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Preparation method of porous orthorhombic-phase niobium pentoxide nano material

A technology of niobium pentoxide and nanomaterials, applied in chemical instruments and methods, nanotechnology for materials and surface science, nanotechnology, etc. Controllable preparation of flowers, difficult to control product morphology, poor repeatability and other problems, to achieve the effect of uniform morphology, low cost and strong controllability

Inactive Publication Date: 2021-05-25
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the morphology of the products obtained by these methods is not easy to control, the crystal form is poor, and the repeatability is not good.
So far, no controllable preparation of porous orthorhombic phase niobium pentoxide nanosheets and nanoflowers

Method used

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  • Preparation method of porous orthorhombic-phase niobium pentoxide nano material
  • Preparation method of porous orthorhombic-phase niobium pentoxide nano material
  • Preparation method of porous orthorhombic-phase niobium pentoxide nano material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Add 0.1g of niobium pentachloride to 50mL of ethanol, sonicate evenly, slowly add sodium hydroxide dropwise to adjust the pH to 8.5, and solvent heat in the reaction kettle for 12h. The reaction product is washed by centrifugation, heated and dried under normal pressure to obtain white niobium pentoxide precursor powder.

[0035] (2) The obtained niobium pentoxide precursor was calcined in a muffle furnace at 600° C. for 5 hours to obtain porous nanoplatelet niobium pentoxide.

[0036] The XRD diffraction peak of the obtained niobium pentoxide belongs to PDF card: 30-0837, which is the orthorhombic phase of niobium pentoxide. The size of the nanosheet is about 1 μm-2 μm, the thickness is about 10 nm, and the pore size ranges from 10-80 nm. Lithium battery test results: when charging and discharging at 100mA / g, the specific capacity of the electrode material is as high as 190mAh / g.

Embodiment 2

[0038] (1) Add 0.15g of niobium oxalate into 80mL of water, shake evenly, slowly add ammonia water dropwise to adjust the pH to 9, and solvoheat in the reaction kettle for 20h. The reaction product was washed by suction filtration and freeze-dried to obtain white niobium pentoxide precursor powder.

[0039] (2) The obtained niobium pentoxide precursor was calcined in a muffle furnace at 650° C. for 3 hours to obtain porous nanosheet-shaped orthorhombic phase niobium pentoxide.

[0040] The obtained niobium pentoxide nano sheet has a size of about 1 μm-3 μm, a thickness of about 20 nm, and a pore diameter range of 50-200 nm. Lithium battery tests show that when charging and discharging at 500mA / g, the specific capacity of the electrode material can reach 170mAh / g.

Embodiment 3

[0042] (1) Add 0.2g of niobium ethanol to a mixed solvent of 100mL of ethanol and ethylene glycol (volume ratio: 1:1), stir evenly, slowly add potassium hydroxide dropwise to adjust the pH to 10, and solvoheat in the reaction kettle for 15h . The reaction product is washed by centrifugation, heated and dried in vacuum to obtain white niobium pentoxide precursor powder.

[0043] (2) The obtained niobium pentoxide precursor was calcined in a muffle furnace at 700° C. for 1.5 h to obtain porous nanoflower-shaped orthorhombic phase niobium pentoxide.

[0044]The obtained niobium pentoxide nanoflowers have a size of about 500nm-1.5μm, are self-assembled by porous nanosheets with a thickness of about 20nm, and have a pore size range of 20-100nm. Lithium battery test results: when charging and discharging at 200mA / g, the specific capacity of the electrode material can reach 185mAh / g.

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Abstract

The invention discloses a preparation method of a porous orthorhombic-phase niobium pentoxide nano material, and belongs to the technical field of controllable preparation and morphology control of metal oxide nano materials. Niobium salt is taken as a raw material, solvothermal reaction is carried out in different solvents, and orthorhombic niobium pentoxide nano sheets and nano flowers with good two-dimensional sheet morphology, porous distribution and excellent electrochemical performance are synthesized. The preparation method has the advantages of simple equipment, convenience in operation, controllable morphology, good repeatability, low cost and easiness in process amplification. The prepared product is uniform in morphology, good in crystal form, high in controllability, high in quality and good in performance, and can be widely applied to various fields of batteries, super capacitors, catalysis and the like. Particularly, as a lithium ion battery negative electrode material, the orthorhombic niobium pentoxide two-dimensional nano material has the advantages of high capacity, high magnification and long cycle life.

Description

technical field [0001] The invention belongs to the technical field of controllable preparation and shape control of metal oxide nanomaterials, and specifically relates to a preparation method of porous orthogonal phase niobium pentoxide nanosheets and nanoflowers. The obtained porous orthorhombic phase niobium pentoxide nanosheets and nanoflowers exhibit excellent electrochemical properties and can be widely used in supercapacitors, batteries, and catalysis. Background technique [0002] Niobium pentoxide (Nb 2 o 5 ), as an important metal oxide material, has excellent physical and chemical properties and is widely used in photocatalysis, supercapacitors, lithium-ion / sodium-ion batteries and sensors. Among them, the orthorhombic phase of niobium pentoxide (T-Nb 2 o 5 ) has a large interlayer distance, which can provide an effective channel for ion migration, and store a large amount of lithium ions without changing the structure, so it shows high lithium storage capacit...

Claims

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Application Information

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IPC IPC(8): C01G33/00H01M4/485H01M10/0525B82Y30/00B82Y40/00H01M4/02
CPCB82Y30/00B82Y40/00C01G33/00C01P2002/72C01P2004/20C01P2004/61C01P2004/62C01P2004/64C01P2006/17C01P2006/40H01M4/485H01M10/0525H01M2004/027Y02E60/10
Inventor 吴忠帅秦洁琼苏峰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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