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A nitrogen-hydrogen in-situ double-doped soft carbon/sodium vanadium phosphate composite material and its preparation method and application

A technology of sodium vanadium phosphate and composite materials, applied in structural parts, electrical components, battery electrodes, etc., can solve the problems of organic solvent DMF, which is not environmentally friendly, poor in electrical conductivity and electrochemical performance, and high cost of synthetic materials, and achieves improved strength and The effect of structural stability, good compatibility and low cost

Active Publication Date: 2020-08-04
江苏富爱科技发展有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, sodium vanadium phosphate has limited its development and application due to poor conductivity and electrochemical performance.
Carbon doping of sodium vanadium phosphate has been proved to be a method that can effectively improve its conductivity and electrochemical performance. At present, carbon coating methods are mostly used. For example, Chinese patent document CN105336924A discloses a carbon-coated vanadium phosphate The preparation method of sodium positive electrode material uses glucose as a reducing agent and a carbon source, water as a dispersant, and NH 4 V O3 , NaH 2 PO 4 2H 2 O and glucose are ball milled in water, spray-dried and calcined to obtain a carbon-coated granular sodium vanadium phosphate positive electrode material. The first charge-discharge specific capacity at 1C rate is up to 93.5mAh / g, and the capacity retention rate after 50 cycles of 1C cycle 97.7%, not only the electrochemical performance is average, but also the preparation process is complicated and the cost is high
Chinese patent document CN109768258A discloses an in-situ synthesis method and application of a sodium vanadium phosphate-carbon-graphene nanocomposite material. In this method, a suspension containing graphene is added when synthesizing sodium vanadium phosphate. , synthesized a graphene-coated sodium vanadium phosphate / carbon composite material; when this material is used as a positive electrode material for a sodium-ion battery, the first discharge specific capacity is 98mAh / g at 1C, which not only has general electrochemical performance but also is caused by the high price of graphene. The cost of its synthetic materials is high, and its use of organic solvent DMF is not environmentally friendly

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  • A nitrogen-hydrogen in-situ double-doped soft carbon/sodium vanadium phosphate composite material and its preparation method and application
  • A nitrogen-hydrogen in-situ double-doped soft carbon/sodium vanadium phosphate composite material and its preparation method and application
  • A nitrogen-hydrogen in-situ double-doped soft carbon/sodium vanadium phosphate composite material and its preparation method and application

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Embodiment 1

[0042] A preparation method of nitrogen-hydrogen in-situ double-doped soft carbon / sodium vanadium phosphate composite material, the steps are as follows:

[0043] Soak 6g of soybeans in 40ml of 15% ethanol aqueous solution for 5h, grind it into a slurry with 60mL of 15wt% ethanol aqueous solution and pass through a 120 mesh sieve, then heat the soybean milk at 100°C for 0.5h to obtain solution A; Add 4.6g of ammonium metavanadate and 4.68g of sodium dihydrogen phosphate dihydrate into solution A, stir in a water bath at 80°C for 0.5h to dissolve and react, then adjust pH=5 with acetic acid to condense the system to obtain condensate and liquid Mixture B; put the mixture B into the reaction kettle and keep it under water heat for 24 hours at 100°C, and dry the obtained solidified body at 80°C for 6 hours; grind the dried solidified body to less than 100um under nitrogen, and pass it from the chamber at 5°C / min The temperature was raised to 350°C for 4 hours, and then heated to ...

Embodiment 2

[0052] A preparation method of nitrogen-hydrogen in-situ double-doped soft carbon / sodium vanadium phosphate composite material, the steps are as follows:

[0053] Soak 7g soybeans in 50ml mass concentration of 10% ethanol aqueous solution for 4h, grind it into a slurry with 60mL 10wt% ethanol aqueous solution and pass through an 80 mesh sieve, then heat the soybean milk at 80°C for 0.5h to obtain solution A; Add 4.6 g of ammonium metavanadate and 4.68 g of sodium dihydrogen phosphate dihydrate to solution A, stir in a water bath at 100°C for 0.5 h to dissolve and react, then adjust the pH to 6 with acetic acid to coagulate the system to obtain condensate and liquid Mixture B; put the mixture B into the reaction kettle and keep it under water heat for 22h at 120°C, and dry the solidified body at 100°C for 5h; grind the dry solidified body to less than 100um, and put it under nitrogen at 4°C / min from the chamber The temperature was raised to 300°C for 6 hours, and then heated to...

Embodiment 3

[0056] A preparation method of nitrogen-hydrogen in-situ double-doped soft carbon / sodium vanadium phosphate composite material, the steps are as follows:

[0057] Soak 5g of black beans in 30ml of 20% ethanol aqueous solution for 8h, grind it into a slurry with 60mL of 20wt% ethanol aqueous solution and pass through a 120 mesh sieve, then heat the soybean milk at 100°C for 0.5h to obtain solution A; Add 4.6g of ammonium metavanadate and 4.68g of sodium dihydrogen phosphate dihydrate to solution A, stir in a water bath at 100°C for 0.5h to dissolve and react, then use acetic acid to adjust pH=4 to coagulate the system to obtain condensate and liquid The mixture B; put the mixture B into the reaction kettle and keep it at 80°C for 26h, and dry the obtained solidified body at 60°C for 8h; grind the dried solidified body to less than 100um and put it under nitrogen at 7°C / min from the chamber The temperature was raised to 400°C for 3 hours, and then heated to 900°C at 5°C / min for ...

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Abstract

The invention provides a nitrogen-hydrogen in-situ double-doped soft carbon / sodium vanadium phosphate composite material and a preparation method and application thereof. Bean or nut plant protein sources are prepared into slurry and then heated, a sodium source, a vanadium source and a phosphorus source are added for reaction and then pH is adjusted; and finally the nitrogen-hydrogen in-situ double-doped soft carbon / sodium vanadium phosphate composite material is prepared by hydrothermal reaction and calcination in the inert atmosphere. The beans or the nuts are used as the carbon source, thenitrogen and hydrogen source, the adsorbent, the complexing agent, the coagulant and the reaction carrier, the mesoporous material composed of nitrogen-hydrogen in-situ double-doped skeleton soft carbon and sodium vanadium phosphate with good electrochemical performance is prepared by adsorption, complexation, condensation of inorganic ions and ion groups, cracking reduction and N, H in-situ doping reactions by utilizing the composition, structure and performance characteristics of protein (amino acid). The carbon source used in the method has low cost and no toxicity and no pollution, and the synthesized composite material has excellent electrochemical properties such as specific capacity, rate performance and cycle performance.

Description

technical field [0001] The invention relates to a nitrogen-hydrogen in-situ double-doped soft carbon / sodium vanadium phosphate composite material and a preparation method and application thereof, belonging to the technical field of anode materials for sodium-ion batteries. Background technique [0002] Sodium-ion batteries have attracted attention due to the low cost and abundant source of sodium. Among the cathode materials for sodium ion batteries, sodium vanadium phosphate is considered to be one of the most potential cathode materials due to its low cost, open 3D framework NASICON structure and large gap channels that can accelerate the migration speed of sodium ions. However, sodium vanadium phosphate has limited its development and application due to its poor electrical conductivity and electrochemical performance. Carbon doping of sodium vanadium phosphate has been proved to be a method that can effectively improve its conductivity and electrochemical performance. At...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M10/054
CPCH01M4/362H01M4/5825H01M4/625H01M10/054Y02E60/10
Inventor 何文张合钰张旭东
Owner 江苏富爱科技发展有限公司
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