Preparation method of nano lanthanum oxide/graphene/sulfur composite material

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

Active Publication Date: 2018-02-27
SYNERGY INNOVATION INST OF GDUT HEYUAN
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  • Abstract
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  • Claims
  • Application Information

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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-lanthanum oxide / 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
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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  • Preparation method of nano lanthanum oxide/graphene/sulfur composite material
  • Preparation method of nano lanthanum oxide/graphene/sulfur composite material
  • Preparation method of nano lanthanum oxide/graphene/sulfur composite material

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Embodiment 1

[0028] (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

[0040] (1) utilize Hummers method to prepare graphene oxide (same as embodiment 1);

[0041] (2) Weigh a certain amount of lanthanum chloride to make a 0.2 mol / L solution, and add NaOH dropwise until pH=10. After standing for 4 hours, the precipitate was filtered, washed 4 times with distilled water, and then dried in an oven at 60°C for 10 hours; the molar concentration of NaOH was 0.6moL / L.

[0042] (3) Grind the dried precipitate slightly, or directly put it into a mortar, put it into a tube furnace, and calcinate it at 450° C. for 3 hours under a nitrogen atmosphere to obtain nano-lanthanum oxide;

[0043] (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 30 mg / mL;

[0044] (5) Take the graphene oxide and nano-lanthanum oxide prepared in the first step according to the ratio of mass ratio 1:15, according to the ratio of mixture and deionized water mass ratio of 0.01:1, the mixture...

Embodiment 3

[0048] (1) utilize Hummers method to prepare graphene oxide (same as embodiment 1);

[0049] (2) Weigh a certain amount of lanthanum chloride to make a 2mol / L solution, and add NaOH dropwise until pH=10. After standing for 4 hours, the precipitate was filtered, washed 6 times with distilled water, and then dried in an oven at 100°C for 12 hours; the molar concentration of NaOH was 0.6moL / L.

[0050] (3) The dried precipitate is slightly ground, or directly put into a mortar, put into a tube furnace, and calcined at 900° C. for 6 hours under a nitrogen atmosphere to obtain nano-lanthanum oxide;

[0051] (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 30 mg / mL;

[0052] (5) Take the graphene oxide and nano-lanthanum oxide prepared in the first step according to the ratio of 1:20 in mass ratio, and add the mixture into deionized water according to the ratio of 0.01:1 in the mass ratio ...

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Abstract

The invention relates to a preparation method of a nano lanthanum oxide / graphene / sulfur composite material. The method comprises the following steps: adding a carbon disulfide / sulfur solution into a graphene oxide / nano lanthanum oxide mixed suspension liquid, and performing hydrothermal reaction in a stainless steel reaction kettle for 5 to 24 h; and cleaning, and vacuum freeze-drying, thus obtaining the nano lanthanum oxide / graphene / sulfur composite material. According to the preparation method, the reduction of the graphene oxide, the doping of nano metal oxide and the thermal reaction of the loaded sulfur solvent are innovatively completed in one step, so that the reaction efficiency is improved, the preparation process is simple, and the weaknesses in the prior art that the utilizationrate of the lithium-sulfur battery positive active substances is low, the rate capacity is poor, the cycle life is short, the reaction efficiency is low, and the preparation process 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-lanthanum oxide / graphene / sulfur composite material. Background technique [0002] Nowadays, problems such as environmental pollution, greenhouse effect, and energy crisis are becoming more and more serious in the world, and secondary batteries with high specific energy are of great significance for solving prominent energy and environmental problems. Lithium-ion secondary batteries have excellent properties such as high reversible capacity, high voltage, high cycle performance, and high energy density, and are currently the dominant power source for practical use. However, traditional lithium-ion battery cathode materials, such as lithium iron phosphate, have low theoretical specific capacity, which limits further development. Lithium-sulfur batteries generally use elemental sulfur or sulf...

Claims

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Application Information

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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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