Preparation method of sodium vanadium trifluorophosphate serving as positive electrode material of sodium-ion battery

A technology of sodium vanadium trifluorophosphate and sodium ion batteries, which is applied in the direction of battery electrodes, positive electrodes, secondary batteries, etc., can solve the problems of battery operating voltage and energy density reduction, cycle stability deterioration, etc., to improve the average working Effects of voltage and energy density, energy density value increase, and easy availability of raw materials

Pending Publication Date: 2020-09-01
HARBIN INST OF TECH
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Problems solved by technology

[0005] In order to solve the problems of heterogeneous sodium vanadium phosphate generated due to the volatilization of fluorine element in the preparation process of sodium vanadium trifluorophosphate, the positive electrode material of sodium ion battery, which leads to the reduction of battery operating voltage and energy density and poor cycle stability, the invention provides a sodium The preparation method of sodium vanadium trifluorophosphate, the cathode material of ion battery, the method simplifies the preparation process, is convenient for practical operation, and eliminates the 3.3V (vs.Na + / Na) left and right low working voltage platform

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specific Embodiment approach 1

[0030] Specific embodiment one: what this embodiment records is a kind of preparation method of sodium vanadium trifluorophosphate sodium ion battery cathode material, the 3.3V (vs. Na + / Na) left and right discharge voltage platform, described method comprises the steps:

[0031] Step 1: Dissolve the carbon source in deionized water at room temperature, stir and mix evenly to obtain a clear solution M 1 , adjust M 1 The pH is weakly acidic; in this step, the total molar amount of carbon source added is affected by the solution M 1Restriction on the maximum dissolved amount of raw materials, the carbon source added and other raw materials added subsequently (vanadium source, phosphorus source, sodium source and fluorine source) must be completely dissolved in the solution during the operation;

[0032] Step 2: Weigh the vanadium source with a molar ratio of 5:2 to the total carbon source, and add it to the solution M 1 In , a clear solution M was obtained after maintaining...

specific Embodiment approach 2

[0037] Specific embodiment two: the preparation method of a kind of sodium-ion battery cathode material sodium vanadium trifluorophosphate described in specific embodiment one, in step one, described carbon source is organic acid and / or ammonium salt, and described organic acid is Citric acid monohydrate and / or anhydrous citric acid; the ammonium salt is a mixture of one or more of ammonium dihydrogen citrate, diammonium hydrogen citrate, and triammonium citrate. When the first type and the second type of carbon source are selected and added at the same time, the acid and the acidic ammonium salt can form a buffering pH conjugate acid-base pair in the solution.

specific Embodiment approach 3

[0038] Embodiment 3: In the preparation method of sodium vanadium trifluorophosphate, a positive electrode material for a sodium ion battery described in Embodiment 1 or 2, in step 1, the weak acidity means that the pH is 3.0-5.0. The purpose is to accelerate the complexation reaction in step two on the one hand, and to suppress the hydrolysis of fluorine and reduce its volatilization on the other hand.

[0039] Specific embodiment four: a kind of preparation method of sodium vanadium trifluorophosphate sodium ion battery anode material described in specific embodiment three, the mode of adjusting solution to be weakly acidic comprises two kinds: the one, drop ammoniacal liquor directly in the solution; On the premise that the total amount of carbon sources to be added has been selected in step 1, organic acid carbon sources and ammonium salt carbon sources are selected to be added at the same time, and it is realized by adjusting the ratio and corresponding amount of these two...

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Abstract

The invention discloses a preparation method of sodium vanadium trifluorophosphate serving as a positive electrode material of a sodium-ion battery and belongs to the technical field of battery material synthesis. The preparation method comprises the following steps: (1) dissolving raw materials such as a carbon source, a vanadium source, a phosphorus source, a fluorine source and a sodium source;(2) removing free water under a heating condition to obtain wet sol; (3) carrying out vacuum drying on the wet sol to obtain dry gel; (4) grinding the dry gel to obtain a powdery precursor; and (5) under the protection of a flowing inert atmosphere, presintering and roasting the precursor, and cooling along with the furnace. The sodium vanadium trifluorophosphate serving as a positive electrode material of a sodium-ion battery prepared by the method is high in purity, a low working voltage platform of about 3.3V (vs.Na<+> / Na) caused by a miscellaneous phase is eliminated, and the working voltage and the energy density of the positive electrode material are improved. The preparation method is simple to operate and good in reproducibility, and the prepared material has relatively high energy density and excellent rate and cycle performances and can meet the requirements of practical application of the sodium ion battery.

Description

technical field [0001] The invention belongs to the technical field of battery material synthesis, and in particular relates to a preparation method of sodium vanadium trifluorophosphate, a positive electrode material of a sodium ion battery. Background technique [0002] Lithium-ion batteries have become an ideal power source for portable electronic devices such as mobile phones, laptop computers, and high-quality cameras due to their high operating voltage, high energy density, and low environmental pollution. With the rise of the electric vehicle industry, the market's demand for lithium resources, which lithium-ion batteries rely on, has increased sharply, and its price has continued to rise. However, lithium reserves are limited after all. In the near future, lithium resources will be depleted and prices will skyrocket. Therefore, it is imminent to develop high-efficiency energy storage materials and devices with abundant resources, low price, high safety and long serv...

Claims

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Application Information

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IPC IPC(8): C01B25/455C01B25/45H01M4/58H01M10/054
CPCC01B25/455C01B25/45H01M4/5825H01M4/582H01M10/054C01P2002/72C01P2006/40H01M2004/021H01M2004/028Y02E60/10
Inventor 王振波邓亮阙兰芳隋旭磊玉富达赵磊
Owner HARBIN INST OF TECH
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