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Sodium-doped lithium vanadium fluorophosphate material and preparation method and application thereof

A lithium vanadium phosphate and sodium doping technology, which is applied in the field of materials, can solve the problems of low conductivity and achieve the effects of good crystallization performance, low production cost, and excellent electrochemical performance

Inactive Publication Date: 2020-04-28
大连融科储能集团股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to, for pure phase LiVPO 4 For the problem of relatively low conductivity of F, a sodium-doped lithium vanadium phosphate material is proposed, which is obtained by doping Na + Effectively improve the electrochemical performance of lithium vanadium phosphate

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  • Sodium-doped lithium vanadium fluorophosphate material and preparation method and application thereof
  • Sodium-doped lithium vanadium fluorophosphate material and preparation method and application thereof
  • Sodium-doped lithium vanadium fluorophosphate material and preparation method and application thereof

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Embodiment 1

[0035] This embodiment discloses a sodium-doped lithium vanadium phosphate material whose general formula is Li 0.9 / Na 0.1 VPO 4 F.

[0036] The preparation method of the sodium-doped lithium vanadium phosphate material comprises the following steps:

[0037] Mix vanadyl oxalate and ammonium dihydrogen phosphate, then add glucose accounting for 40% of the total mass fraction, mix and stir evenly in a water bath, the temperature of the water bath is 70°C, and the stirring time is 20min. Thick, put into 60 ℃ oven to dry. The dried samples were calcined in a tube furnace filled with argon to obtain VPO 4 / C. Calcination conditions are: 750°C, 10h.

[0038] will VPO 4 / C and LiF dry milled with Na source, VPO 4 The molar ratio of vanadium and lithium elements of / C and LiF is 1:1. The ball milling conditions are: 200r / min, run for 6h, separate the balls and grind them into powder. Among them, sodium sources NaCl, NaOH, CH 3 COONa.

[0039] The powdered samples were cal...

Embodiment 2

[0046] This embodiment discloses a sodium-doped lithium vanadium phosphate material whose general formula is Li 0.85 / Na 0.15 VPO 4 F.

[0047] The preparation method of the sodium-doped lithium vanadium phosphate material comprises the following steps:

[0048] Mix ammonium metavanadate and ammonium dihydrogen phosphate at V:P=1, and then add 30% of the total weight of glucose to obtain a vanadium phosphate precursor. After drying at 60°C for 4 hours, put it in a tube furnace under the protection of nitrogen atmosphere Raise it to 900°C at a rate of 5°C / min, keep it at this temperature for 10 hours, and then lower it to room temperature to obtain vanadium phosphate, and then mix vanadium phosphate, lithium fluoride and sodium fluoride in the molar ratio V:Li:Na= Mix 1:0.85:0.15, raise the temperature to 600°C at a rate of 4°C / min under a nitrogen protective atmosphere, keep it warm for 6 hours, and cool to room temperature with the tube furnace to obtain sodium-doped lithi...

Embodiment 3

[0051] This embodiment discloses a sodium-doped lithium vanadium phosphate material whose general formula is Li 0.9 / Na 0.1 VPO 4 F.

[0052] The preparation method of the sodium-doped lithium vanadium phosphate material comprises the following steps:

[0053] Mix ammonium metavanadate and concentrated phosphoric acid at V:P=1, and then add fructose accounting for 40% of the total weight to obtain a vanadium phosphate precursor. After drying at 80°C for 3 hours, put it in a tube furnace under the protection of nitrogen atmosphere Raise to 800°C at a rate of 5°C / min, keep at this temperature for 10 hours, then drop to room temperature to obtain vanadium phosphate, and then mix vanadium phosphate, lithium fluoride and sodium fluoride in the molar ratio Li:Na::V : P=0.9:0.1:1:1 for mixing, under a nitrogen protective atmosphere, the heating rate is raised to 600°C at a rate of 4°C / min, kept for 6 hours, and cooled to room temperature with the tube furnace to obtain sodium-dope...

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Abstract

The invention provides a sodium-doped lithium vanadium fluorophosphate material and a preparation method and application thereof, the general formula of the sodium-doped lithium vanadium fluorophosphate material is Li(1-x) / NaxVPO4F, and x is more than 0 and less than or equal to 0.3. The preparation method of the sodium-doped lithium vanadium fluorophosphate material comprises the following steps:mixing a vanadium source, a phosphorus source and a carbon source at 60-100 DEG C, and performing drying; calcining the product in an inert atmosphere to obtain carbon-doped vanadium phosphate; mixing carbon-doped vanadium phosphate, LiF and a sodium source, and performing dry ball milling to obtain uniformly mixed powder; and calcining the powder at 650-800 DEG C for 1-6 hours to obtain the sodium-doped lithium vanadium fluorophosphate material, so as to obtain the sodium-doped lithium vanadium fluorophosphate material. The electrochemical performance of lithium vanadium fluorophosphate is effectively improved by doping Na+, the method is simple in process route, easy to operate and low in production cost, and large-scale production can be realized.

Description

technical field [0001] The invention relates to material technology, in particular to a sodium-doped lithium vanadium phosphate material, its preparation method and application. Background technique [0002] Lithium-ion batteries have been widely used in various fields such as life, production, and energy storage this year, so it is imminent to develop high-performance energy storage materials. Traditional lead-acid, cadmium-nickel, and nickel-metal hydride batteries have a series of shortcomings such as low working voltage and density and pollute the environment, and are gradually being eliminated from the market. Lithium-ion batteries are well known for their good safety performance, no memory effect, and no pollution. As a key factor of lithium-ion batteries, cathode materials have a direct impact on the overall performance of lithium-ion batteries. With the development of lithium-ion battery industrialization, obtaining batteries with high specific capacity, high cycle...

Claims

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Application Information

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IPC IPC(8): C01B25/455H01M4/58H01M10/0525
CPCC01B25/455H01M4/5825H01M4/582H01M10/0525C01P2002/72C01P2004/03Y02E60/10
Inventor 唐雨微杜乃旭邸卫利王隆菲阎成友
Owner 大连融科储能集团股份有限公司
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