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Graphene-loaded rhombohedron ferric oxide composite material and hydrothermal synthesis method thereof

A composite material, hydrothermal synthesis technology, applied in electrical components, battery electrodes, circuits, etc., can solve the problems of high rate and long-cycle cycle performance, single structure of iron oxide particles, complex preparation process, etc., to achieve the preparation cycle Short, simple preparation process, high efficiency

Active Publication Date: 2013-05-01
SHANGHAI UNIV
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  • Claims
  • Application Information

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Problems solved by technology

Although the reported graphene and iron oxide composite materials have improved low-rate charge-discharge performance, their high-rate and long-cycle performance is not good.
In addition, the structure of iron oxide particles in composite materials is relatively simple, and they are often particles or spheres, which do not involve microscopic material design and synthesis.
Moreover, most of the preparation process is complicated, the cost is high, and it is difficult to prepare in large quantities.

Method used

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  • Graphene-loaded rhombohedron ferric oxide composite material and hydrothermal synthesis method thereof
  • Graphene-loaded rhombohedron ferric oxide composite material and hydrothermal synthesis method thereof
  • Graphene-loaded rhombohedron ferric oxide composite material and hydrothermal synthesis method thereof

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Embodiment 1

[0031] Embodiment one : Preparation of graphene-supported rhombohedral iron oxide composites using ferric sulfate as iron source.

[0032] Potassium persulfate (K 2 S 2 o 8 ) 2.5 g, phosphorus pentoxide (P 2 o 5 ) 2.5 g, dissolved in 12 mL of concentrated sulfuric acid, heated to 80°C; then 3 g of natural graphite was added to the above solution, kept at 80°C for 4.5 hours; cooled to room temperature, diluted with 500 mL of deionized water, and left standing overnight ; filter, float residual acid with 0.2 mm filter; dry in a vacuum oven at 60°C; add the obtained preoxide to 120 mL of ice-bathed concentrated sulfuric acid, slowly add 15 g of KMnO under stirring 4 , Keep the temperature below 20°C during the addition process. Then the temperature was controlled at 35°C and stirred for 2 h. Add 250 mL of deionized water to dilute, and keep the temperature below 50°C in an ice bath during the dilution process. Stir for another 2 h, add 0.7 L of deionized water, and immed...

Embodiment 2

[0036] Embodiment two : Preparation of graphene-supported rhombohedral iron oxide composites using ferric nitrate as iron source.

[0037] Add 0.808g of ferric nitrate into 100 mL of deionized water, add 100 mg of graphene into it, stir for 15 min, sonicate for 0.5 h, then add 0.50 g of NaAc and stir for 30 min, then transfer to the reaction kettle and heat at 160°C for 24 hours, centrifuge, ethanol washing and water washing 3 times each, and drying at 80°C to obtain the product.

[0038] The scanning electron microscope photo of the dried product is shown in figure 2 , it can be seen from the figure that the rhombohedral iron oxide has a diameter of 50-100 nm, and each surface is a parallelogram deformation. The reversible capacity is 1037.2 mAh / g at a current density of 100 mA / g in the voltage window of 5mV-3.0 V, and it can still maintain 677.2 mAh / g after 50 charge-discharge cycles.

Embodiment 3

[0039] Embodiment Three : Preparation of graphene-loaded rhombohedral iron oxide composites using iron acetate as iron source.

[0040] Take 0.246 g of ferric acetate and add it to 50 mL of deionized water, add 50 mg of graphene to it, stir for 15 min, sonicate for 0.5 h, then add 0.5 g of NaAc and stir for 30 min, then transfer to the reaction kettle and heat at 180°C for 24 hours, centrifuge, ethanol washing and water washing 3 times each, and drying at 80°C to obtain the product.

[0041] The scanning electron microscope photograph of the product is shown in image 3 , it can be seen that rhombohedral iron oxide particles with a diameter of 80-150 nm are evenly loaded on the surface of graphene, and no obvious agglomeration and stacking phenomenon is seen. And some particles are covered by a layer of transparent tulle graphene, indicating that the rhombohedral iron oxide particles are distributed on both sides of the graphene. Electrochemical tests show that the prepare...

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Abstract

The invention relates to a graphene-loaded rhombohedron ferric oxide composite material and a hydrothermal synthesis method thereof. The composite material is characterized in that a single layer of graphene is used as a matrix skeleton, and rhombohedron ferric oxide uniformly grows on two surfaces of the graphene piece layer; and the particle sizes of the rhombohedron ferric oxide are 50-150 nm, and each surface is a regular parallelogram. The rhombohedron ferric oxide can realize a good electrical conductivity through the graphene piece layer, and therefore the apparent electrical conductivity of the composite material is increased. The material is prepared through two typical steps: 1, preparing pyrolytic graphene; and 2, hydrothermally synthesizing the graphene-loaded rhombohedron ferric oxide composite material. Thegraphene-loaded rhombohedron ferric oxide composite material prepared by the method has a simple process, high reversible capacity and good cycle performance and is a lithium-ion battery anode material with a research value.

Description

technical field [0001] The invention relates to a three-dimensional graphene composite material used as a lithium battery negative electrode material, in particular to a graphene-loaded rhombohedral iron oxide composite material and a hydrothermal synthesis method thereof, belonging to the fields of electrochemistry and material synthesis. Background technique [0002] Since Japan's Sony Corporation announced in 1990 that it had successfully developed a LiCoO 2 / C rocking chair lithium-ion battery started, setting off an upsurge of research and industrialization of lithium-ion battery in the world. The development of lithium-ion batteries, as a new type of green high-energy power supply, can meet the needs of the rapid development of the modern electronics industry due to its excellent comprehensive performance, so its prospects are very broad. At present, lithium-ion battery technology is constantly improving and perfecting, its application fields are also expanding, and i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/52H01M4/62
CPCY02E60/12Y02E60/10
Inventor 赵兵蒋永蔡新辉马启亮凌学韬刘瑞喆焦正陈丹丹
Owner SHANGHAI UNIV
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