US20130270118A1 - Polycrystalline cuprous oxide nanowire array production method using low-temperature electrochemical growth - Google Patents

Polycrystalline cuprous oxide nanowire array production method using low-temperature electrochemical growth Download PDF

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US20130270118A1
US20130270118A1 US13/978,416 US201213978416A US2013270118A1 US 20130270118 A1 US20130270118 A1 US 20130270118A1 US 201213978416 A US201213978416 A US 201213978416A US 2013270118 A1 US2013270118 A1 US 2013270118A1
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nanopore
solution
manufacturing
anodic oxidation
layer
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Bae Ho Park
Sung Oong Kang
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University Industry Cooperation Corporation of Konkuk University
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University Industry Cooperation Corporation of Konkuk University
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D1/00—Electroforming
    • C25D1/04—Wires; Strips; Foils
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D1/00—Electroforming
    • C25D1/006—Nanostructures, e.g. using aluminium anodic oxidation templates [AAO]
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
    • 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
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/045—Anodisation of aluminium or alloys based thereon for forming AAO templates

Definitions

  • the present invention relates to a monocrystalline copper oxide (I) nanowire array manufacturing method using low-temperature electrochemical growth, and more particularly, to a manufacturing method allowing easy vapor deposition at low temperatures and also a monocrystalline copper oxide (I) nanowire array manufacturing method using low-temperature electrochemical growth which retains characteristics such as large-area growth, high-crystallinity nanowire, uniform radial distribution, easy length, radius adjustment, and the like.
  • a nanowire is a wire structure with a diameter of the order of nanometer (nm). Due to its geometrical nanostructure having a high aspect ratio and a large surface area, the nanowire is an important nano material in a wide range of future industrial fields (e.g., a semiconductor memory field, an LED field, a solar cell field, a sensor field, a catalyst field, a battery electrode material field, etc.). As for a nano device having wire structures made of various nano materials as basic constituent units, the constituent units have the same structure and size and a monocrystalline nanowire assuring an electrical property and continuity of electron transport is very important.
  • a monocrystalline nanowire array obtained by a self-assembling process has been recognized as a main functional unit of a high-efficiency and high-integration nano device.
  • an electrochemical growth method using a nanopore membrane (AAO) as a nano molding flask is characterized by low costs and high efficiency and is capable of adjusting a size and a length of a nanowire ranging from nanometer to micrometer in a predetermined pattern.
  • AAO nanopore membrane
  • a monocrystalline copper oxide (I) nanowire array manufacturing method suggested in the present invention is a method for manufacturing a monocrystalline oxide nanowire array having high production yield a radius of which is very uniform and a length of which can be adjusted in the range of from several ten nanometers to several micrometers by inducing complex formation and a decomposition reaction within an electrochemical aqueous solution.
  • a monocrystalline copper oxide (I) nanowire array manufacturing method using low-temperature electrochemical growth in which the method includes: a step of manufacturing a nanopore alumina layer (anodized alumina (AAO)) from a high-purity aluminum (Al) sheet by using a two-step anodic oxidation method; and a step of manufacturing a monocrystalline copper oxide (I) nanowire array by using the nanopore alumina layer as a nanopore molding flask by means of a low-temperature electrochemical growth method.
  • AAO anodized alumina
