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Lithium iron phosphate nanorod/graphene composite material as well as preparation method and application thereof

A composite material, lithium iron phosphate technology, applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc. The problem of uneven dispersion of graphene, etc., can achieve the effect of ensuring that the capacity does not decay, increasing the transmission rate, improving the rate performance and cycle performance.

Inactive Publication Date: 2019-06-18
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the preparation process, the molar ratio of raw materials in the solvothermal reaction and the reaction temperature need to be strictly controlled, and a large amount of ethylene glycol is required as a solvent in the reaction process, which not only increases the cost of raw materials, but also causes a lot of waste of raw materials, making it difficult to realize industrial production
[0004] The powder particles prepared by the traditional solid phase method have no agglomeration, good filling, low cost, large output, and simple preparation process, such as Li Qiru et al. (Li Qiru. Preparation and electrochemical performance of graphene-coated lithium iron phosphate cathode material[ D]. Soochow University, 2016.) In the preparation and electrochemical performance of graphene-coated lithium iron phosphate cathode materials, a simple solid-phase method was used, using ferrous oxalate, ammonium dihydrogen phosphate, and lithium carbonate as raw materials. The organic carbon source glucose and graphene oxide were used as composite carbon sources, and LiFePO was successfully synthesized 4 / graphene / C composite material, and proved that the double-coated lithium iron phosphate material has a higher discharge specific capacity than the sample only coated with graphene, but the obtained LiFePO 4 / Graphene composite materials are all granular, which will affect the transmission rate of ions, and the capacity will easily decay during high-current discharge; at the same time, there are problems such as uneven dispersion and easy agglomeration of graphene, which leads to the conductivity and rate performance of the composite material. and cycle performance may be affected. At the same time, the preparation process has the disadvantages of high energy consumption, low efficiency, powder is not fine enough, and impurities are easily mixed

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  • Lithium iron phosphate nanorod/graphene composite material as well as preparation method and application thereof
  • Lithium iron phosphate nanorod/graphene composite material as well as preparation method and application thereof
  • Lithium iron phosphate nanorod/graphene composite material as well as preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0040] Example 1 Preparation of lithium iron phosphate nanorods / graphene composites

[0041] 1. Method

[0042] 1. Preparation of ferrous oxalate / graphene oxide composites

[0043] First, 4 mmol of graphene oxide was dissolved in deionized water, and ultrasonically dispersed for 2 h to obtain a graphene oxide dispersion. Then, 10 mmol of ferrous sulfate heptahydrate was added to the above graphene oxide dispersion and stirred for 12 h to obtain a mixed solution. , slowly pour 10.5 mmol oxalic acid solution into the mixture, continue stirring for 1.5 h, and then heat it in a drying box at 90 °C for 7 h to make it react completely to obtain a solid precipitate; The ferrous oxalate / graphene oxide composite material is obtained by grinding after drying.

[0044] 2. Preparation of LiFePO4 nanorods / graphene composites

[0045] Grind and mix 10 mmol of the above ferrous oxalate / graphene oxide with 10.5 mmol of lithium acetate dihydrate for 15 min until fully mixed, and then add 10...

Embodiment 2

[0048] Example 2 Preparation of lithium iron phosphate nanorods / graphene composites

[0049] 1. Method

[0050] Preparation of ferrous oxalate / graphene oxide composite material: First, 10 mmol of graphene oxide was dissolved in deionized water, and ultrasonically dispersed for 2 h to obtain a graphene oxide dispersion, and then 8 mmol of graphene oxide was added to the above graphene oxide dispersion. Hydrate ferrous sulfate, stir for 10 h to obtain a mixed solution, slowly pour 8.5 mmol of oxalic acid solution into the mixed solution, continue stirring for 2 h, heat at 80 °C for 8 h in a drying box to complete the reaction, and obtain a solid precipitate; The above-mentioned solid precipitate is suction-filtered and washed three times, and after vacuum drying, it is ground to obtain a ferrous oxalate / graphene oxide composite material.

[0051] Preparation of lithium iron phosphate nanorods / graphene composites: 8 mmol of the above ferrous oxalate / graphene oxide was thoroughly...

Embodiment 3

[0052] Example 3 Preparation of lithium iron phosphate nanorods / graphene composites

[0053] 1. Method

[0054] Preparation of ferrous oxalate / graphene oxide composite material: First, 15 mmol of graphene oxide was dissolved in deionized water, and ultrasonically dispersed for 2 h to obtain a graphene oxide dispersion, and then 12 mmol of graphene oxide was added to the above graphene oxide dispersion. Hydrate ferrous sulfate, stir for 14 h to obtain a mixed solution, slowly pour 12.5 mmol of oxalic acid solution into the mixed solution, continue stirring for 1 h, and then heat it in a drying box at 100 °C for 6 h to complete the reaction to obtain a solid precipitate The above-mentioned solid precipitate is filtered and washed three times, and after vacuum drying, it is ground to obtain ferrous oxalate / graphene oxide composite material.

[0055] Preparation of lithium iron phosphate nanorods / graphene composites: 12 mmol of the above ferrous oxalate / graphene oxide was thoroug...

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Abstract

The invention discloses a lithium iron phosphate nanorod / graphene composite material as well as a preparation method and an application thereof; the preparation method comprises the following steps offirstly, providing ferrous oxalate / graphene oxide composite material and then carrying out mixing on the ferrous oxalate / graphene oxide composite material and ammonium dihydrogen phosphate and lithium acetate dihydrate according to a certain molar ratio, and carrying out grinding and drying, and next, carrying out high-temperature reaction under the protection of inert gas to obtain the compositematerial. The lithium iron phosphate nanorod / graphene composite material prepared by adopting a two-step solid phase reaction method is small in particle size and uniform in particle size distribution, and has a one-dimensional nanorod-shaped structure, so that the transmission rate of ions can be effectively increased, and the capacity in large-current discharge is not attenuated; graphene is added, so that the surface conductivity of the material is further improved, and meanwhile, the rate performance and the cycling performance of the material are remarkably improved; and in the preparation process of the lithium iron phosphate nanorod / graphene composite material, the reaction conditions are easy to control, the operation is simple, the production cost is low, and industrial production is easy to realize.

Description

technical field [0001] The invention belongs to the technical field of positive electrode materials for lithium ion batteries. Specifically, it relates to a lithium iron phosphate nanorod / graphene composite material and its preparation method and application. Background technique [0002] Lithium iron phosphate with olivine structure is regarded as one of the most promising cathode materials for power batteries. It has many advantages such as abundant raw material sources, safety and environmental protection, and stable cycle performance. However, due to its structural limitations, the electronic and ionic conductivity is low. , resulting in a lower actual capacity. The composite of graphene and lithium iron phosphate can significantly improve its electrochemical performance. [0003] At present, the method for preparing lithium iron phosphate / graphene oxide composite cathode material is mainly the liquid phase method, because the liquid phase method can control the partic...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M10/0525B82Y30/00B82Y40/00
CPCY02E60/10
Inventor 孙志鹏程文华邵涟漪史晓艳方路峻吴方丹余锦超
Owner GUANGDONG UNIV OF TECH
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