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Method for synthesizing zinc oxide nano tube array by low-temperature hydrothermal method

A zinc oxide nanotube, hydrothermal technology, applied in the direction of zinc oxide/zinc hydroxide, etc., can solve the problems of large capital investment, unfavorable environmental protection, high energy consumption, etc., and achieves short production cycle, low cost, and low reaction temperature. Effect

Inactive Publication Date: 2010-11-17
TIANJIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to overcome the disadvantages of large capital investment, high energy consumption, and unfavorable environmental protection in the traditional preparation of ZnO nanotube array technology, and to provide a low-temperature hydrothermal method and a pure chemical etching process, which can be used at extremely low A method for large-scale production of high-quality ZnO nanotube arrays at low cost

Method used

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  • Method for synthesizing zinc oxide nano tube array by low-temperature hydrothermal method
  • Method for synthesizing zinc oxide nano tube array by low-temperature hydrothermal method
  • Method for synthesizing zinc oxide nano tube array by low-temperature hydrothermal method

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Embodiment 1

[0028] (1) Preparation of ZnO seed layer

[0029] Zinc acetate and monoethanolamine are used as precursor raw materials, and they are dissolved in ethylene glycol methyl ether to form a solution with a concentration of 0.5M, stirred at 50°C for 10 minutes, and then formed on the conductive glass by film pulling. layer amorphous film. The sample is then transferred to a muffle furnace and annealed for 1 hour at a temperature of 300 °C, and the amorphous film is transformed into a ZnO nanocrystalline seed layer (such as image 3 ).

[0030] (2) Low temperature hydrothermal growth of ZnO nanowires

[0031] Using 0.01M zinc nitrate as zinc source, 0.01M hexamethylenetetramine provides OH - Source, grow ZnO nanowires for 2 hours under the condition of airtight and water bath temperature of 80°C, Figure 4 is a cross-sectional view of ZnO nanowire arrays on conductive glass. After finishing the growth of ZnO nanowires, the conductive glass with ZnO nanowires grown was washed wi...

Embodiment 2

[0035] (1) Preparation of ZnO seed layer

[0036] Zinc acetate and monoethanolamine are used as precursor raw materials, and they are dissolved in ethylene glycol methyl ether to form a solution with a concentration of 0.5M, stirred at 50°C for 10 minutes, and then formed on the conductive glass by film pulling. layer amorphous film. The sample was then transferred to a muffle furnace and annealed at 300°C for 1 hour, and the amorphous film was transformed into a ZnO nanocrystalline seed layer on the conductive glass substrate.

[0037] (2) Low temperature hydrothermal growth of ZnO nanowires

[0038] Using 0.5M zinc sulfate as zinc source, 0.5M hexamethylenetetramine provides OH - Source, under the condition of airtight, water bath temperature is 80 ℃ for 2 hours to obtain ZnO nanowires. After finishing the growth of ZnO nanowires, the conductive glass with ZnO nanowires grown was washed with deionized water. Dry at 50° C. for 0.5 hours.

[0039] (3) ZnO nanowires are ch...

Embodiment 3

[0042] (1) Preparation of ZnO seed layer

[0043] A layer of ZnO seed layer was sputtered on the plastic substrate (PET) by magnetron sputtering, the sputtering parameters were: power 100W, air pressure 0.6Pa; Ar gas flow 120 / sccm; time 1 minute.

[0044] (2) Low temperature hydrothermal growth of ZnO nanowires

[0045] Using 0.025M zinc sulfate as zinc source, 0.025M hexamethylenetetramine provides OH -Source, under the condition of airtight, water bath temperature is 80 ℃ for 2 hours to obtain ZnO nanowires. After finishing the growth of ZnO nanowires, the conductive glass with ZnO nanowires grown was washed with deionized water. Dry at 50° C. for 0.5 hours.

[0046] (3) ZnO nanowires are chemically etched into ZnO nanotubes

[0047] Transfer the substrate grown with ZnO nanowires into a closed hydrothermal reactor. The reaction raw material in the hydrothermal reactor is 0.06M NaOH aqueous solution, etched at a reaction temperature of 40°C for 20 minutes, and can be obt...

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Abstract

The invention discloses a method for synthesizing a zinc oxide nano-tube array by a low-temperature hydrothermal method, which comprises: firstly, preparation of ZnO crystal seed layers; secondly, low-temperature hydrothermal growth of ZnO nano wires; and thirdly, chemical etching of the ZnO nano wires into ZnO nano-tubes. The method adopts the low-temperature hydrothermal method and utilizes pure chemical etching technology to synthesize the ZnO nano-tube array, does not need electrochemical assistance and a template, can prepare the ZnO nano-tubes with controllable pipe diameters on different types of substrates by controlling the concentration of a reactant, the hydrothermal growth time and the etching time of an alkali liquor, has low cost, low reaction temperature, short production cycle and high investment-return rate, can be directly performed in an aqueous solution, and does not generate toxic and harmful waste.

Description

technical field [0001] The invention relates to the preparation of zinc oxide (ZnO) nanometer materials, in particular to a method for synthesizing and preparing zinc oxide (ZnO) nanotube arrays by a low-temperature hydrothermal method. Background technique [0002] In the 60th issue of "Materials Express" in 2006, pages 1918-1921, the article "Polyethylene Glycol (PEG)-Assisted Synthesis of Zinc Oxide Nanotubes" written by Duan Jinxia and others mentioned: Compared with ZnO nanowires or nanorods, Hollow ZnO nanotube arrays have large surface area and strong spatial confinement effect, which have attractive application prospects in catalysts, gas-phase sensors, solar cells, next-generation ultraviolet light source materials, electronic optical displays, and electromagnetic wave shielding. Current data indicate that the synthesis of ZnO nanotubes requires high temperature (over 900 °C) or special reaction conditions (such as chemical vapor deposition device, microwave or ultr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G9/02
Inventor 杜希文傅英松刘建勇孙景
Owner TIANJIN UNIV
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