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Preparation method of hydro-thermal coupling spray pyrolysis MnO2/graphene electrode material

A graphene electrode and spray pyrolysis technology, applied in the field of nano-electrode materials for energy storage systems, can solve problems such as volume expansion of transition metal oxide materials, difficult industrialization of sol-gel methods, and uneven mixing of high-temperature solid-phase methods. Achieve good electrochemical performance, good practical value and market prospects, and high product quality consistency

Inactive Publication Date: 2014-07-09
SHANDONG RUNSHENG POWER TECH +1
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Problems solved by technology

[0005] In 2000, P. Poizot et al. published an article in the journal Nuture. They first studied nano-transition metal oxides as anode materials for lithium-ion batteries and found that transition metal oxides The initial discharge capacity of the material is high, but the capacity drops rapidly after repeated charge and discharge, the main reason is that the volume expansion and contraction of the transition metal oxide material during the charge and discharge process is large, resulting in the destruction of the electrode structure and poor cycle performance
Subsequently, related patents and literature reported some methods to improve the conductivity and circulation of transition metal oxides. These methods have their own advantages and disadvantages: the high-temperature solid-phase method is unevenly mixed, and the particle size of the synthesized products is mostly micron-scale, and the distribution is wide. , the sintered particles are seriously agglomerated, often contain impurities, and have irregular shapes. The electrochemical properties of different batches of materials vary greatly, and the energy consumption is large; the sol-gel method is not easy to industrialize; the electrodeposition method is not easy to control and difficult to scale The hydrothermal method is a commonly used process for the preparation of nanomaterials; the spray pyrolysis process is relatively mature, which can quickly dry nanomaterials, prevent material agglomeration and growth, and is easy to scale

Method used

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  • Preparation method of hydro-thermal coupling spray pyrolysis MnO2/graphene electrode material

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Embodiment 1

[0032] Preparation of Nano-MnO as Lithium Battery Electrode Material 2 / graphene composite, proceed as follows:

[0033] (1) With graphite, potassium permanganate, H 2 SO 4 / H 3 PO 4 (volume ratio 9:1) and H 2 o 2 As a raw material, graphite oxide (GO) was prepared by the improved Hummers method, and the obtained GO had a multilayer 5×5 μm flake structure;

[0034] (2) Take 0.005g of GO prepared in step (1), add 20mL of deionized water, and sonicate for 0.5hr at 200w power to obtain a uniform GO deionized water dispersion;

[0035] (3) Using potassium permanganate and manganese acetate as raw materials, weigh 0.3g potassium permanganate and 0.7g manganese acetate, add 30mL deionized water, add 20mL GO deionized water dispersion prepared in step (2), 20mL 0.001M Ni(NO 3 ) 2 Solution, 0.1g sodium lauryl sulfate, ultrasonic 0.5hr, form a uniform mixed solution, put it into a hydrothermal kettle, control the reaction temperature to 250°C, and continue the reaction time fo...

Embodiment 2

[0042] Preparation of Nano-MnO as Lithium Battery Electrode Material 2 / graphene composite, proceed as follows:

[0043] (1) With graphite, potassium permanganate, H 2 SO 4 / H 3 PO 4 (volume ratio 9:1) and H 2 o 2 As a raw material, graphite oxide (GO) was prepared by the improved Hummers method, and the obtained GO had a multilayer 5×5 μm sheet structure;

[0044] (2) Take 0.05g of GO prepared in step (1), add 20mL of ethanol, and sonicate at 200w power for 1hr to obtain a uniform GO dispersion;

[0045] (3) Using potassium permanganate and manganese acetate as raw materials, weigh 1.6g of potassium permanganate and 3.7g of manganese acetate, add 30mL of deionized water, 0.3g of sodium lauryl sulfate, and add 20mL of step (2) to prepare GO dispersion, 20mL 0.025M Ni(NO 3 ) 2 The solution was ultrasonicated for 1 hr to form a uniform mixed solution, placed in a hydrothermal kettle, the reaction temperature was controlled at 160°C, and the reaction time was continued f...

Embodiment 3

[0052] Preparation of Nano-MnO as Lithium Battery Electrode Material 2 / graphene composite, proceed as follows:

[0053] (1) With graphite, potassium permanganate, H 2 SO 4 / H 3 PO 4 (volume ratio 9:1) and H 2 o 2 As a raw material, graphite oxide (GO) was prepared by the improved Hummers method, and the obtained GO had a multilayer 5×5 μm flake structure;

[0054] (2) Take 0.2g of GO prepared in step (1), add 20mL of deionized water, and ultrasonicate for 2 hours at 200w power to obtain a uniform dispersion of GO in deionized water;

[0055] (3) Using potassium permanganate and manganese acetate as raw materials, weigh 3.2g of potassium permanganate and 7.5g of manganese acetate, add 30mL of deionized water, 0.5g of polyvinyl alcohol, and add 20mL of GO prepared in step (2). Ionic water dispersion, 20mL 0.08mol / L Ni(NO 3 ) 2 solution, sonicated for 2 hours to form a uniform mixed solution, put it into a hydrothermal kettle, control the reaction temperature to 180°C, ...

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Abstract

The invention discloses a preparation method of a hydro-thermal coupling spray pyrolysis MnO2 / graphene electrode material, belonging to the technical field of electrode materials for energy storage systems. The preparation method comprises the following steps: uniformly mixing graphene oxide (GO) prepared by using a Hummer method with an aqueous solution of bivalent manganese salt and a doped metal ion compound, adding a dispersing agent, an oxidant and a surfactant, and ultrasonically dispersing for a certain period of time; putting the mixed solution into a hydrothermal kettle, adjusting the temperature, and keeping for a certain period of time; filtering and washing a reaction product to obtain a precursor; adding the dispersing agent and the surfactant into the precursor, uniformly stirring for mixing, and adjusting the solid-liquid ratio, inlet temperature and outlet temperature to perform spray pyrolysis in order to obtain a metal ion-doped MnO2 / graphene nanometer composite electrode material. According to the nanometer composite electrode material prepared by using the method, components are uniform and the batch stability is high.

Description

technical field [0001] The invention belongs to the technical field of nano electrode materials for energy storage systems, in particular to a hydrothermal coupling spray pyrolysis of MnO 2 The preparation method of / graphene electrode material. Background technique [0002] Energy and environmental issues are two major problems facing mankind at present, forcing people to constantly search for cleaner new energy sources. Solar energy, wind energy, nuclear energy, ocean energy, etc. are clean energies that exist in large quantities on the earth, but the use of these energies is limited by certain conditions, and they must be efficiently utilized through special energy storage devices. Only by solving the problems of energy storage and efficient energy conversion can the efficient use of new energy be truly realized. Therefore, the development of key materials for lithium-ion batteries, lithium secondary batteries and supercapacitors with excellent comprehensive performance ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/50H01M4/62H01G11/46B82Y30/00
CPCB82Y40/00H01G11/30H01M4/362H01M4/505H01M4/625H01M10/052Y02E60/10
Inventor 蒲薇华王珊珊李青海陈敏叶霞唐廎
Owner SHANDONG RUNSHENG POWER TECH
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