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A kind of preparation method of nano ceria/graphene/sulfur composite material

A technology of nano-cerium oxide and composite materials, which is applied in the field of preparation of nano-cerium oxide/graphene/sulfur composite materials, can solve the problems of low utilization rate of positive electrode active materials, complex preparation process, short cycle life, etc., and achieve easy realization The effect of industrialization, simple process and low production cost

Active Publication Date: 2020-11-03
SYNERGY INNOVATION INST OF GDUT HEYUAN
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical solution adopted by the present invention to solve the technical problem is: the present invention provides a nano-ceria / graphene / sulfur composite material for the problems of low utilization rate of positive electrode active materials, poor rate performance and short cycle life of lithium-sulfur batteries preparation method
This method innovatively completes the graphene oxide reduction, nano-metal oxide doping and sulfur-loaded solvothermal reaction in one step, improves the reaction efficiency, and has a simple preparation process, which overcomes the low utilization rate of the positive electrode active material of the lithium-sulfur battery in the prior art. Disadvantages of poor rate performance, short cycle life, low reaction efficiency, and complex preparation process

Method used

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  • A kind of preparation method of nano ceria/graphene/sulfur composite material
  • A kind of preparation method of nano ceria/graphene/sulfur composite material
  • A kind of preparation method of nano ceria/graphene/sulfur composite material

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Embodiment 1

[0026] (1) Graphene oxide was prepared by the Hummers method: first, 1 g of graphite (325 mesh), 0.5 g of NaNO 3 Pour 23mL of concentrated sulfuric acid into a 250mL beaker, add 3g KMnO4 into the above beaker in an ice bath, then stir for 30min, then add 30mL of deionized water while stirring, and continue stirring for 15min. Then add 50 mL of deionized water again, and finally add 30 mL of H to the mixed solution 2 o 2 , to obtain a graphite oxide solution (containing a large amount of H + ). Add deionized water to the prepared graphite oxide solution, place it in a centrifuge tube for centrifugation (6000 rpm / min), remove the supernatant in the centrifuge tube after centrifugation, add deionized water again, and centrifuge (6000 rpm / min ), repeat this operation until the solution pH=7, and finally obtain the neutral graphite oxide solution. The prepared graphite oxide solution was ultrasonically dispersed at room temperature using an ultrasonic disperser at 50 kHz for 2 ...

Embodiment 2

[0038] (1) utilize Hummers method to prepare graphene oxide (same as embodiment 1);

[0039] (2) Weigh a certain amount of Ce(N03) 3 ·6H 2 O was made into a 1mol / L solution, and ammonia water was added dropwise to pH=10. Continue to stir for 3 hours, after standing for 6 hours, filter, wash with distilled water, and then dry in an oven at 100°C for 12 hours;

[0040] (3) Grind the dried precipitate slightly, or directly put it into a mortar, put it into a muffle furnace, and roast it at 300° C. for 6 hours to obtain nano-cerium dioxide;

[0041] (4) Take a certain amount of nano-sulfur powder (purity is 99.99%) and dissolve it in carbon disulfide (purity is 99.5%) to form a solution of 20 mg / mL;

[0042] (5) Take the graphene oxide and nano-cerium dioxide prepared in the first step according to the ratio of 1:15 in mass ratio, and add the mixture into deionized water according to the ratio of 0.01:1 in the mass ratio of mixture and deionized water, At room temperature, use...

Embodiment 3

[0046] (1) utilize Hummers method to prepare graphene oxide (same as embodiment 1);

[0047] (2) Weigh a certain amount of Ce(N03) 3 ·6H 2 O was made into a 2mol / L solution, and ammonia water was added dropwise to pH=10. Continue to stir for 5 hours, after standing for 8 hours, filter, wash with distilled water, and then dry in an oven at 110°C for 12 hours;

[0048] (3) Grind the dried precipitate slightly, or directly put it into a mortar, put it into a muffle furnace, and roast it at 450°C for 8h to obtain nano-cerium dioxide;

[0049] (4) Take a certain amount of nano-sulfur powder (purity is 99.99%) and dissolve it in carbon disulfide (purity is 99.5%) to form a solution of 20 mg / mL;

[0050] (5) Take the graphene oxide and nano ceria prepared in the first step according to the ratio of 1:9 in mass ratio, and add the mixture into deionized water according to the ratio of 0.01:1 in the mass ratio of mixture and deionized water, At room temperature, use an ultrasonic di...

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Abstract

The invention relates to a nanometer cerium dioxide / graphene / sulphur composite material preparation method. The method comprises the following steps that a carbon disulfide / sulphur solution is added into a graphene oxide / nanometer cerium dioxide mixed suspension, a graphene oxide / nanometer cerium dioxide / sulphur mixed solution is obtained, the mixed solution is loaded into a stainless steel reaction kettle, and a hydrothermal reaction is performed for 5-24 h at 100-200 DEG C; cleaning and vacuum freeze drying are performed, and the nanometer cerium dioxide / graphene / sulphur composite material is obtained. Accordingly, graphene oxide reduction, nanometer metal oxide doping and a loaded sulphur solvent thermal reaction are completed in one step creatively, the reaction efficiency is improved,the preparation technology is simple, and the defects that in the prior art, the lithium-sulfur battery positive active material utilization rate is low, the rate capability is poor, the cycle life is short, the reaction efficiency is low, and the preparation technology is complex are overcome.

Description

technical field [0001] The invention relates to the field of preparation of cathode materials for lithium-sulfur batteries, in particular to a preparation method and application of a nano-cerium oxide / graphene / sulfur composite material. Background technique [0002] In recent years, with the decline of oil production and the intensification of global environmental pollution, countries around the world have generally recognized that clean and pollution-free electric vehicles to replace fuel vehicles is an inevitable choice for a country's sustainable development. The power battery technology with high specific capacity has become the key to the development of pure electric vehicles. However, the specific energy of commercial lithium-ion batteries based on lithium intercalation / extraction is limited by the theoretical specific capacity of the cathode material, and the specific energy of current lithium-ion batteries is difficult to exceed 200Wh / kg. The stagnation of cathode m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/38H01M4/62H01M10/0525B82Y30/00
CPCB82Y30/00H01M4/362H01M4/38H01M4/625H01M4/628H01M10/0525Y02E60/10
Inventor 张永光王新
Owner SYNERGY INNOVATION INST OF GDUT HEYUAN
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