8 → Cu (OH) 2 +
4 (a) is an X-ray diffractometer (XRD) diagram illustrating the conversion of a copper hydroxide (II) nanostructure into a copper oxide nanostructure according to a heat treatment time, and FIG. 4 (b) XRD diffractometer (XRD) diagram illustrating the conversion of a copper (II) hydroxide nanocomposite into a copper oxide nanostructure.
It can be seen that the intensity of the peak of the copper (111) oxide increases as the annealing temperature and time are increased. At this time, the copper hydroxide (II) nanostructure can be converted into the copper oxide nanostructure while the reaction represented by the general formula (2) takes place.
(2)
FIG. 5 is a scanning electron microscope (SEM) image of a three-dimensional nanocomposite of copper oxide grown according to the concentration of a solution and the thickness of a seed layer by chemical precipitation.
5 (b) shows the result according to the low concentration, thick seed layer, and FIG. 5 (c) shows the result according to the low concentration and thin seed layer. (E) - (i) thicker concentration, (e) - (i), which results from the thickening of the seed layer .
It can be seen that as the concentration of the solution increases, as the thickness of the seed layer increases, the branch grows uniformly at a higher density. At this time, a copper oxide three-dimensional nanostructure can be formed while a two-step reaction is performed as shown in Formula (3).
(3)
6 is an X-ray diffraction (XRD) diagram of the grown copper-based nanostructures. It can be seen that copper (110) and (200) peaks appear in the copper oxide three-dimensional nanostructure. It can be seen that copper oxide having different crystal planes is grown by wet chemical oxidation and chemical precipitation.
FIG. 7 shows a process of reducing a copper oxide three-dimensional nanostructure to a copper three-dimensional nanostructure through a hydrogen plasma treatment process.
8 is a scanning electron microscope (SEM) observation of the copper nanostructure. 8 (a) shows a copper nanostructure subjected to hydrogen plasma treatment at 75 ° C for 30 minutes, and FIG. 8 (b) shows a copper nanostructure subjected to hydrogen plasma treatment at 100 ° C for 30 minutes (C) of FIG. 8 shows a copper nanostructure subjected to a hydrogen plasma treatment at 125 ° C. for 30 minutes, and FIG. 8 (d) shows a copper nanostructure subjected to hydrogen plasma treatment at 150 ° C. for 30 minutes will be. As in the scanning electron micrograph, the shape of the nanowire is maintained, but the shape is bent.
9 is an X-ray diffractometer (XRD) diagram illustrating the conversion from a copper oxide nanostructure to a copper three-dimensional nanostructure according to a hydrogen plasma treatment temperature.
As the hydrogen plasma treatment temperature increases, the intensity of the copper (111) peak gradually decreases and disappears. Thus, it can be seen that the copper oxide nanostructure completely converted into the copper three-dimensional nanostructure.
Hereinafter, a method for reducing a copper three-dimensional nanostructure from a copper (II) hydroxide nanostructure according to another embodiment of the present invention will be described.
FIG. 10 shows a process of reducing copper (II) hydroxide nanoparticles to copper three-dimensional nanostructures through a hydrogen plasma treatment process.
11 is a scanning electron microscope (SEM) observation of a copper three-dimensional nanostructure. 11 (a) shows a copper nanostructure subjected to a hydrogen plasma treatment at 75 ° C for 30 minutes, and FIG. 11 (b) shows a copper nanostructure subjected to hydrogen plasma treatment at 100 ° C for 30 minutes 11 (c) shows a copper nanostructure subjected to hydrogen plasma treatment at 125 ° C for 30 minutes, and FIG. 11 (d) shows a copper nanostructure subjected to hydrogen plasma treatment at 150 ° C for 30 minutes will be. As in the scanning electron micrograph, the shape of the nanowire is maintained, but the shape is bent.
12 is an X-ray diffraction (XRD) diagram illustrating the conversion of a copper (II) hydroxide nanocomposite into a copper nanostructure according to a hydrogen plasma treatment temperature. It can be seen that as the hydrogen plasma treatment temperature is increased, the intensity of the copper (021) and (002) peaks gradually decreases and disappears. It can be confirmed that copper nanostructures are completely converted to copper nanostructures at lower temperatures than copper oxide nanostructures. That is, it can be seen that a copper nanostructure can be obtained from a copper hydroxide (II) nanostructure directly without passing through a copper oxide nanostructure.