  • the step of manufacturing a nanopore membrane from a high-purity aluminum (Al) sheet by using a two-step anodic oxidation method includes: a step of electrolytically polishing the high-purity aluminum sheet by applying direct current (DC) voltage thereto in an electrolytic polishing solution; a step of primary anodic oxidation for anodically oxidizing the electrolytically polished aluminum sheet in a sulfuric acid (H 2 SO 4 ) aqueous solution or an oxalic acid (H 2 C 2 O 4 ) aqueous solution; a step of etching and removing a porous alumina layer formed by the primary anodic oxidation process with a mixed solution of phosphoric acid (H 3 PO 4 ) and chromic acid (CrO 3 ); a step of secondary anodic oxidation for anodically oxidizing the alumina sheet, from which an alumina oxide layer is removed, in a sulfuric acid (H 2 SO 4 ) aqueous solution or an
  • the electrolytic polishing solution includes chloric acid (HClO 4 ) and ethanol at a volume ratio of 1:4.
  • the step of electrolytically polishing includes electrolytically polishing the high-purity aluminum sheet at a temperature of 10° C. for 4 minutes by applying direct current voltage of +20 V thereto in an electrolytic polishing solution.
  • the step of primary anodic oxidation includes anodically oxidizing the electrolytically polished aluminum sheet at a temperature of 10° C. for 12 hours by applying voltage of +20 V thereto in a 0.3 M sulfuric acid (H 2 SO 4 ) aqueous solution or a 0.3 M oxalic acid (H 2 C 2 O 4 ) aqueous solution.
  • the step of etching and removing a porous alumina layer formed by the primary anodic oxidation process with a mixed solution of phosphoric acid (H 3 PO 4 ) and chromic acid (CrO 3 ) includes etching and removing a porous alumina layer formed by the primary anodic oxidation process at a predetermined temperature with a mixed solution of phosphoric acid (H 3 PO 4 ) and 1.8 wt % of chromic acid (CrO 3 ).
  • the step of secondary anodic oxidation includes anodically oxidizing the aluminum sheet, from which an alumina oxide layer is removed, at a temperature of 10° C. for a desired time period by applying voltage of +20 V thereto in a 0.3 M sulfuric acid (H 2 SO 4 ) aqueous solution or a 0.3 M oxalic acid (H 2 C 2 O 4 ) aqueous solution.
  • the step of protecting the nanopore alumina layer from an etching process includes protecting the nanopore alumina layer from an etching process by coating a mixture of nitrocellulose and polyester thereon after the step of secondary anodic oxidation.
  • the step of forming a nanopore channel includes forming a nanopore channel by etching the nanopore alumina layer with 5 wt % of a phosphoric acid (H 3 PO 4 ) solution at a temperature of 30° C. for 15 minutes.
  • a phosphoric acid (H 3 PO 4 ) solution at a temperature of 30° C. for 15 minutes.
  • the step of depositing a Pt layer or an Au layer includes depositing a platinum (Pt) layer or a gold (Au) layer on one side surface of the nanopore membrane to a thickness of 200 nm or more.
  • the step of manufacturing a monocrystalline copper oxide (I) nanowire array by using the nanopore alumina layer as a nanopore molding flask includes: a step of manufacturing an electrochemical deposition solution by mixing copper nitrate hydrate (Cu(NO 3 ) 2 .2.5H 2 O) and hexamethylenetetramine; a step of stirring the electrochemical deposition solution and heating the electrochemical deposition solution in a boiling water bath; a step of stirring the electrochemical deposition solution at a predetermined temperature; a step of applying a predetermined current density to the nanopore molding flask in an electrochemical reaction solution; a step of washing an electrochemically grown nanowire with ethanol and deionized water and drying the nanowire; a step of performing a heat treatment to improve crystallinity of the nanowire; and a step of removing a nanopore membrane with an NaOH aqueous solution.
  • an electrochemical deposition solution by mixing copper nitrate hydrate (Cu(NO 3 ) 2 .2.5H 2 O) and
  • FIG. 1 is a schematic diagram of a low-temperature electrochemical reaction for manufacturing a monocrystalline copper oxide (I) nanowire array
  • FIGS. 2 to 4 provide scanning electron micrographs (SEMs) ( FIGS. 2 and 3 ) and an X-ray diffraction diagram ( FIG. 4 ) of monocrystalline copper oxide (I) nanowire arrays manufactured by an electrochemical deposition method using complex formation and a decomposition reaction;
