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A kind of preparation method of phosphorus niobium oxide

A technology of niobium oxides and oxides, which is applied in the fields of niobium compounds, chemical instruments and methods, and inorganic chemistry, and can solve problems such as long reaction cycles, environmental pollution, and complicated preparation processes

Active Publication Date: 2019-10-25
YANSHAN UNIV
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  • 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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  • A kind of preparation method of phosphorus niobium oxide
  • A kind of preparation method of phosphorus niobium oxide
  • A kind of preparation method of phosphorus niobium oxide

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preparation example Construction

[0021] The present invention provides a kind of preparation method of phosphorus niobium oxide, comprises the following steps:

[0022] Dissolving niobium pentachloride in an alcoholic solvent, performing a reduction reaction in a closed condition to obtain a niobium oxide precursor;

[0023] placing the red phosphorus and the niobium oxide precursor in the upstream and downstream areas of the flowing protective atmosphere respectively; raising the temperature of the upstream area to the temperature of the first area, keeping it warm for 1-10 hours, and then raising the temperature of the downstream area to the temperature of the second area , carrying out a compound reaction to obtain phosphorus and 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 invention, niobium pentachloride is dissolved in an alcohol solvent, and a reduction reaction is carried out in an airtight condition to obtain a nio...

Embodiment 1

[0048] Add niobium pentachloride powder into ethylene glycol, and stir at room temperature for 0.5 hours to obtain a solution with a concentration of 2 mol / L. ℃ for 24 hours; after the reaction is completed, filter the reaction mixture, then wash the filtered solid three times with distilled water and absolute ethanol respectively, then dry the washed solid at 70 ℃, and grind to obtain A niobium oxide precursor with an average particle size of 5nm;

[0049]The niobium oxide precursor and red phosphorus are placed in ceramic crucibles at a mass ratio of 1:3, and placed in the downstream and upstream of a vacuum atmosphere tube furnace. The distance between the niobium oxide precursor and 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 warm for 3 hours; then in an inert gas atmosphere (argon), at a rate of 2°C / min The downstream area was heated to 900°C and kept for 3 hours to obtain phosphorus niobiu...

Embodiment 2

[0051] Add niobium pentachloride powder into ethylene glycol, and stir at room temperature for 0.5 hours to obtain a solution with a concentration of 1.5 mol / L, and then put the solution into a polytetrafluoroethylene reactor. React at 150°C for 3 hours; after the reaction is completed, filter the reaction mixture, then wash the filtered solid with distilled water and absolute ethanol for 3 times respectively, then dry the washed solid at 70°C, grind, A niobium oxide precursor with an average particle size of 4nm is obtained;

[0052] The niobium oxide precursor and red phosphorus are placed in a ceramic crucible at a mass ratio of 1:6, respectively, and placed in the downstream and upstream of a 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 warm for 3 hours; then in an inert gas atmosphere (argon), at a rate of 4°...

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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 and niobium oxide. Background technique [0002] Phosphorous 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 tetrahedra along the c-axis provides three different channels for ion diffusion, namely: perovskite tunnel, four-sided tunnel and twisted four-sided tunnel. These three tunnels are not only beneficial to ion diffusion, but also PO 4 3- The stable structure of the electrode can reduce the polarization of the electrode and slow down the change of the volume of the material structure during the charge-discharge cycle, thereby improving the long-term cycle stability of the material. Application prospects. [0003] At present, phosphorous niobium oxide (PNb 9 o 25 ) is mainly prepared by multi-step chemical vapor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G33/00B82Y40/00
CPCB82Y40/00C01G33/00C01P2002/72C01P2004/64
Inventor 赵玉峰王苗
Owner YANSHAN UNIV
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