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Preparation of high-purity phase ti by one-step method under inert atmosphere 4 o 7 nanomaterials approach

An inert atmosphere, nanomaterial technology, applied in the field of material science, can solve the problems of complex preparation process, high energy, difficult conversion, etc., and achieve the effect of simplifying preparation steps, improving purity, and low equipment requirements

Active Publication Date: 2020-12-01
CHONGQING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] For TiO existing in the prior art 2 As a precursor, to convert it into a Magnéli phase triclinic structure requires a lot of energy, is not easy to convert, and the preparation process is complicated. An inert atmosphere is provided for the next step to prepare high-purity phase Ti. 4 o 7 The method of nanomaterials, the preparation method can realize the preparation of high-purity phase Ti in one step 4 o 7 , and low energy consumption, avoiding the potential safety hazards of using hydrogen as a reducing agent at high temperatures

Method used

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  • Preparation of high-purity phase ti by one-step method under inert atmosphere <sub>4</sub> o <sub>7</sub> nanomaterials approach
  • Preparation of high-purity phase ti by one-step method under inert atmosphere <sub>4</sub> o <sub>7</sub> nanomaterials approach
  • Preparation of high-purity phase ti by one-step method under inert atmosphere <sub>4</sub> o <sub>7</sub> nanomaterials approach

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Effect test

Embodiment 1

[0031] A one-step method for preparing high-purity phase Ti in an inert atmosphere 4 o 7 The method for nanometer material, its specific preparation steps are:

[0032] Using metatitanic acid as a precursor, the weight ratio of the metatitanic acid precursor and reducing agent charcoal powder is 98.7:1.3. After mixing, put it into the reaction boat, then place the reaction boat in a closed tube furnace for calcination, and feed N into the tube furnace. 2 , control N 2 The flow rate is 30sccm. First, heat up to the first temperature of 800°C at a rate of 5°C / min and hold for 5 hours, then raise the rate of 1°C / min to the second temperature of 950°C and hold for 10 hours to obtain high-purity Phase Ti 4 o 7 .

[0033] Wherein, the metatitanic acid used in this embodiment is commercially available metatitanic acid, and the manufacturer is Zhengzhou Qichen Chemical Products Co., Ltd.

Embodiment 2

[0035] A one-step method for preparing high-purity phase Ti in an inert atmosphere 4 o 7 The method for nanomaterials, comprising the steps of:

[0036] (1) Dissolve titanium dioxide in 3M KOH, stir for 6 hours to form a uniform colloid, then pour the above colloid solution into a polytetrafluoroethylene high-pressure reactor, and place the reactor in an oven with a temperature of 120°C for 24 hours ; After the reaction finishes, wait for natural cooling and filter to obtain the precipitate;

[0037] (2) The precipitate prepared above is washed with deionized water until the solution is neutral;

[0038] (3) Add 0.05M HCl solution to the solution in step (2), adjust the pH value of the solution to 0.1, stir and react for 24 hours; clean the reacted precipitate with deionized centrifugation, and dry it at 60°C for 12 hours , namely to obtain the metatitanic acid precursor.

[0039] Using metatitanic acid as a precursor, the weight ratio of the metatitanic acid precursor and...

Embodiment 3

[0041] A one-step method for preparing high-purity phase Ti in an inert atmosphere 4 o 7 The method for nanomaterials, comprising the steps of:

[0042] (1) Dissolve titanium dioxide in 10M NaOH, stir for 3 hours to form a uniform colloid, then pour the above colloid solution into a polytetrafluoroethylene high-pressure reactor, and place the reactor in an oven at 200°C for 3 hours ; After the reaction finishes, wait for natural cooling and filter to obtain the precipitate;

[0043] (2) The precipitate prepared above is washed with deionized water until the solution is neutral;

[0044] (3) Add 2M H to the solution of step (2) 2 SO 4 solution, adjusting the pH value of the solution to 1, stirring and reacting for 24 hours; cleaning the reacted precipitate by deionized centrifugation, and drying at 60° C. for 12 hours to obtain a metatitanic acid precursor.

[0045] Using metatitanic acid as a precursor, the weight ratio of the metatitanic acid precursor and reducing agent a...

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Abstract

The invention provides a method for preparing a high-purity-phase Ti4O7 nano-material in an inert atmosphere through a one-step technology. Metatitanic acid serves as a precursor, the metatitanic acidprecursor and a reducing agent carbon powder are mixed, then are placed in a closed reactor and are calcined, an inert gas is introduced into the reactor, heat preservation is conducted for a certainperiod of time at a first temperature of 800-950 DEG C, and then heat preservation is conducted for a certain period of time at a second temperature of 950-1300 DEG C to obtain the high-purity-phaseTi4O7. The metatitanic acid is used as the precursor, the carbon powder is used as the reducing agent, the carbon powder can be converted into CO or CO2 after reaction, the CO or CO2 overflows and isautomatically eliminated, subsequent separation steps are not needed, one-step preparation can be realized, the preparation steps are greatly simplified, and the purity of the product is improved.

Description

technical field [0001] The invention belongs to the technical field of material science, and in particular relates to the preparation of high-purity phase Ti by a next-step method in an inert atmosphere 4 o 7 methods for nanomaterials. Background technique [0002] Magnéli phase titanium oxide, also known as titanium suboxide, is a general term for a series of non-stoichiometric titanium oxides, with the general formula Ti n o 2n-1 . It is based on rutile TiO 2 In the lattice structure, one oxygen atom is lost every n layers, and the two-dimensional chains of the octahedron are shared by planes, forming ordered planar oxygen vacancies. [0003] In recent years, Magnéli phase titanium oxide has received widespread attention at home and abroad. Due to its high conductivity, chemical stability, and strong corrosion resistance, it has been widely used in inert electrodes, HER, ORR, NRR, fuel cells, and lithium batteries. field has great application value. Of all the phase...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/04
CPCC01G23/04C01P2002/72C01P2002/85C01P2004/03C01P2004/04C01P2004/61C01P2004/62
Inventor 王煜张慧娟
Owner CHONGQING UNIV