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Phosphorus niobium oxide preparation method

A niobium oxide and oxide technology, applied in niobium compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of complex preparation process, environmental pollution, long reaction period and so on

Active Publication Date: 2019-02-19
YANSHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, phosphorous niobium oxide (PNb 9 o 25 ) is mainly prepared by multi-step chemical vapor deposition method, the preparation process is complicated, the reaction cycle is long (about 20 days) and high temperature (>1000°C) is required, and the risk factor is high. At the same time, in the post-processing process, it is necessary to introduce Highly corrosive hydrofluoric acid (HF), which will pollute the environment

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preparation example Construction

[0021] The present invention provides a method for preparing phosphorus niobium oxide, which includes the following steps:

[0022] Dissolving niobium pentachloride in an alcohol solvent, and performing a reduction reaction under airtight conditions to obtain a niobium oxide precursor;

[0023] Place the red phosphorus and the niobium oxide precursors in the upstream and downstream regions of the flowing protective atmosphere respectively; heat the upstream region to the temperature of the first region for 1-10 hours, and then heat the downstream region to the temperature of the second region , The compound reaction is carried out to obtain phosphorus niobium oxide; the temperature in the first zone is 425-550°C, and the temperature in the second zone is 650-950°C.

[0024] In the present invention, niobium pentachloride is dissolved in an alcohol solvent, and a reduction reaction is performed under a closed condition to obtain a niobium oxide precursor. The invention utilizes the r...

Embodiment 1

[0048] The niobium pentachloride powder was added to ethylene glycol and stirred at room temperature for 0.5 hours to obtain a solution with a concentration of 2 mol / L. Then the solution was charged into a polytetrafluoroethylene reactor. React at ℃ for 24 hours; after the reaction is complete, filter the mixture obtained from the reaction, and then wash the filtered solids with distilled water and absolute ethanol three times respectively, and then dry the washed solids at 70°C and grind to obtain Niobium oxide precursor with an average particle size of 5nm;

[0049] Put the niobium oxide precursor and red phosphorus into a ceramic crucible at a mass ratio of 1:3, and place them in the downstream and upstream of the vacuum atmosphere tube furnace. The distance between the niobium oxide precursor and the red phosphorus is 50cm, in an inert gas atmosphere (argon), heat the upstream area to 450°C at a rate of 2°C / min and keep it for 3 hours; then in an inert gas atmosphere (argon) ...

Embodiment 2

[0051] The niobium pentachloride powder was added to ethylene glycol and stirred at room temperature for 0.5 hours to obtain a solution with a concentration of 1.5 mol / L. Then the solution was put into a polytetrafluoroethylene reactor. Under airtight conditions, React at 150°C for 3 hours; after the reaction is complete, filter the reaction mixture, and then wash the filtered solids with distilled water and absolute ethanol for 3 times, and then dry the washed solids at 70°C and grind. Obtain a niobium oxide precursor with an average particle size of 4nm;

[0052] Put the niobium oxide precursor and red phosphorus into a ceramic crucible at a mass ratio of 1:6, and place them in the downstream and upstream of the vacuum atmosphere tube furnace. The distance between the niobium oxide precursor and red phosphorus is 65cm, in an inert gas atmosphere (argon), heat the upstream area to 450°C at a rate of 2°C / min, and keep it for 3 hours; then in an inert gas atmosphere (argon), at a ...

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Abstract

The invention relates to the technical field of electrochemical energy source materials and provides a phosphorus niobium oxide preparation method. The method includes: dissolving columbium pentachloride into an alcohol solvent, and subjecting to reduction reaction under airtight conditions to obtain a niobium oxide precursor; putting red phosphorus and the niobium oxide precursor in an upstream area and a downstream area of a flowing protective atmosphere respectively; heating the upstream area into a first area temperature in a range of 425-550 DEG C, keeping the temperature for 1-10h, heating the downstream area to a second area temperature in a range of 650-950 DEG C, and performing combination reaction to obtain a phosphorus niobium oxide. The preparation method is simple, easy to operate and free of high-corrosiveness reagents, thereby being a green environmental-friendly process.

Description

Technical field [0001] The invention relates to the technical field of electrochemical energy materials, in particular to a preparation method of phosphorus niobium oxide. Background technique [0002] Phosphorus niobium oxide (PNb 9 O 25 ) Structure is NbO shared by vertices 6 Octahedron and PO 4 The three-dimensional structure formed by stacking layers of tetrahedrons along the c-axis. The special structure provides three different channels for ion diffusion, namely: perovskite tunnel, four-sided tunnel and twisted four-sided tunnel. These three tunnels are not only conducive to ion diffusion, but also PO 4 3- The stable structure of the electrode can reduce the polarization of the electrode, slow down the change of the material structure and volume during the charge and discharge cycle, thereby improving the long-cycle stability of the material, and has a wide range of energy storage in secondary batteries such as lithium sodium / potassium ion batteries. Application prospects. ...

Claims

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Application Information

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IPC IPC(8): C01G33/00B82Y40/00
Inventor 赵玉峰王苗
Owner YANSHAN UNIV
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