Although the preferred embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims. In addition, it is a matter of course that various modifications and variations are possible without departing from the scope of the technical idea of the present invention by anyone having ordinary skill in the art.
Claims (8)
Preparing a copper oxide nanostructure from a copper (II) hydroxide nanostructure;
Forming a seed layer;
Forming a copper oxide three-dimensional nanostructure using a chemical precipitation method or a hydrothermal synthesis method; And
Reducing the copper oxide three-dimensional nanostructure to a copper three-dimensional nanostructure;
A method for producing a copper three-dimensional nanostructure comprising
Wherein the copper (II) hydroxide nanostructure is synthesized by wet chemical oxidation. ≪ RTI ID = 0.0 > 11. < / RTI >
Wherein the copper (II) hydroxide nanostructure is formed using an aqueous solution for synthesizing a copper (II) hydroxide nanostructure containing sodium hydroxide and ammonium persulfate. ≪ / RTI >
Wherein the copper oxide nanostructure is converted from the copper (II) hydroxide nanostructure through annealing.
Wherein the seed layer is formed using at least one of a thermal deposition method, an electron beam deposition method, and a sputter deposition method.
Wherein the seed layer comprises at least one of Pt, Au, Ag, Cu, Fe, Ni, Al, Ti, Cr and Co.
Wherein the copper oxide three-dimensional nanostructure is formed using an aqueous solution for synthesizing a copper oxide three-dimensional nanostructure containing copper (II) nitrate trihydrate and sodium hydroxide. Dimensional nanostructure.
Wherein the copper three-dimensional nanostructure is formed by hydrogen plasma treatment of the copper oxide three-dimensional nanostructure.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021006439A1 (en) * | 2019-07-08 | 2021-01-14 | 전북대학교산학협력단 | Electrochemical water decomposition catalyst and method for producing same |
| KR20210069347A (en) | 2019-12-03 | 2021-06-11 | 인하대학교 산학협력단 | Method for manufacturing leaf-like CuO nanostructures using in-situ solution precipitation and their lithium ion battery application |
| US20220380925A1 (en) * | 2021-05-25 | 2022-12-01 | Korea Advanced Institute Of Science And Technology | Copper nanowire grown shape-memory-alloy, artificial muscle including the same, and manufacturing method thereof |
| KR20240072452A (en) | 2022-11-16 | 2024-05-24 | 한국전기연구원 | Binder Free Ink and Method for Manufactring Copper Structures Using the Same |
-
2015
- 2015-11-12 KR KR1020150159214A patent/KR20170056104A/en not_active Application Discontinuation
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021006439A1 (en) * | 2019-07-08 | 2021-01-14 | 전북대학교산학협력단 | Electrochemical water decomposition catalyst and method for producing same |
| KR20210006216A (en) * | 2019-07-08 | 2021-01-18 | 전북대학교산학협력단 | Water-spliting electrocatalyst and manufacturing method thereof |
| KR20210069347A (en) | 2019-12-03 | 2021-06-11 | 인하대학교 산학협력단 | Method for manufacturing leaf-like CuO nanostructures using in-situ solution precipitation and their lithium ion battery application |
| US20220380925A1 (en) * | 2021-05-25 | 2022-12-01 | Korea Advanced Institute Of Science And Technology | Copper nanowire grown shape-memory-alloy, artificial muscle including the same, and manufacturing method thereof |
| KR20220159016A (en) * | 2021-05-25 | 2022-12-02 | 한국과학기술원 | Copper nanowire grown shape-memory-alloy , artificial muscle including the same, and manufacturing thereof |
| US11692279B2 (en) | 2021-05-25 | 2023-07-04 | Korea Advanced Institute Of Science And Technology | Copper nanowire grown shape-memory-alloy, artificial muscle including the same, and manufacturing method thereof |
| KR20240072452A (en) | 2022-11-16 | 2024-05-24 | 한국전기연구원 | Binder Free Ink and Method for Manufactring Copper Structures Using the Same |
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