Preparation method of graphene/lithium titanate composite anode material

A negative electrode material, graphene technology, applied in the field of preparation of graphene/lithium titanate composite negative electrode materials, can solve problems such as difficult to achieve large-scale industrial production, long diffusion distance, complex process, etc., and achieve easy realization of large-scale industrial production , good magnification, and high phase purity

Active Publication Date: 2013-04-03
ZHANGJIAGANG IND TECH RES INST CO LTD DALIAN INST OF CHEM PHYSICS CHINESE ACADEMY OF SCI +1
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  • Abstract
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Problems solved by technology

However, graphene as an electrode material needs to solve two problems: one is the relatively low specific capacity, because a lithium ion can only combine with six carbon atoms to form LiC between the structure of graphene and the relatively dense graphite layer. 6 Second, the special shape and size of graphene lead to a longer diffusion distance between lithium ions into graphene layers
[0007] At present, the composite method of lithium titanate and graphene mostly adopts the in-situ composite method using graphene as the raw material, but the preparation process from graphene oxide to graphene is complex and difficult to achieve large-scale industrial production.

Method used

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  • Preparation method of graphene/lithium titanate composite anode material
  • Preparation method of graphene/lithium titanate composite anode material
  • Preparation method of graphene/lithium titanate composite anode material

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Embodiment 1

[0046] Graphene oxide with a particle size of about 100 μm was added to ethanol, and ultrasonically dispersed for 2 hours to obtain a solution with a concentration of 1 g / L. Butyl titanate and lithium acetate were selected as the titanium source compound and lithium source compound, respectively. The aforementioned titanium source and lithium source compounds were dissolved in ethanol to prepare a solution with a concentration of 1 kg / L. According to the molar ratio of lithium to titanium N Li :N Ti =0.84:1, the mass percentage of graphene in the graphene / lithium titanate composite negative electrode material is 5wt.%, the ethanol solution of the prepared butyl titanate, lithium acetate solution and oxalic acid is successively added to the oxidation graphene in ethanol solution. The pH value of the above mixed solution was adjusted to 5.6 with ammonia water. Stir at 30°C for 3 hours, then raise the temperature to 60°C, and stir until gelatinous. The wet gel is converted i...

Embodiment 2

[0064] Graphene oxide with a particle size of about 100 μm was added to water and ultrasonically dispersed for 0.5 hour to obtain a 3 g / L graphene oxide aqueous solution. Tetraisopropyl titanate and lithium hydroxide were selected as the titanium source compound and the lithium source compound, respectively. Under stirring conditions, according to the molar ratio of lithium to titanium N Li :N Ti =0.80:1, successively add 1ml of 30% hydrogen peroxide and 1mmol of tetraisopropyl titanate to 20ml of 0.4M lithium hydroxide aqueous solution, and stir until completely dissolved. Finally, the above solution was mixed with the graphene oxide aqueous solution according to the mass ratio of graphene to lithium titanate of 7:93. The resulting mixed solution was poured into a 50ml stainless steel reaction kettle with polytetrafluoroethylene as a liner, sealed and placed in a blast drying oven, and reacted for 2 hours at 150°C. After naturally cooling to room temperature, the reaction ...

Embodiment 3

[0066] According to the mass percentage of graphene and lithium titanate being about 10wt%, graphite oxide with a particle size of about 150 μm was dissolved in secondary water to form a 1 g / L solution, and ultrasonically dispersed for 1 hour. Tetraisopropyl titanate and lithium hydroxide were selected as the titanium source compound and the lithium source compound, respectively. Under stirring conditions, according to the molar ratio of lithium to titanium N Li :N Ti =0.82:1, successively add 1ml of 30% hydrogen peroxide and 1mmol of tetraethyl titanate to 20.5ml of 0.4M lithium hydroxide aqueous solution, stir until completely dissolved. Finally, the above solution was mixed with the graphene oxide aqueous solution according to the mass ratio of graphene to lithium titanate of 10:90. The resulting mixed solution was poured into a 50ml stainless steel reactor with polytetrafluoroethylene as a liner, sealed and placed in a microwave oven at 180°C for 10 minutes to insulate t...

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Abstract

The invention discloses a preparation method of a graphene/lithium titanate composite anode material, which comprises the following steps: compounding compounds serving as a lithium source and a titanium source and graphene oxide through a liquid-phase method and reducing graphene oxide of the compound in inert gas mixed with reducing gas into graphene so as to obtain the graphene/lithium titanate composite anode material. The method has the characteristic of realizing uniform distribution of graphene in lithium titanate through an in-situ compounding technique. Under the same conditions, the discharge time of a hybrid capacitor which respectively takes the graphene/lithium titanate composite anode material and activated carbon as the anode and cathode is obviously greater than that of an electric double-layer capacitor which takes activated carbon as an electrode and that of a hybrid capacitor which respectively takes lithium titanate and activated carbon as the anode and cathode. The lithium titanate phase purity of a hybrid supercapacitor and lithium ion battery composite anode materials prepared by the method disclosed by the invention is higher. Furthermore, the preparation method further has the characteristic of easily realizing the large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of hybrid supercapacitors and lithium battery electrodes, and in particular relates to a preparation method of a graphene / lithium titanate composite negative electrode material. Background technique [0002] With the aggravation of environmental pollution, climate warming and the gradual depletion of fossil energy such as petroleum, the efficient use of renewable energy such as wind energy and solar energy has attracted widespread attention. In the field of new energy, the development and application of low-cost, environmentally friendly electrochemical energy storage devices have become a top priority. In this research field, the development and application of lithium-ion batteries and supercapacitors are in a leading position. Lithium-ion batteries and supercapacitors have played an important role in our daily life, such as providing power for portable electronic devices (mobile phones, laptops, etc.), fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/485H01M4/583H01G11/86
CPCY02E60/10
Inventor 阎景旺薛荣郝立星衣宝廉
Owner ZHANGJIAGANG IND TECH RES INST CO LTD DALIAN INST OF CHEM PHYSICS CHINESE ACADEMY OF SCI
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