Preparation method of stannic oxide or metallic tin and grapheme lamella composite material

A technology of graphene sheets and composite materials, which is applied in the direction of electrical components, battery electrodes, circuits, etc., can solve the problems of metal tin particle coating structure, difficult to control product morphology, and low charge and discharge performance of composite materials, and achieve enhanced Conductivity and fast charge-discharge performance, improve structural stability and electrochemical performance, and improve the effect of charge-discharge cycle stability

Active Publication Date: 2011-11-23
陕西埃普诺新能源科技有限公司
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Problems solved by technology

CN1812167A discloses a preparation method of a lithium ion battery negative electrode material composited with tin dioxide and graphite material, but due to the small specific surface area of ​​graphite, the negative electrode material cannot be fully contacted with the electrolyte, which affects the rapid charge and discharge performance of the electrode material
CN101478043A discloses a kind of graphene nano sheet loaded tin dioxide as the preparation method of lithium-ion battery negative electrode material, reversible specific capacity remains on more than 600mAh / g when charging and discharging with the electric current of 300mA / g, and GuoxiuWang etc. (J.Mater. Chem., 2009, 19, 8378-8384) using NaHB 4 The Sn / Graphene composites prepared by reducing agents used as lithium-ion battery electrode materials also have high reversible capacity, but these methods use strong reducing agents such as hydrazine hydrate, NaHB 4 etc. Such strong reducing agents will affect the formation process of tin dioxide particles and the recombination with graphene sheets, thereby affecting the electrochemical performance of electrode materials
However, most of these methods are simply mechanically mixing metal tin particles and carbon precursor substances. The obtained sample material is only filled with metal tin particles in the porous skeleton formed by the carbon matrix, and it is difficult to control the shape of the product during the pyrolysis process. appearance
CN101202340A discloses a kind of preparation method of tin-carbon nanocomposite material for negative electrode of lithium ion battery, but this method adopts starch as carbon source, and the amorphous carbon after high-temperature carbonization can not form good coating structure to metal tin particle, causes negative electrode material Low capacity, poor cycle performance
Recent studies (Nano Letters, 2008, 8, (8), 2277-2282) show that graphene sheets (Graphene Nanosheets, GNS) have high reversible capacity as lithium-ion battery electrode materials; graphene sheets can also be combined with other Metal oxides such as SnO 2 (Nano Letters, 2009, 9, (1), 72-75) or TiO 2 (ACS Nano, 2009, 3, (4), 907-914) composite as the negative electrode material, but due to the weak bonding force between the graphene sheet and tin dioxide, the charge and discharge performance of the composite material is not high

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  • Preparation method of stannic oxide or metallic tin and grapheme lamella composite material
  • Preparation method of stannic oxide or metallic tin and grapheme lamella composite material

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[0030] The invention provides a preparation method of a composite material of tin dioxide and graphene sheet. The method comprises: after mixing organic solvent, graphene oxide sheet hydrosol and tin salt, heating at 60-200°C for 0.5- After 12 hours, a solid substance was obtained; the obtained solid substance was heated at a temperature of 400-700° C. for 0.5-10 hours under the protection of an inert gas. Preferably, after mixing the organic solvent, graphene oxide lamellar hydrosol and tin salt, heat at 120-150°C for 0.5-3h to obtain a solid substance; ℃ temperature heating 0.5-2h.

[0031] According to the preparation method of a tin dioxide and graphene sheet composite material provided by the present invention, the volume ratio of the graphene oxide sheet hydrosol to the organic solvent is 1: 10-50, and the pH of the reaction is 2-6 ; The content of graphene oxide sheet in the graphene oxide sheet hydrosol is 5-20% by weight, and the content of water is 80-95% by weight,...

Embodiment 1

[0042] This embodiment is used to illustrate the preparation method of the tin dioxide and graphene sheet composite material provided by the present invention.