  • FIGS. 5 and 6 provide transmission electron micrographs (TEMs) of manufactured monocrystalline copper oxide (I) nanowire arrays.
  • FIGS. 7 and 8 provide high resolution transmission electron micrographs (HRTEMs) of monocrystalline copper oxide (I) nanowires.
  • a high-integration and high-quality copper oxide nanowire array is manufactured by a low-temperature electrochemical reaction using complex formation and a decomposition reaction.
  • monocrystalline nanowires or nanowire arrays require high temperature and high pressure conditions or complicated and expensive manufacturing process and equipment.
  • monocrystalline nanowires manufactured according to the present invention are grown at a low temperature in an aqueous solution composed of a small amount (typically, in the unit of mg) of eco-friendly samples, the monocrystalline nanowires having very high crystallinity are arrayed and grown with uniform size and gap and adjusted length.
  • a monocrystalline copper oxide (I) nanowire array manufacturing method using low-temperature electrochemical growth is roughly divided into a step of manufacturing a nanopore membrane with desired size and thickness and a step of manufacturing a monocrystalline copper oxide (I) nanowire array using a low-temperature electrochemical growth method.
  • Example 1 was a step of manufacturing a nanopore membrane (anodized alumina (AAO)) from a high-purity aluminum (Al) sheet by using a two-step anodic oxidation method.
  • AAO anodized alumina
  • the high-purity aluminum sheet was electrolytically polished at a temperature of 10° C. for 4 minutes by applying direct current (DC) voltage of +20 V thereto in an electrolytic polishing solution (including chloric acid (HClO 4 ) and ethanol at a volume ratio of 1:4).
  • DC direct current
  • a porous alumina layer formed by the primary anodic oxidation was etched and removed with a mixed solution of 6 wt % of phosphoric acid (H 3 PO 4 ) and 1.8 wt % of chromic acid (CrO 3 ) at a temperature of 60° C. for 24 hours.
  • the nanopore alumina layer formed as described above was protected from an etching process by coating a mixture of nitrocellulose and polyester thereon.
  • the manufactured nanopore alumina layer was etched with 5 wt % of a phosphoric acid (H 3 PO 4 ) solution at a temperature of 30° C. for 15 minutes or more so as to form a nanopore channel.
  • a phosphoric acid H 3 PO 4
  • a platinum (Pt) layer or a gold (Au) layer was deposited on one side surface of the manufactured nanopore membrane to a thickness of 200 nm or more. These metal layers were used as working electrodes in an electrochemical growth reaction.
  • Example 2 was a step of manufacturing a monocrystalline copper oxide (I) nanowire array by using the nanopore alumina layer obtained from Example 1 as a nanopore molding flask.
  • a 20 mM aqueous solution was prepared by mixing copper nitrate hydrate (Cu(NO 3 ) 2 .2.5H 2 O) and hexamethylenetetramine.
  • the prepared electrochemical deposition solution was heated in a boiling water bath until a temperature thereof reached 80° C. with stirring at a speed of 100 rpm.
  • the electrochemical deposition solution was stirred at a speed of 100 rpm for 10 minutes.
  • an electrochemically grown nanowire was washed with ethanol and deionized water and then dried.
  • a heat treatment was performed onto the manufactured nanowire to further improve crystallinity of the nanowire at a temperature of 200° C. for 10 minutes.
  • a nanopore membrane was removed with a 1.0 M NaOH aqueous solution.
  • the electrochemical growth method for manufacturing a monocrystalline copper oxide (I) nanowire array as described above is based on the present inventors' patent application (Korean Patent Application No. 10-2009-0022569) relating to a method for forming a high-crystallinity copper oxide (I) thin film.
  • copper ions (Cu 2+ ) and hydroxyl ions (OH—) required to form copper oxide (I) are generated through complex formation and a decomposition reaction within an electrochemical aqueous solution, and two-dimensional nucleation and growth for monocrystalline growth is carried out effectively through an adsorption reaction between the formed complex and a specific growing surface of the copper oxide (I).
