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Large-scale preparation method of niobium pentoxide nanowires and hydrogen-sensitive element thereof

A niobium pentoxide nanometer, large-area technology, applied in chemical instruments and methods, electrical components, nanotechnology, etc., can solve the problems of high cost, low repeatability, disadvantage, etc., to reduce equipment and production costs, improve The effect of surface area, low power consumption

Inactive Publication Date: 2011-09-14
武汉正光恒远科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the production of Nb2O5 nanowires by hydrothermal method is low, the morphology is not easy to control, and the repeatability is not high, so it is not suitable for large-scale and rapid synthesis of Nb 2O5 nanowires; and the plasma oxidation method is suitable for large-area synthesis of Nb2O5 nanowires , but its cost is high, and the equipment and process methods are relatively complicated; the literature published by Varghese et al. in 2008 reported a thermal oxidation method to prepare Nb2O5 nanowires And its field emission characteristics, put the Nb foil cut into 0.5mm length and width into a small tube with a diameter of 2.5mm, and put it in a vacuum tube furnace for thermal oxidation treatment
Although the use of small tubes can stabilize the gas flow, it limits the size of the prepared samples and cannot realize large-area Nb 2 o 5 Preparation of nanowire samples, which are based on Nb 2 o 5 The production of nanowires for various gas sensors, dye-sensitized solar cells and field emission devices is extremely unfavorable

Method used

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  • Large-scale preparation method of niobium pentoxide nanowires and hydrogen-sensitive element thereof
  • Large-scale preparation method of niobium pentoxide nanowires and hydrogen-sensitive element thereof
  • Large-scale preparation method of niobium pentoxide nanowires and hydrogen-sensitive element thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Prepare Nb according to the previous steps 2 o 5 Nanowires, where the Nb foils are cut into small pieces of 5mm×10mm in steps 1 and 2, and after cleaning, place 3-5 pieces of cut Nb foils in a ceramic burning boat and place them in the furnace tube for heating The center of the zone, other steps are the same as above, and the specific process conditions are shown in the table below:

[0039]

[0040] In the first embodiment above, on the basis of ensuring that the flow rate of Ar is constant, change O 2 flow rate, the surface morphology of the obtained sample is as attached image 3 shown. In order to obtain large area, high aspect ratio Nb 2 o 5 For nanowires, the oxygen flow rate should be controlled not to exceed 20 sccm, and the Nb prepared by too high oxygen flow rate 2 o 5 The aspect ratio and density of nanowires are both low. Nb prepared under the conditions of No. 2 2 o 5 With the best surface morphology, its phase and microstructure are as attache...

Embodiment 2

[0042] Prepare Nb according to the previous steps 2 o 5 Nanowires, wherein in steps 1 and 2, the Nb foil is cut into a strip-shaped foil of 60mm×30mm-60mm×50mm, and after the cleaning process is completed, it is bent into a cylindrical shape and attached to the furnace of the vacuum tube furnace The inner wall of the tube and placed in the center of the heating zone, if attached figure 1 (b) shown.

[0043] Other steps are all the same as above, and the specific process conditions are shown in the table below:

[0044]

[0045] In above-mentioned embodiment two, determine that Ar flow rate, heating rate and holding temperature are constant, at lower O 2 The heat preservation and oxidation time under the flow rate is longer, with the O 2 The flow rate is gradually increased, and the holding oxidation time is gradually reduced to 60min. In this example, a large area of ​​uniformly grown Nb can be obtained 2 o 5 nanowire film structure.

Embodiment 3

[0047] Prepare Nb according to the previous steps 2 o 5 Nanowires, where in steps 1 and 2, the Nb foil is cut into 120mm×30mm-120mm×50mm strip foil and the cleaning process is completed, and it is folded and bent every 2-4mm to form an organ shape and rolled into a circle The cylindrical shape makes it attached to the inner wall of the furnace tube of the vacuum tube furnace and placed in the center of the heating area. Other steps are all the same as above, and the specific process conditions are shown in the table below:

[0048]

[0049] In the above example three, it is determined that the Ar flow rate, heating rate and holding temperature are constant, and at a lower O 2 The heat preservation and oxidation time under the flow rate is longer, with the O 2 The flow rate is gradually increased, and the holding oxidation time is gradually reduced to 60min. In this example, a large area of ​​uniformly grown Nb can be obtained 2 o 5 nanowire film structure.

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Abstract

The invention discloses a large-scale preparation method of niobium pentoxide nanowires and a hydrogen-sensitive element thereof. The preparation method particularly comprises the following steps of: strictly cleaning Nb foils cut into suitable sizes, arranging the foils in a vacuum tube type furnace after a bending or folding treatment, and strictly controlling processing conditions (such as Ar flow rate, O2 flow rate, holding temperature, time and the like) of a thermal oxidation process to synthesize large-scale Nb2O5 nanowires with higher length diameter ratios. By adopting the large-scale preparation method disclosed by the invention, the large-scale synthesis of the Nb2O5 nanowires with the higher length diameter ratios can be realized in a limited-volume furnace tube, thus the production cost can be effectively reduced. Hydrogen-sensitive elements manufactured from Pt electrodes, prepared by sputtering Nb2O5 nanowires as sensitive materials, have the characteristics of small size, low energy consumption and the like, and represent higher response speed and higher sensitivity at the room temperature towards a hydrogen-containing atmosphere; and the size, the energy consumption and the production cost of hydrogen sensors can be hopefully reduced.

Description

technical field [0001] The invention relates to a large-area preparation method of niobium pentoxide nanowire (and its hydrogen sensitive element), which belongs to the technical field of inorganic semiconductor nanometer material preparation technology. Background technique [0002] Hydrogen is an ideal renewable clean energy. Its flammability and explosiveness caused by its low flash point make hydrogen sensors particularly important in chemical and safety fields such as fire alarms, gas leakage, and combustion control. In addition, in medical fields such as detecting bacterial infection, hydrogen sensors also have high application value. metal oxide semiconductor (TiO 2 , ZnO and SnO 2 etc.) Thin-film hydrogen sensor is currently the most researched type of hydrogen sensor, and the concentration of hydrogen can be detected by using the change degree of the resistance value of the sensitive element in the hydrogen-containing atmosphere. However, at present, the semicond...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G33/00B82Y40/00H01L49/00G01N27/04H10N99/00
Inventor 顾豪爽王钊胡永民胡明哲王威
Owner 武汉正光恒远科技有限公司
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