Preparation method of novel porous skeleton MIL-101(Cr)@S/graphene composite material for cathode of lithium sulfur battery

A composite material and graphene technology, applied in battery electrodes, circuits, electrical components, etc., can solve problems such as poor cycle performance and uneven dispersion of coated sulfur, improve adhesion, simple and easy-to-operate preparation method, and promote cycle performance Effect

Inactive Publication Date: 2012-10-24
GUANGZHOU HKUST FOK YING TUNG RES INST
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Problems solved by technology

[0007] The purpose of the present invention is to provide a method for preparing a lithium-sulfur positive electrode material that uses porous materials to carry sulfur and then composites with graphene for the defects of existing mesoporous carbon materials and graphene-coated sulfur, such as uneven dispersion and poor cycle performance.

Method used

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  • Preparation method of novel porous skeleton MIL-101(Cr)@S/graphene composite material for cathode of lithium sulfur battery
  • Preparation method of novel porous skeleton MIL-101(Cr)@S/graphene composite material for cathode of lithium sulfur battery
  • Preparation method of novel porous skeleton MIL-101(Cr)@S/graphene composite material for cathode of lithium sulfur battery

Examples

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Effect test

Embodiment 1

[0035] (1) Synthesis of MIL-101(Cr) metal-organic framework: 2.0 g of Cr(NO 3 ) 3 9H 2 O and 0.833 g of terephthalic acid H 2Dissolve BDC in 30 mL of deionized water, then add 0.26 mL of HF, move the solution into a 50 mL polytetrafluoroethylene reaction tank after fully dissolving, then place the reaction tank in a stainless steel jacket and seal it; put the reaction tank in The hydrothermal reaction was carried out in a temperature-programmed furnace, and the heating program was as follows: the solution was heated from room temperature to 210 oC at 5 oC / min, and kept for 8 h, and then the solution was lowered to room temperature at a cooling rate of 0.4 oC / min; After the solution was cooled to room temperature, the crystals were washed with water, dimethylformamide (DMF) and ethanol in sequence, centrifuged, filtered and dried to obtain the MIL-101(Cr) metal-organic framework material. (2) Preparation of metal-organic framework MIL-101(Cr)S composite material: mix sulfur ...

Embodiment 2

[0037] (1) Synthesis of MIL-101(Cr) metal-organic framework: 2.2 g of Cr(NO 3 ) 3 9H 2 O and 0.900 g of terephthalic acid H 2 Dissolve BDC in 40 mL of deionized water, then add 0.28 mL of HF, and after fully dissolved, move the solution into a 100 mL capacity polytetrafluoroethylene reaction tank, then place the reaction tank in a stainless steel jacket and seal it; put the reaction tank in The hydrothermal reaction was carried out in a temperature-programmed furnace, and the heating program was as follows: the solution was heated from room temperature to 220 oC at 8.0 oC / min, and kept for 9 h, and then the solution was lowered to room temperature at a cooling rate of 0.5 oC / min; After the solution was cooled to room temperature, the crystals were washed with water, dimethylformamide (DMF) and ethanol in sequence, centrifuged, filtered and dried to obtain the MIL-101(Cr) metal-organic framework material. (2) Preparation of metal-organic framework MIL-101(Cr)S composite mate...

Embodiment 3

[0039] (1) Synthesis of MIL-101(Cr) metal-organic framework: 2.4 g of Cr(NO 3 ) 3 9H 2 O and 0.996 g of terephthalic acid H 2 Dissolve BDC in 50 mL of deionized water, then add 0.30 mL of HF, and after fully dissolved, move the solution into a 100 mL capacity polytetrafluoroethylene reaction tank, then place the reaction tank in a stainless steel jacket and seal it; put the reaction tank in The hydrothermal reaction was carried out in a temperature-programmed furnace, and the heating program was as follows: the solution was heated from room temperature to 220 oC at 10.0 oC / min, and kept for 10 h, and then the solution was lowered to room temperature at a cooling rate of 0.6 oC / min; After the solution was cooled to room temperature, the crystals were washed with water, dimethylformamide (DMF) and ethanol in sequence, centrifuged, filtered and dried to obtain the MIL-101(Cr) metal-organic framework material. (2) Preparation of metal-organic framework MIL-101(Cr)S composite ma...

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Abstract

The invention discloses a preparation method of a metal organic skeleton MIL-101(Cr)@S/graphene composite material as the cathode material of a lithium sulfur battery. The preparation method comprises the following steps of: evenly loading sulfur into a three-dimensional pore channel of MIL-101(Cr) by a melting diffusing method, and mixing with graphene, so that the MIL-101(Cr)@S/graphene composite material can be prepared. The metal organic skeleton crystal material in the composite material is has superhigh specific surface area and pore volume and has a skeleton structure which has medium-mirco double pores, so that the dual effects of dispersing and fixing the sulfur grains can be played, and the whole electrical conductivity of the composite material can be improved due to graphene, so that the polarization of the material can be weakened, the discharge multiplying power performance can be improved, the coulomb efficiency can be improved and the like. The electrochemical performance test shows that the discharge specific capacity of the MIL-101(Cr)@S/graphene composite material prepared by the method can reach 1087mAh/g under the condition that the multiplying power is less than 0.1C, and the discharge specific capacity of the MIL-101(Cr)@S/graphene composite material prepared by the method is respectively kept at 807 and 387mAh/g under the condition that the multiplying power is 0.8C and 2.4C when the circulation times is 116 and 150. The preparation method has the advantages that the preparation method has the characteristics of being simple in process, convenient to operate, good in material performance and the like, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of material chemistry, and relates to a porous material as a skeleton, through processes such as melting-diffusion-adsorption, the sulfur component is fixed in the pores of the porous material as nanoparticles, and then mixed with graphene, and specifically relates to a new porous skeleton Preparation method of MIL-101(Cr)S / graphene lithium-sulfur battery cathode composite material. Background technique [0002] Lithium-sulfur battery is a type of lithium secondary battery that uses elemental sulfur (or sulfur-containing compounds) as the positive electrode and metal lithium as the negative electrode, and realizes the mutual conversion of chemical energy and electrical energy through the chemical reaction between sulfur and lithium. Compared with lithium-ion secondary batteries, lithium-sulfur batteries have a high theoretical capacity, up to 2600 Wh / kg, and are high-energy-density, environmentally friendly, and cheap...

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 赵祯霞施志聪陈国华邓胜男
Owner GUANGZHOU HKUST FOK YING TUNG RES INST
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