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Method for preparing high-pressure alpha-PbO2-phase TiO2 nanometer material

A nanomaterial, high pressure technology, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve problems such as the difficulty of high pressure phase nanomaterials, and achieve the effect of easy control and simple preparation process

Inactive Publication Date: 2013-04-03
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, so far, TiO with a high-pressure phase 2 The preparation of nanomaterials is still a challenging work
At the same time, because the use of high-pressure technology to obtain the high-pressure phase structure of nanomaterials is often accompanied by the destruction of its morphology and changes in size, it is particularly difficult to obtain high-pressure phase nanomaterials with special morphology.
So far, there is no relevant quasi-one-dimensional high-pressure phase TiO at home and abroad. 2 Reports on the Preparation of Nanomaterials

Method used

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  • Method for preparing high-pressure alpha-PbO2-phase TiO2 nanometer material
  • Method for preparing high-pressure alpha-PbO2-phase TiO2 nanometer material
  • Method for preparing high-pressure alpha-PbO2-phase TiO2 nanometer material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A diamond anvil press with an anvil surface of 400 μm was used to pre-press a T301 steel sheet (about 10 mm×10 mm), and a hole with a diameter of 120 μm was drilled in the center of the indentation, which was used as a sample cavity for loading raw materials. anatase phase TiO 2 The nanowire raw material is filled to about 50% of the volume of the steel sheet hole (sample cavity), then ruby ​​microspheres are added as a pressure mark (to detect the pressure in the pressure cavity), and a mixed solution of formazan / ethanol with a volume ratio of 4:1 is added dropwise As a pressure transmission medium, then seal the press and pressurize. When the pressure rises to 35GPa, and the pressure is released to normal pressure, a high-pressure α-PbO 2 Phase TiO 2 Nanowires. α-PbO 2 Phase TiO 2 Nanowire SEM photos and Raman spectra see image 3 and Figure 4 .

[0033] Conclusion: When anatase phase TiO 2 The nanowire raw material is filled to about 50% of the pore volume ...

Embodiment 2

[0035] The press, sample chamber and pressure transmission medium are the same as those in Embodiment 1. anatase phase TiO 2 The nanowire raw material is filled to about 60% of the volume of the hole (sample cavity) of the steel sheet, then ruby ​​microspheres and pressure transmission medium are added, and then the press is sealed and pressurized. When the pressure rises to 30GPa, the pressure is released to normal pressure, and a high-pressure α-PbO 2 Phase TiO 2 Nanowires. α-PbO 2 Phase TiO 2 Nanowire SEM photos and Raman spectra see Figure 5 and Figure 6 .

[0036] Conclusion: When anatase phase TiO 2 The nanowire raw material is filled to about 60% of the pore volume of the steel sheet, pressurized to 30GPa, and α-PbO can be obtained after the pressure is released. 2 Phase TiO 2 Nanowires.

Embodiment 3

[0038] The press, sample chamber and pressure transmission medium are the same as those in Embodiment 1. anatase phase TiO 2 The nanowire raw material is filled to about 70% of the volume of the steel sheet hole (sample cavity), then ruby ​​microspheres and pressure transmission medium are added, and then the press is sealed and pressurized. When the pressure rises to 35GPa, the pressure is released to normal pressure, and a high-pressure α-PbO 2 Phase TiO 2 Nanowires. α-PbO 2 Phase TiO 2 Nanowire SEM photos and Raman spectra see Figure 7 and Figure 8 .

[0039] Conclusion: When anatase phase TiO 2 The nanowire raw material is filled to about 70% of the pore volume of the steel sheet, pressurized to 35GPa, and α-PbO can be obtained after the pressure is released. 2 Phase TiO 2 Nanowires.

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Abstract

The invention relates to a method for preparing a high-pressure alpha-PbO2-phase TiO2 nanometer material, which belongs to the technical field of TiO2 nanometer material preparation. A diamond anvil cell press is taken as a pressing device, an anatase TiO2 nanometer material is taken as a raw material and a mixed liquid of methanol and ethanol is taken as a pressure transmitting medium to be filled into a sample chamber, and the filling amount of the raw material is 10%-90% of the volume of the sample chamber; and the pressing device is well sealed to press, the pressure is relieved to normal pressure when reaching 18-35 GPa, so that the high-pressure alpha-PbO2-phase TiO2 nanometer material is obtained. The stable pure high-pressure alpha-PbO2-phase TiO2 nanometer material is prepared through the method; the high-pressure alpha-PbO2-phase TiO2 nanometer materials with different sizes and a mixture of nanorods and nanoparticles can be obtained through regulating the filling amount of the raw material; and a preparation process is simple, and product appearance is easily controlled.

Description

technical field [0001] The invention belongs to the preparation of high-pressure phase TiO 2 The technical field of nanomaterials, specifically related to the use of crystalline TiO 2 Nanowires are prepared by high-pressure method with high-pressure phase TiO 2 New approaches to nanomaterials. Background technique [0002] TiO 2 It is an important industrial raw material and has important application prospects in the fields of coatings, ceramics, solar cells, and photocatalysis. In nature, common TiO 2 The crystal has three structures: anatase phase, rutile phase and brookite phase. In recent years, with the continuous development of material preparation technology, new TiO 2 -B-type structure was also found. In addition, α-PbO was also found under high pressure 2 phase, baddeleyite equivalent TiO 2 of isomorphs. It is expected that these novel structures of TiO 2 May have excellent physical and chemical properties, and began to pay attention to and explore the sy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/047B82Y30/00
Inventor 刘冰冰李全军胡舒贺刘然程本源
Owner JILIN UNIV
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