  • the copper ions (Cu 2+ ) generated through complex formation and a decomposition reaction are reduced to cuprous oxide ions (Cu + ) and grown to become a copper oxide (I) structure through a condensation reaction with the hydroxyl ions (OH—) on a conductive metal film.
  • high-density nanowires having very uniform radius are arrayed and grown at regular positions in a regular pattern.
  • Radiuses of the manufactured nanowires can be determined by a pore size of the nanopore membrane and lengths thereof can be adjusted by an electrochemical reaction time.
  • Radiuses of the monocrystalline copper oxide (I) nanowires manufactured by the above-described method can be adjusted in the range of about 20 nm to about 450 nm and lengths thereof can be readily adjusted in the range of from several ten nanometers to several micrometers.
  • Nanowires as shown in FIG. 3 have a small radius range of about 25 ⁇ 3 nm and are grown to a length of at least 3 ⁇ m.
  • such a nanowire array can be grown to have a large area of the order of centimeter and the area is determined by an area of a nanopore membrane.
  • FIG. 4 is an X-ray diffraction diagram of manufactured monocrystalline copper oxide (I) nanowire arrays. Incubation and growth directions of the manufactured nanowires are determined by crystallinity of a metal film (a working electrode) deposited on one side surface of a nanopore membrane.
  • a metal film a working electrode
  • the deposited metal film are incubated and grown in directions [111] and [200], and thus, the incubation and growth directions of the manufactured nanowires follow these two crystal growth directions.
  • the manufactured nanowires are straightly grown in a longitudinal direction and have very smooth surfaces.
  • High resolution transmission electron micrographs (HRTEMs) ( FIGS. 7 and 8 ) of the manufactured nanowires show that crystal lattices of the manufactured nanowires are uniformly arrayed with gaps of 0.247 nanometers and 0.210 nanometers, respectively.
  • the manufactured monocrystalline copper oxide (I) nanowires are incubated and grown in directions and [200].
  • the gaps of 0.247 nanometers and 0.210 nanometers between the crystal lattices respectively correspond to a surface (111) and a surface (200) of cubic copper oxide (I).
  • the manufacturing method of the present invention it is possible to manufacture a monocrystalline oxide nanowire array having high production yield, a radius of which is very uniform and a length of which can be adjusted in the range of from several ten nanometers to several micrometers, and also possible to achieve characteristics such as large-area growth, high-crystallinity nanowire, uniform radial distribution, and easy length and radius adjustment.
  • a monocrystalline oxide nanowire array having high production yield a radius of which is very uniform and a length of which can be adjusted in the range of from several ten nanometers to several micrometers, can be manufactured at low temperatures.
  • the present invention it is possible to achieve characteristics such as large-area growth, high-crystallinity nanowire, uniform radial distribution, and easy length and radius adjustment.

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  • Organic Chemistry (AREA)
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US13/978,416 2011-01-07 2012-01-04 Polycrystalline cuprous oxide nanowire array production method using low-temperature electrochemical growth Abandoned US20130270118A1 (en)

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KR10-2011-0001703 2011-01-07
KR1020110001703A KR101332422B1 (ko) 2011-01-07 2011-01-07 전기화학성장을 이용한 단결정 산화구리 (ｉ) 나노선 어레이 제조 방법
PCT/KR2012/000076 WO2012093847A2 (ko) 2011-01-07 2012-01-04 저온전기화학성장을 이용한 단결정 산화구리 (ｉ) 나노선 어레이 제조 방법

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CN112164597A (zh) * 2020-09-28 2021-01-01 桂林理工大学 氧化铜纳米阵列电极、氧化铜纳米阵列的非固态水系柔性储能器件及其制备方法
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US20160181121A1 (en) * 2013-07-25 2016-06-23 The Board Of Trustees Of The Leland Stanford Junior University Electro-assisted transfer and fabrication of wire arrays
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