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Nano iron phosphate hollow sphere/graphene composite material and preparation method thereof

A nano-iron phosphate and composite material technology, applied in electrical components, battery electrodes, circuits, etc., can solve the problems of poor electronic conductivity, limited electrochemical performance of LiFePO4, low diffusion rate, etc. The effect of large-scale industrial promotion and simple equipment

Inactive Publication Date: 2011-09-14
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But since LiFePO 4 Due to its own structural characteristics and the large particle size of the material prepared by the traditional high-temperature sintering method, the electronic conductivity inside the material is poor. + In LiFePO 4 The diffusion rate in the particles is very low, which greatly limits the LiFePO 4 electrochemical performance

Method used

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  • Nano iron phosphate hollow sphere/graphene composite material and preparation method thereof
  • Nano iron phosphate hollow sphere/graphene composite material and preparation method thereof
  • Nano iron phosphate hollow sphere/graphene composite material and preparation method thereof

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Embodiment 1

[0038] Graphene oxide was ultrasonically dispersed with deionized water for 30 min to obtain a 1 mg / ml suspension. In 20 mL of deionized water, add (NH 4 ) 2 Fe(SO 4 ) 2 ·6H 2 O and phosphoric acid, 0.5 ml of graphene suspension, and then add 1.2 g of urea (urea) as a precipitant and 0.1 g of sodium dodecyl sulfate (SDS) as a surfactant, in which the ferrous ammonium sulfate hexahydrate The amount is 0.1 mmol. The mixture was ultrasonically dispersed for 1-10 minutes. After uniform dispersion, pour it into a stainless steel reaction kettle lined with polytetrafluoroethylene, close the reaction kettle, place it in an oven, heat at 80-100°C for 3-12 hours, and cool to room temperature. The product was washed by centrifugation with ethanol and deionized water for 6-8 times respectively, and the product obtained by centrifugation was placed in a vacuum drying oven at 80-100°C for 10-24 h in a vacuum to obtain a nano-iron phosphate hollow sphere / graphene composite material. ...

Embodiment 2

[0040] Graphene oxide was ultrasonically dispersed with deionized water for 30 min to obtain a 1 mg / ml suspension. In 20 mL of deionized water, add (NH 4 ) 2 Fe(SO 4 ) 2 ·6H 2 O and phosphoric acid, 1 ml of graphene suspension, and then add 1.2 g of urea (urea) as a precipitant and 0.1 g of sodium dodecyl sulfate (SDS) as a surfactant, the amount of substance of ferrous ammonium sulfate hexahydrate 0.1 mmol. Place the mixture in an ultrasonic wave and ultrasonically disperse for 1-10 minutes. After the dispersion is uniform, pour it into a stainless steel reaction kettle lined with polytetrafluoroethylene, close the reaction kettle, and heat it in an oven at 100-120 ℃ for 3-12 hours. , cooled to room temperature. The product was centrifuged and washed 6-8 times with ethanol and deionized water respectively, and the product obtained by centrifugation was placed in a vacuum drying oven at 50-100 °C for 10-24 h in a vacuum to obtain a nano-iron phosphate hollow sphere / graph...

Embodiment 3

[0042] Graphene oxide was ultrasonically dispersed with deionized water for 30 min to obtain a 2 mg / ml suspension. In 20 mL of deionized water, add (NH 4 ) 2 Fe(SO 4 ) 2 ·6H 2 O and phosphoric acid, 0.5 ml of graphene dispersion, then add 0.6 g of urea (urea) as a precipitant and 0.05 g of sodium dodecyl sulfate (SDS) as a surfactant, the amount of ammonium ferrous sulfate hexahydrate is 0.05 mmol. Place the mixture in an ultrasonic wave for ultrasonic dispersion for 1-10 minutes. After the dispersion is uniform, pour it into a stainless steel reaction kettle lined with polytetrafluoroethylene, close the reaction kettle, and heat it in an oven at 60-100 °C for 3-12 hours. , cooled to room temperature. The product was centrifuged and washed 6-8 times with ethanol and deionized water respectively, and the product obtained by centrifugation was placed in a vacuum drying oven at 50-100 °C for 10-24 h in a vacuum to obtain a nano-iron phosphate hollow sphere / graphene composit...

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Abstract

The invention relates to a nano iron phosphate hollow sphere / graphene composite material with graphene as a carrier, and the nano iron phosphate of a hollow spherical structure with the particle size 50-100nm grows on the graphene. The preparation method of the composite material provided by the invention comprises the following steps: carrying out a hydro-thermal reaction on a mixed liquid containing oxidized graphene, hexahydrate ammonium ferrous sulfate and phosphoric acid at 60-120 DEG C by using urea as a precipitator and adding a surfactant (lauryl sodium sulfate); washing the products;and carrying out vacuum drying, obtaining the nano iron phosphate hollow sphere / graphene composite material. The nano iron phosphate hollow sphere / graphene composite material provided by the invention has the advantages of unique nano hollow structure, excellent electrical conductivity and discharge stability, small particle size, good dispersity and suitability for the anode material of a lithium ion secondary electrode; and the preparation method based on a low-temperature hydro-thermal method is simple and economic, thereby being suitable for realization of industrial large-scale production.

Description

technical field [0001] The invention relates to a nano-iron phosphate hollow sphere / graphene composite material and a low-temperature hydrothermal preparation method thereof. The composite material can be used as a positive electrode active material of a lithium-ion secondary battery, and belongs to the technical fields of material chemistry and energy battery. Background technique [0002] Lithium-ion batteries have been widely used in portable electronic products and communication tools in recent years because of their excellent environmental protection properties. They also have broad applications in the power plant applications of electric vehicles (EV) and hybrid electric vehicles (HEV) Therefore, improving the performance of lithium-ion batteries is a hot research topic at present. Among them, the selection of electrode materials is a key determinant of the performance of lithium-ion batteries. [0003] Since Goodenough et al first reported the LiFePO with olivine str...

Claims

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Application Information

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IPC IPC(8): H01M4/58H01M4/1397
CPCY02E60/122Y02E60/10
Inventor 印亚静蔡称心张卉吴萍
Owner NANJING NORMAL UNIVERSITY
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