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Preparation method of iron trioxide/graphene composite material, negative electrode of lithium-ion battery and lithium-ion battery

A technology of ferric oxide and lithium-ion batteries, which is applied in the field of nanomaterials, can solve problems such as difficult large-scale synthesis, high energy consumption, and decreased conductivity of the negative electrode, and achieve low requirements for equipment, simple synthesis steps, and improved battery performance. Effect

Active Publication Date: 2016-11-16
云南宝利硅芯科技有限公司
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  • Abstract
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  • Application Information

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Problems solved by technology

Ferric oxide is a semiconductor material. On the one hand, its electronic conductivity is poor, and there is a serious voltage hysteresis phenomenon, resulting in low energy efficiency, and it will cause a large amount of heat to be generated during the continuous intercalation / extraction of lithium ions, resulting in Huge potential safety hazard; on the other hand, in the process of lithium intercalation / delithiation, the electrode material will be broken and powdered, which will easily cause the active particles of the electrode material to lose good electrical and mechanical contact, as well as the solid electrolyte phase interface film on the electrode surface. Crack, lose the protection of the electrode, greatly reduce the cycle life
Chinese invention patent CN103449427A discloses a method for synthesizing ferric oxide / porous graphene composite nanomaterials, which requires freeze-drying and high-temperature treatment, consumes a lot of energy, and has poor distribution uniformity of ferric oxide on porous graphene, making it difficult to large-scale synthesis
For example, in Li Xiao et al. (ACS Appl.Mater.Interfaces 2013,5,3764-3769) using a one-step hydrothermal method to prepare ferric oxide and graphene airgel composites, ferric oxide is condensed on graphene The surface and bulk phase distribution of the glue is uneven, which affects the performance of lithium-ion batteries
In summary, most graphene composite materials are currently a mixed state of graphene and ferric oxide, and ferric oxide is unevenly distributed on the surface and interior of graphene. It is easy to fall off on graphene, which reduces the conductivity of the negative electrode and ultimately affects the cycle stability of lithium-ion batteries

Method used

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  • Preparation method of iron trioxide/graphene composite material, negative electrode of lithium-ion battery and lithium-ion battery
  • Preparation method of iron trioxide/graphene composite material, negative electrode of lithium-ion battery and lithium-ion battery
  • Preparation method of iron trioxide/graphene composite material, negative electrode of lithium-ion battery and lithium-ion battery

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Experimental program
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Effect test

Embodiment 1

[0036] Preparation of graphite oxide: weigh 5.0g graphite and 3.75g NaNO respectively 3 Put it into a 1L beaker, stir vigorously, slowly add 150mL of concentrated sulfuric acid, stir for 0.5 hours, then slowly add 20g of KMnO 4 , Added in 0.5 hours, and continued to stir for 20 hours, the viscosity of the reactant increased, and the stirring was stopped to obtain a paste-like purple-red substance. After standing for 5 days, slowly add 500mL deionized water and 30mLH 2 o 2 At this time, the color of the solution becomes more obvious bright yellow. After the solution is fully reacted, it is centrifuged and washed to obtain graphite oxide.

[0037] Hydrothermal process: Dissolve 70mg graphite oxide in 80mL deionized water, add 6mL concentrated sulfuric acid (ρ=1.84g / cm 3 ), ultrasonically dispersed for 3 hours, the solution was moved into a small glass bottle, and then it was transferred to five hydrothermal reactors on average, reacted in a 200 ° C oven for 30 hours, washed, ...

Embodiment 2

[0041] The preparation method of graphite oxide is with embodiment 1.

[0042] Hydrothermal process: Dissolve 100mg of graphite oxide in 80mL of deionized water, add 8mL of concentrated sulfuric acid, ultrasonically disperse for 3 hours, transfer the solution into a small glass bottle, and then transfer it to 5 hydrothermal reaction kettles on average, React in an oven at 180°C for 20 hours, wash, and collect to obtain 20 mg of three-dimensional columnar reduced graphene oxide.

[0043] Composite process: Dissolve 1.8g of ferric chloride in 14mL of deionized water, add 4.0g of urea, add 20mg of three-dimensional columnar reduced graphene oxide to the above solution, soak in a water bath at 10°C for 3 days, then mix the solution with the three-dimensional The columnar reduced graphene oxide was transferred to a reaction kettle, reacted in an oven at 210°C for 34 hours, washed the product, dried in vacuum at 60°C for 4 hours, and collected the product.

[0044] Roasting process...

Embodiment 3

[0046] The preparation method of graphite oxide is with embodiment 1.

[0047] Hydrothermal process: Dissolve 120mg of graphite oxide in 80mL of deionized water, add 10mL of concentrated sulfuric acid, ultrasonically disperse for 3 hours, transfer the solution into a small glass bottle, and then transfer it to 5 hydrothermal reaction kettles on average. React in an oven for 18 hours, wash, and collect to obtain 24 mg of three-dimensional columnar reduced graphene oxide.

[0048] Composite process: Dissolve 2.0g ferrous sulfate in 14mL deionized water, add 2.5g urea, add 24mg three-dimensional columnar reduced graphene oxide to the above solution, soak in a water bath at 50°C for 3 days, then mix the solution and three-dimensional columnar The reduced graphene oxide was transferred to a reaction kettle, reacted in an oven at 210°C for 36 hours, washed the product, dried in vacuum at 60°C for 4 hours, and collected the product.

[0049] Roasting process: take the product and ro...

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Abstract

The invention discloses a preparation method of an iron trioxide / graphene composite material, a negative electrode of a lithium-ion battery and the lithium-ion battery. The preparation method comprises a hydrothermal procedure and a compound procedure. According to the preparation method, iron trioxide nanoparticles are uniformly loaded on the surface of three-dimensional graphene and in a pore structure; and the iron trioxide / graphene composite material is obtained through washing and drying. The material is applied to the lithium-ion battery and has excellent properties of high capacity, long cycle lifetime, low cost and the like; and mass production is easy to implement.

Description

technical field [0001] The invention relates to the technical field of nanomaterials, in particular to a preparation method of a ferric oxide / graphene composite material, a negative electrode of a lithium ion battery, and a lithium ion battery. Background technique [0002] As the most promising new type of energy storage device, lithium-ion battery has high energy density, high working voltage, long cycle life, low self-discharge rate, good cycle performance, no memory effect, safety and good thermal stability. And other advantages, has been widely used in various portable electronic equipment, electric vehicles and aerospace and other fields. At present, the anode materials of commercial lithium-ion batteries are mainly graphite-based carbon materials, which are stable and safe, but their low specific capacity limits the further improvement of lithium-ion battery performance. Non-carbon materials have high energy density, but their conductivity is not good, and electrons ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/13H01M10/0525H01M4/62
CPCH01M4/13H01M4/362H01M4/625H01M10/0525Y02E60/10
Inventor 谷翠萍崔艳威黄家锐高绿绿
Owner 云南宝利硅芯科技有限公司
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