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 va

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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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Example Embodiment

[0034] Example 1

[0035] This embodiment discloses a sodium-doped lithium vanadium fluorophosphate material, the general formula of which is Li 0.9 / Na 0.1 VPO 4 F.

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

[0037] Mix vanadyl oxalate and ammonium dihydrogen phosphate, then add 40% of the total mass fraction of glucose, mix and stir in a water bath, the temperature of the water bath is 70℃, the stirring time is 20min, the poured liquid is uniformly viscous Thick, put it in an oven at 60℃ to dry. The dried sample is calcined in a tube furnace filled with argon to obtain VPO 4 / C. The calcination conditions are: 750°C, 10h.

[0038] VPO 4 / C and LiF and sodium source for dry ball milling, VPO 4 The molar ratio of vanadium and lithium between / C and LiF is 1:1. The ball milling conditions are: 200r / min, running for 6 hours, and the ball is separated and ground into powder. Among them, sodium source NaC...

Example Embodiment

[0045] Example 2

[0046] This embodiment discloses a sodium-doped lithium vanadium fluorophosphate material, the general formula of which is Li 0.85 / Na 0.15 VPO 4 F.

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

[0048] Ammonium metavanadate and ammonium dihydrogen phosphate were mixed at V:P=1, and 30% of the total weight of glucose was added to obtain a vanadium phosphate precursor. After the material was dried at 60°C for 4 hours, it was dried in a tube furnace under nitrogen atmosphere. Raise the temperature to 900°C at a heating rate of 5°C / min, keep it at this temperature for 10 hours, and then lower to room temperature to obtain vanadium phosphate, and then combine vanadium phosphate, lithium fluoride and sodium fluoride in a molar ratio of V:Li:Na= 1:0.85:0.15 was mixed, and the temperature was raised to 600°C at a heating rate of 4°C / min under a nitrogen atmosphere, kept for 6 hours, and cooled...

Example Embodiment

[0050] Example 3

[0051] This embodiment discloses a sodium-doped lithium vanadium fluorophosphate material, the general formula of which is Li 0.9 / Na 0.1 VPO 4 F.

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

[0053] Ammonium metavanadate and concentrated phosphoric acid were mixed at V:P=1, and 40% of the total weight of fructose was added to obtain the vanadium phosphate precursor. After the material was dried at 80°C for 3 hours, it was dried in a tube furnace under nitrogen atmosphere. Raise the temperature to 800°C at a heating rate of 5°C / min, keep it at this temperature for 10 hours, and then lower to room temperature to obtain vanadium phosphate, and then combine vanadium phosphate, lithium fluoride and sodium fluoride in a molar ratio of Li:Na::V :P=0.9:0.1:1:1 for mixing, raise to 600℃ at a heating rate of 4℃ / min under a nitrogen atmosphere, keep it for 6 hours, and cool to room temperature w...

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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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