Preparation method for cathode material Na3V2(PO4)3/C of sodium ion battery

A sodium-ion battery and cathode material technology, applied in battery electrodes, secondary batteries, circuits, etc., can solve the problems of inability to obtain electrochemical properties of sodium vanadium phosphate, inability to guarantee high-valence vanadium reduction, and impurities in the product, etc., and achieve excellent rate Discharge performance, good application prospects, simple synthesis process

Inactive Publication Date: 2015-12-09
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These methods use carbothermal reduction of vanadium or high-temperature hydrogen reduction, high synthesis temperature, long preparation cycle, product containing impurities, high cost ...

Method used

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  • Preparation method for cathode material Na3V2(PO4)3/C of sodium ion battery
  • Preparation method for cathode material Na3V2(PO4)3/C of sodium ion battery
  • Preparation method for cathode material Na3V2(PO4)3/C of sodium ion battery

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Embodiment 1

[0024] Taking sodium dihydrogen phosphate, vanadium pentoxide and oxalic acid as raw materials, wherein the mol ratio of sodium, vanadium and phosphorus is 3:2:3, and the mol ratio of oxalic acid and vanadium pentoxide in terms of vanadium is 6:1. The raw material was mechanically ball milled for 6 hours to obtain the precursor. Transfer the precursor to a tube furnace, raise the temperature to 800 °C in a nitrogen atmosphere, and keep the temperature constant for 12 hours to obtain Na 3 V 2 (PO 4 ) 3 / C material, analyzed by X-ray diffraction ( figure 1 ) determined that the method synthesized Na 3 V 2 (PO 4 ) 3 , the space group is R-3c. figure 2 A Raman spectrum of the resulting material was shown, confirming the presence of carbon in the material.

Embodiment 2

[0026] Using sodium carbonate, ammonium dihydrogen phosphate, vanadium pentoxide, and oxalic acid as raw materials, wherein the molar ratio of sodium, vanadium, and phosphorus is 3:2:3, and the molar ratio of oxalic acid and vanadium pentoxide in terms of vanadium is 4: 1. Mechanical ball milling of raw materials for 12 hours to obtain precursors. The precursors were transferred to a tube furnace under Ar / H 2 (H 2 The content is 10%) in the atmosphere, the temperature is raised to 850 ° C, and the temperature is kept constant for 8 hours to obtain Na 3 V 2 (PO 4 ) 3 / C material.

[0027] According to Na 3 V 2 (PO 4 ) 3 / C, acetylene black, PVDF mass ratio is 80:10:10 to prepare electrode, with metal sodium as counter electrode, 1mol / LNaPF 6 Ethylene carbonate / diethyl carbonate (volume ratio 1:1) is the electrolyte, and the separator is cellgard2035. The battery is assembled in the glove box and subjected to cyclic voltammetry test. The voltage range is 2.7-3.8V, and ...

Embodiment 3

[0029] Using sodium dihydrogen phosphate, vanadium pentoxide, oxalic acid, and citric acid as raw materials, wherein the molar ratio of sodium, vanadium, and phosphorus is 3:2:3, and the molar ratio of oxalic acid and vanadium pentoxide in terms of vanadium is 3: 1. The molar ratio of citric acid and vanadium pentoxide in terms of vanadium is 1:1, and the raw materials are mechanically ball milled for 12 hours to obtain the precursor. Transfer the precursor to a tube furnace, raise the temperature to 600°C in a nitrogen atmosphere, and keep the temperature constant for 20 hours to obtain Na 3 V 2 (PO 4 ) 3 / C material.

[0030] According to Na 3 V 2 (PO 4 ) 3 / C, acetylene black, PVDF mass ratio is 70:20:10 to prepare electrode, with metal sodium as counter electrode, 1mol / LNaClO 4 PC is the electrolyte, and the separator is cellgard2035. The battery is assembled in a glove box and tested for its charge and discharge rate. The voltage range is 2-4V, and the current den...

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Abstract

The invention discloses a preparation method for a cathode material Na3V2(PO4)3/C of a sodium ion battery. The preparation method comprises the following steps of: (1) taking a high-valent vanadium source compound, a sodium source compound, a phosphorus source compound and a reducing agent as raw materials, weighing the reaction raw materials according to the molar ratio of a sodium element, a vanadium element and a phosphorus element of being 3:2:3 and the molar ratio of the reducing agent and the high-valent vanadium source compound of being 3:1 to 15:1, carrying out mechanical ball grinding for 2 to 20 hours, and reducing high-valent vanadium into low-valent vanadium at a normal temperature; and (2) forwarding a precursor obtained through ball grinding in the step (1) into an inert atmosphere or a reducing atmosphere, and carrying out heat preservation for 4 to 20 hours at 600-900 DEG C to obtain the Na3V2(PO4)3/C. The method has the advantages of short flow and low cost, and is easy to control, the prepared Na3V2(PO4)3/C is high in purity and crystallinity, and the production of the cathode material Na3V2(PO4)3/C of the sodium ion battery at a large scale is easy to realize.

Description

technical field [0001] The invention relates to a kind of sodium ion battery cathode material Na 3 V 2 (PO 4 ) 3 The preparation method of / C belongs to the field of energy materials and technology. Background technique [0002] Sodium vanadium phosphate (Na 3 V 2 (PO 4 ) 3 ) is a new type of anode material for sodium-ion batteries. It has the advantages of stable structure, flat charging and discharging platform, high capacity, and good cycle performance. It is a very promising anode material for sodium-ion batteries. The traditional preparation methods include high-temperature solid phase sintering, sol-gel method, carbothermal reduction method, hydrothermal method and so on. These methods use carbothermal reduction of vanadium or high-temperature hydrogen reduction, high synthesis temperature, long preparation cycle, product containing impurities, high cost consumption, and cannot ensure that high-valent vanadium is fully reduced under high temperature conditions,...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/58H01M4/587H01M10/054
CPCH01M4/362H01M4/5825H01M4/587H01M10/054Y02E60/10
Inventor 曹余良方永进杨汉西艾新平
Owner WUHAN UNIV
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