[0043] (1) Preparation of graphene oxide: adding 5.0 g of natural flaky graphite (particle size is 10-100 μm), 4.0 g of sodium nitrate and 20.0 g of permanganate in the concentrated sulfuric acid of 98% by weight to the concentration of 300 g Potassium, the resulting mixture was stirred under 0°C ice bath conditions (that is, the temperature of the mixture was 0°C by means of an ice bath) was stirred for 2h, and then stirred at 30°C for 5h; then 600ml of water was added to the resulting mixture for dilution, Heat up to 90° C. and stir for 0.5 h; add 10 ml of hydrogen peroxide with a concentration of 30% by weight, stir for 30 min and then filter, then centrifuge and wash the obtained filter cake 5 times with hydrochloric acid with a concentration of 3% by weight at a speed of 5000 r / min , and then use deionized water ...

Embodiment 2

[0051] This embodiment is used to illustrate the preparation method of the tin dioxide and graphene sheet composite material provided by the present invention.

[0052] (1) Preparation of graphene oxide: adding 5.0 g of natural flake graphite (10-100 μm in particle size), 5.0 g of sodium nitrate and 25.0 g of permanganate in the concentrated sulfuric acid of 98% by weight to the concentration of 1500 g Potassium, the resulting mixture was stirred at 0°C in an ice bath (that is, the temperature of the mixture was 0°C through an ice bath) for 5 h, and then stirred at 30°C (30°C) for 10 h; then 500 ml of Diluted with water, then heated up to 70°C and stirred for 2h; then added 6ml of hydrogen peroxide with a concentration of 30% by weight, stirred for 60min and filtered, and then the obtained filter cake was treated with hydrochloric acid with a concentration of 10% by weight at 5000r / min Centrifugal washing 5 times at a rotating speed of 5000r / min, followed by centrifugal washin...

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Abstract

The invention provides a preparation method of a stannic oxide and grapheme lamella composite material. The preparation method comprises the following steps of mixing at least one organic solvents, graphene oxide lamella hydrosol and at least one tin salt, heating the mixture at a temperature of 60 to 200 DEG C for 0.5 to 12 hours to obtain a solid substance, and heating the solid substance in the inert gas atmosphere at a temperature of 400 to 700 DEG C for 0.5 to 10 hours. The invention also provides a preparation method of a metallic tin and grapheme lamella composite material. The preparation method comprises the following step of preparing a stannic oxide and grapheme lamella composite material through the preparation method of a stannic oxide and grapheme lamella composite material, and heating the prepared stannic oxide and grapheme lamella composite material in the reducing gas atmosphere at a temperature of 400 to 1000 DEG C for 0.5 to 4 hours. The preparation methods of the invention can improve a structural stability and an electrochemical performance of a material and is beneficial to improve a high-speed charging and discharging performance and a conductivity of a composite material. The preparation methods have the characteristics of cheap and easily available raw materials, simple process, and good applicability for industrial continuous production.

Description

technical field [0001] The invention relates to a preparation method of a composite material of tin dioxide or metal tin and graphene sheets. Background technique [0002] Metal tin and tin dioxide are very potential negative electrode materials for lithium-ion batteries. The theoretical capacities of the two have reached 990mAh / g and 781mAh / g respectively. However, metal tin and tin dioxide will generate The large volume change (J. Electrochem. Soc., 1997, 144: 2045) results in poor cycle performance and low service life of the battery. At present, one of the main ways to solve this problem is to optimize the structure and composition of electrode materials by introducing active or inactive substances. When nano-active substances are uniformly dispersed in a certain conductive matrix material, the matrix material or alloy structure can be effective. It prevents the agglomeration of active materials, and at the same time acts as a buffer layer for the volume change during c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/139H01M4/36
CPCY02E60/122Y02E60/12Y02E60/10
Inventor 智林杰罗彬
Owner 陕西埃普诺新能源科技有限公司
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