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Preparation method of lithium iron phosphate/graphene nano composite material

A nanocomposite material, lithium iron phosphate technology, applied in the direction of structural parts, electrical components, battery electrodes, etc., can solve the problem of low bonding force between graphene and grain interface, inability to control the grain size of lithium iron phosphate, and limit composite materials Electronic conductivity and other issues, to achieve the effect of simple and controllable preparation method, low price, and simple and controllable process

Inactive Publication Date: 2012-10-24
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Journal of Materials Chemistry (2010) 10.1039 / c0jm01633k disclosed that the mechanical mixing method was used to compound the pre-prepared lithium iron phosphate and graphene. This simple physical mixing cannot control the grain size of lithium iron phosphate. The interfacial bonding force of the composite material is poor, and graphene is difficult to achieve uniform dispersion in the composite material, but it is easy to form agglomeration in the composite material, which greatly limits the improvement of the electronic conductivity of the composite material.
CN102185139A discloses a preparation method of nano-metal oxide / graphene-doped lithium iron phosphate electrode material, which solves the problem of easy agglomeration of graphene in the process of doping with lithium iron phosphate by modifying graphene with nano-metal oxide
However, this method also adopts the method of mechanical ball mixing. Although it improves the dispersion of graphene to a certain extent compared with the traditional mechanical mixing method, the interfacial bonding force between the obtained material graphene and the crystal grains is still not high.

Method used

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  • Preparation method of lithium iron phosphate/graphene nano composite material
  • Preparation method of lithium iron phosphate/graphene nano composite material
  • Preparation method of lithium iron phosphate/graphene nano composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] 1) Add 0.27 g ferric chloride and 1.8 g urea to 100 mL and 1 g / L graphene oxide sol, respectively, and stir well;

[0053] 2) Transfer the mixed solution in step 1) to a heating container such as an oil bath at 95 °C for 1.5 hours;

[0054] 3) After the reaction is complete, add 1.0 mL of hydrazine hydrate to the above solution and microwave for 2 minutes, filter and wash with suction to obtain Fe 2 o 3 / GS complex;

[0055] 4) Re-disperse the precursor ultrasonically into a mixed solution of 150 mL DMF and water (50:1), add lithium hydroxide, phosphoric acid and 0.44 g ascorbic acid in an equimolar amount to the iron element, and stir well;

[0056] 5) Transfer the above mixture to a polytetrafluoroethylene-lined stainless steel reactor. Put it in an oven, and heat the solvent at 180°C for 12 hours;

[0057] 6) After the reaction is completed, let it cool down naturally, open the container, wash the collected samples with water and ethanol respectively, and then dr...

Embodiment 2

[0060] 1) Add 5.0 g of ferric chloride and 0.05 g of urea to 100 mL and 0.5 g / L graphene oxide sol, respectively, and stir well

[0061] 2) Transfer the mixed solution in step 1) to a heating container such as an oil bath at 80 °C for 6 hours

[0062] 3) After the reaction is completed, add 0.1 mL of hydrazine hydrate to the above solution and microwave for 4 minutes, filter and wash with suction to obtain Fe 2 o 3 / GS complex

[0063] 4) Fe 2 o 3 / GS complex was re-dispersed ultrasonically into a mixed solution of 296 mL DMF and water (1:1), adding lithium hydroxide, phosphoric acid and 0.30 g ascorbic acid in an equimolar amount to iron, and stirring well

[0064] 5) Transfer the above mixed solution to a polytetrafluoroethylene-lined stainless steel reaction kettle, place it in an oven, and heat the solvent at 180°C for 36 hours;

[0065] 6) After the reaction is completed, let it cool down naturally, open the container, wash the collected samples with water and ethano...

Embodiment 3

[0068] 1) Add 0.4 g of ferric chloride and 40 g of urea to 100 mL and 4 g / L graphene oxide sol, respectively, and stir well;

[0069] 2) Transfer the mixed solution in step 1) to a heating container such as an oil bath at 180°C for 0.5 hours;

[0070] 3) After the reaction was completed, 5 mL of hydrazine hydrate was added to the above solution and microwaved for 2 minutes, suction filtered and washed to obtain Fe 2 o 3 / GS complex;

[0071] 4) Fe 2 o 3 The / GS complex was re-dispersed ultrasonically into a mixed solution of 236.8 mL DMF and water (100:1), adding lithium hydroxide, phosphoric acid and 4.74 g ascorbic acid in an equimolar amount to the iron element, and fully stirred evenly;

[0072] 5) Transfer the above mixed solution to a polytetrafluoroethylene-lined stainless steel reaction kettle, place it in an oven, and heat the solvent at 200 ° C for 8 hours;

[0073]6) After the reaction is completed, let it cool down naturally, open the container, wash the colle...

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Abstract

The invention relates to a preparation method of lithium iron phosphate / graphene nano composite material. The preparation method comprises the steps of dispersing iron trioxide / graphene composite into a solvent, and adding ascorbic acid, lithium hydrate and phosphoric acid to obtain a precursor dispersing agent; and arranging the precursor dispersing agent into a reactor, and conducting solvent thermal reaction for 1-48h at 90-350 DEG C.

Description

technical field [0001] The invention belongs to the field of preparation of inorganic materials, in particular to the field of lithium ion battery cathode materials, in particular to a lithium iron phosphate / graphene nanocomposite material and a preparation method thereof. Background technique [0002] The continuous development and utilization of new energy is the basis for the sustainable development of human society. At present, for most new energy sources (wind energy, solar energy, tidal energy, etc.), their discontinuity makes it necessary to use large-capacity energy storage devices to store these intermittent energies, and then provide them evenly and continuously. use. Therefore, higher requirements are placed on the energy density of large-scale energy storage devices. Compared with other energy storage devices, lithium-ion batteries have the advantages of high energy density, low self-discharge rate, wide operating temperature range, long cycle life, no memory e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M4/583
CPCY02E60/12Y02E60/10
Inventor 孙静王荣华徐朝和高濂
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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