Preparation method of autodoped modified high-conductivity TiO2 nanotube array

A nanotube array and electrode technology, which is applied in the field of nanomaterials, can solve problems such as inequalities, and achieve the effects of simple process, superior energy storage performance, and saving raw materials and equipment

Inactive Publication Date: 2013-10-02
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method greatly improves the TiO 2 Specific capacitance of nanotubes, but still not an economical approach considering its requirements for additional raw materials (hydrogen) and equipment

Method used

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  • Preparation method of autodoped modified high-conductivity TiO2 nanotube array
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  • Preparation method of autodoped modified high-conductivity TiO2 nanotube array

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Embodiment 1

[0030] 1) Substrate pretreatment: polish the pure titanium sheet until there is no scratch on the surface, then ultrasonically clean it in acetone, ethanol, and deionized water, and dry it;

[0031] 2) Preparation of electrolyte: weigh a certain amount of NH 4 F was dissolved in a mixture of deionized water and glycerol with a volume ratio of 1:9 to prepare a 1mol / L electrolyte;

[0032] 3) Preparation of TiO by anodic oxidation 2 Nanotubes: With the treated titanium sheet as the anode and the platinum sheet as the cathode, the anodic oxidation reaction was carried out at 20V DC voltage for 3 hours. After the reaction, it was washed with deionized water and dried in air to obtain amorphous TiO 2 nanotube arrays;

[0033] 3) The amorphous TiO 2 The nanotubes were placed in a muffle furnace, calcined at 450 °C for 2 h, and cooled naturally to obtain anatase crystal TiO 2 Nanotube array, its XRD spectrum is as follows figure 1 shown;

[0034] 4) Preparation of self-doped Ti...

Embodiment 2

[0036] 1) Substrate pretreatment: polish the pure titanium sheet until there is no scratch on the surface, then ultrasonically clean it in acetone, ethanol, and deionized water, and dry it;

[0037] 2) Preparation of electrolyte: Weigh a certain amount of NaF and dissolve it in a mixture of deionized water and ethylene glycol with a volume ratio of 1:100 to prepare a 0.1mol / L electrolyte;

[0038] 3) Preparation of TiO by anodic oxidation 2 Nanotubes: With the treated titanium sheet as the anode and graphite as the cathode, the anodic oxidation reaction was carried out at 10V DC voltage for 24 hours. After the reaction, it was washed with deionized water and dried in air to obtain amorphous TiO 2 nanotube arrays;

[0039] 3) The amorphous TiO 2 The nanotubes were placed in a muffle furnace, calcined at 700 °C for 1 h, and cooled naturally to obtain anatase crystal TiO 2 nanotube array,

[0040] 4) Preparation of self-doped TiO by cathodic reduction treatment 2 Nanotube ar...

Embodiment 3

[0042] 1) Substrate pretreatment: polish the pure titanium sheet until there is no scratch on the surface, then ultrasonically clean it in acetone, ethanol, and deionized water, and dry it;

[0043] 2) Preparation of electrolyte: weigh a certain amount of NH 4 F is dissolved in a mixture of deionized water and glycerin with a volume ratio of 5:1 to prepare a 1.5mol / L electrolyte;

[0044] 3) Preparation of TiO by anodic oxidation 2 Nanotubes: With the treated titanium sheet as the anode and glassy carbon as the cathode, the anodic oxidation reaction was carried out at a 70V DC voltage for 10 minutes. After the reaction was completed, it was washed with deionized water and dried in air to obtain amorphous TiO 2 nanotube arrays;

[0045] 3) The amorphous TiO 2 The nanotubes were placed in a muffle furnace, calcined at 400 °C for 16 hours, and cooled naturally to obtain anatase crystal TiO 2 nanotube arrays;

[0046] 4) Preparation of self-doped TiO by cathodic reduction tre...

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Abstract

The invention provides a preparation method of an autodoped modified high-conductivity TiO2 nanotube array, which comprises the following steps: growing TiO2 nanotubes on a titanium sheet in a fluorine-containing electrolyte by using a two-electrode system, and calcining at 400-700 DEG C in an air atmosphere; and polarizing the calcined TiO2 nanotube array under constant negative potential in an inert electrolyte for some time to obtain the autodoped (Ti<3+>-doped) modified high-conductivity TiO2 nanotube array. The invention is simple in technique, can easily control the doping amount, and can greatly enhance the conductivity of the TiO2 nanotubes, so that the prepared autodoped modified TiO2 nanotube array not only can be used in the fields of environmental treatment, photoelectric conversion, catalytic hydrogen production and the like, but also can be used in the fields of super capacitors, lithium ion batteries and other energy storage devices.

Description

technical field [0001] The invention belongs to the technical field of nanomaterials, and more specifically relates to a preparation method of a self-doping modified high-conductivity titanium dioxide nanotube array. Background technique [0002] In recent years, due to the rapid development of electronic science and technology, the demand for high-performance and large-capacity energy storage components is also increasing. People begin to look for green and efficient new nanomaterials to replace traditional energy storage materials. Titanium dioxide nanotubes prepared by anodic oxidation have played an important role in many scientific fields such as environmental governance, catalytic hydrogen production, and energy storage due to their excellent properties such as high order, large specific surface area, safety and stability, and controllability in synthesis. critical use. However, the inherent semiconducting properties of titanium dioxide—poor electrical conductivity an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/26C25D9/08
Inventor 张延荣周鹤
Owner HUAZHONG UNIV OF SCI & TECH
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