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A kind of preparation method of aluminum oxide and carbon composite coating vanadium sodium fluorophosphate positive electrode material

A technology for carbon-coated sodium vanadium fluorophosphate and sodium vanadium fluorophosphate is applied in the field of electrochemical power sources, which can solve the problems of low electronic conductivity, side reactions between active materials and electrolyte, and decreased material cycle performance, and achieves a reduction in Effects of polarization, suppression of side reactions, and improvement of structural stability

Active Publication Date: 2020-11-06
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the NASICON structure, VO 6 The octahedron is covered with polyanionic groups PO 4 The tetrahedrons are separated, resulting in a smaller electronic conductivity of the material; in addition, Na 3 V 2 (PO 4 ) 2 f 3 In the process of charging and discharging, a higher voltage is required, which makes some side reactions between the active material and the electrolyte prone to occur, resulting in a decrease in the cycle performance of the material.

Method used

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  • A kind of preparation method of aluminum oxide and carbon composite coating vanadium sodium fluorophosphate positive electrode material
  • A kind of preparation method of aluminum oxide and carbon composite coating vanadium sodium fluorophosphate positive electrode material

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Embodiment 1

[0025] Dissolve oxalic acid (11.3459 g), sodium fluoride (2.5193 g), vanadium pentoxide (4.6010 g) and ammonium dihydrogen phosphate (3.6376 g) in deionized water and stir at 60 °C to form a gel. After drying The precursor was pre-calcined at 350 °C for 6 hours under a nitrogen atmosphere; 0.45 g of glucose was added to 5 g of the precursor, ball milled for 2 hours and then dried in an oven at 50 °C; the obtained powder was dried in a tube furnace at 700 °C under a nitrogen atmosphere Sintering for 10 hours; after cooling, grind and sieve to obtain NVPF / C cathode material. Take 1 g NVPF / C and add it into 50 ml deionized water for 40 minutes, stir to form a black suspension, then add 0.01 g aluminum nitrate nonahydrate Al(NO 3 ) 3 9H 2O, sonicate for 20 minutes and then stir for 30 minutes, then add ammonia NH 3 ·H 2 O, continue to stir at 60°C for 1.5 hours, then filter with suction, wash with deionized water several times and dry, sinter the resulting powder in a tube fur...

Embodiment 2

[0027] Dissolve oxalic acid (11.3459 g), sodium fluoride (2.5193 g), vanadium pentoxide (4.6010 g) and ammonium dihydrogen phosphate (3.6376 g) in deionized water and stir at 60 °C to form a gel. After drying The precursor was pre-calcined at 350 °C for 6 hours under a nitrogen atmosphere; 0.45 g of glucose was added to 5 g of the precursor, ball milled for 2 hours and then dried in an oven at 50 °C; the obtained powder was dried in a tube furnace at 700 °C under a nitrogen atmosphere Sintering for 10 hours; after cooling, grind and sieve to obtain NVPF / C cathode material. Take 1 g NVPF / C and add it into 50 ml deionized water for 40 minutes, stir to form a black suspension, then add 0.02 g aluminum nitrate nonahydrate Al(NO 3 ) 3 9H 2 O, sonicate for 20 minutes and then stir for 30 minutes, then add ammonia NH 3 ·H 2 O, continue to stir at 60°C for 1.5 hours, then filter with suction, wash with deionized water several times and dry, sinter the resulting powder in a tube fu...

Embodiment 3

[0029] Dissolve oxalic acid (11.3459 g), sodium fluoride (2.5193 g), vanadium pentoxide (4.6010 g) and ammonium dihydrogen phosphate (3.6376 g) in deionized water and stir at 60 °C to form a gel. After drying The precursor was pre-calcined at 350 °C for 6 hours under a nitrogen atmosphere; 0.45 g of glucose was added to 5 g of the precursor, ball milled for 2 hours and then dried in an oven at 50 °C; the obtained powder was dried in a tube furnace at 700 °C under a nitrogen atmosphere Sintering for 10 hours; after cooling, grind and sieve to obtain NVPF / C cathode material. Take 1 g of NVPF / C and add it to 50 ml of deionized water for 40 minutes, stir to form a black suspension, then add 0.03 g of aluminum nitrate nonahydrate Al(NO 3 ) 3 9H 2 O, sonicate for 20 minutes and then stir for 30 minutes, then add ammonia NH 3 ·H 2 O, continue to stir at 60°C for 1.5 hours, then filter with suction, wash with deionized water several times and dry, sinter the resulting powder in a ...

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Abstract

The invention provides an aluminum oxide and carbon composite coated sodium vanadium fluorophosphate positive electrode material and a preparation method therefor. The preparation method comprises the steps of dissolving oxalic acid H<2>C<2>O<4>, sodium fluoride NaF, a vanadium source and a phosphorus source into deionized water, and stirring at a temperature of 60 DEG C to form gel, and performing pre-calcining on the obtained powder after drying in a tubular furnace to obtain a precursor; and adding a carbon source to the precursor, performing ball milling and drying and then performing calcining in the tubular furnace in nitrogen atmosphere, and then sieving to obtain carbon-coated sodium vanadium fluorophosphate positive electrode material, performing uniform ultrasonic dispersion on the carbon-coated sodium vanadium fluorophosphate in deionized water, then adding aluminium nitrate nonahydrate Al(NO<3>)<3>.9H<2>O and performing ultrasonic processing for 20min and then stirring for 30min, next, adding ammonium hydroxide NH<3>.H<2>O, continuously stirring at a temperature of 60 DEG C for 1.5h and then performing suction filtration, washing by deionized water for multiple times and drying, and finally performing final calcining in the tubular furnace, and cooling and then sieving to obtain the aluminum oxide and carbon composite coated sodium vanadium fluorophosphate positive electrode material.

Description

technical field [0001] The invention relates to an aluminum oxide and carbon composite coating sodium vanadium phosphate cathode material and a preparation method thereof, belonging to the field of electrochemical power sources. Background technique [0002] In recent years, with the widespread application of lithium-ion batteries in the portable electronics market, especially the rapid development of the electric vehicle market, lithium resources have been consumed in large quantities and will face depletion. Therefore, sodium-ion batteries based on the abundant, low-cost, and widely distributed sodium have attracted extensive attention. Similar to lithium-ion batteries, sodium-ion batteries also work on the "rocking chair" principle. During charging and discharging, sodium ions move back and forth between the positive and negative electrodes. Compared with lithium-ion batteries, sodium-ion batteries have many potential advantages, such as: sodium is the sixth most abundan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M10/054
CPCH01M4/366H01M4/5825H01M4/625H01M4/628H01M10/054Y02E60/10
Inventor 张露露马迪杨学林周英贤
Owner CHINA THREE GORGES UNIV