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Method for preparing TinO2n-1/TiO2 composite nano fiber based on phase transformation without reducing agent

A composite nanofiber, tino2n-1 technology, applied in chemical instruments and methods, inorganic raw material artificial filaments, inorganic chemistry and other directions, can solve the problems of difficult to control product types and low product purity, and achieve good interface lattice matching, Effects of low reaction temperature, low mismatch degree and defect density

Inactive Publication Date: 2017-05-24
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method utilizes the organic carbon source to reduce the reaction temperature, due to the introduction of other elements, the type of product is difficult to control, and the product purity is low

Method used

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  • Method for preparing TinO2n-1/TiO2 composite nano fiber based on phase transformation without reducing agent
  • Method for preparing TinO2n-1/TiO2 composite nano fiber based on phase transformation without reducing agent
  • Method for preparing TinO2n-1/TiO2 composite nano fiber based on phase transformation without reducing agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1. Preparation of H 2 Ti 3 o 7 Nanofiber Precursor

[0030] 10g TiOSO 4 ·H 2 O was mixed with 220mL of 6mol / L NaOH aqueous solution and placed in a stainless steel autoclave, and the reactor was heated to 200°C and kept for 48 hours to make TiOSO 4 ·H 2 The hydrothermal reaction of O and NaOH fully takes place, and the obtained paste precipitate product is washed repeatedly with deionized water to remove the remaining original reactants, and centrifuged (the speed is 10000 rpm, and the centrifugation time is 5min), and then Rinse repeatedly with 1mol / L hydrochloric acid and dry at 100°C to obtain H 2 Ti 3 o 7 Nanofiber precursors.

[0031] 2. Vacuum heat treatment

[0032] H obtained in step 1 2 Ti 3 o 7 Nanofiber precursors placed on Al 2 o 3 In the crucible, place the crucible in a tube furnace, and use a two-stage pump to vacuum the furnace to 1×10 -3 Pa, then raise the temperature of the furnace to 300°C at a heating rate of 5°C / min, hold for 1 hour,...

Embodiment 2

[0036] 1. Preparation of H 2 Ti 3 o 7 Nanofiber Precursor

[0037] This step is the same as Step 1 of Example 1.

[0038] 2. Vacuum heat treatment

[0039] H obtained in step 1 2 Ti 3 o 7 Nanofiber precursors placed on Al 2 o 3 In the crucible, place the crucible in a tube furnace, and use a two-stage pump to vacuum the furnace to 1×10 -4 Pa, then raise the temperature of the furnace to 300°C at a heating rate of 5°C / min, hold for 1 hour, then raise the temperature to 600°C at a heating rate of 5°C / min, and keep holding for 1 hour, so that H 2 Ti 3 o 7 Complete conversion of nanofiber precursors to anatase TiO 2 ; Then raise the furnace temperature to 800°C and keep it for 2 hours to promote the anatase TiO 2 rutile TiO 2 The phase transition occurs, and finally the temperature is raised to 950°C and kept for 3 hours to realize the rutile TiO 2 To Ti 8 o 15 phase transition.

[0040] 3. In-situ stress relief annealing

[0041] After the holding time of step ...

Embodiment 3

[0043] 1. Preparation of H 2 Ti 3 o 7 Nanofiber precursors.

[0044] This step is the same as Step 1 of Example 1.

[0045] 2. Vacuum heat treatment.

[0046] H obtained in step 1 2 Ti 3 o 7 Nanofiber precursors placed on Al 2 o 3 In the crucible, place the crucible in a tube furnace, and use a two-stage pump to vacuum the furnace to 1×10 -4 Pa, then raise the temperature to 300°C at a rate of 5°C / min, and keep it warm for 1 hour, so that the H 2 Ti 3 o 7 Complete conversion of nanofiber precursors to TiO 2 (B) Structure, then raise the temperature to 650°C at a heating rate of 10°C / min, and keep the temperature for 4 hours to make TiO 2 (B) To Ti 3 o 5 phase transition occurs.

[0047] 3. In-situ stress relief annealing

[0048] After the holding time of step 2 is reached, lower the furnace temperature to 500°C at a cooling rate of 5°C / min and hold it for 3 hours for in-situ stress relief annealing to release the stress at the phase interface; The cooling ra...

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Abstract

The invention discloses a method for preparing TinO2n-1 / TiO2 composite nano fiber based on phase transformation without a reducing agent. According to the method, H2Ti3O7 nano fiber grown by using a hydrothermal method is adopted as a precursor, and a heating calcining method is implemented in a vacuum environment to cause phase transformation on the precursor, so that the phase transformation temperature of TiO2->TinO2n-1 is reduced; and as the oxygen concentration in the environment is reduced, Ti-O bands on the surface of TiO2 are automatically broken, and thus the TinO2n-1 / TiO2 composite nano fiber of different n values can be obtained. The method is simple in process, free of reducing agent in the preparation process and low in reaction temperature; and the prepared composite nano material is good in interface lattice matching and relatively low in mismatching rate and defect density, and can be used for manufacturing visible light catalysts, lithium battery electrodes and the like.

Description

technical field [0001] The present invention relates to a kind of preparation method of composite nanofiber, particularly relate to a kind of Ti n o 2n-1 / TiO 2 Reducing agent-free preparation method of composite nanofibers. Background technique [0002] Ti n o 2n-1 It is a reducing titanium oxide material with excellent visible light response ability, electrical conductivity and electrochemical stability, and has broad application prospects in the fields of energy and environment. By adding Ti n o 2n-1 with TiO 2 Composite, can effectively improve TiO 2 Visible light responsiveness and conductivity improve the problems existing in its application. Currently, the TiO 2 Precursors undergo high-temperature heat treatment under reducing conditions to prepare Ti n o 2n-1 The most commonly used method is to obtain Ti with different n values ​​by using different reducing agents and simultaneously controlling parameters such as heat treatment temperature and time. n o ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/04C01G23/053C01G23/08D01F9/08
CPCC01G23/04C01G23/043C01G23/0532C01G23/08C01P2002/01D01F9/08
Inventor 孙颉王芳王大鹏
Owner SHAANXI NORMAL UNIV
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