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Synthesis method for preparing carbon-coated CoTiO3 nanocrystalline material through MOF derivation

A technology of nano crystallite and synthesis method, which is applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of high cost, inability to ensure uniform loading of cobalt titanate nanoparticles, etc., and achieve synthesis Low cost, improved electrochemical performance, and excellent high-rate discharge performance

Active Publication Date: 2018-10-16
YANSHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires high-quality graphene to be used as a carrier, and the cost is relatively high, and it cannot ensure that cobalt titanate nanoparticles are evenly loaded on graphene.

Method used

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  • Synthesis method for preparing carbon-coated CoTiO3 nanocrystalline material through MOF derivation
  • Synthesis method for preparing carbon-coated CoTiO3 nanocrystalline material through MOF derivation
  • Synthesis method for preparing carbon-coated CoTiO3 nanocrystalline material through MOF derivation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) 237mg CoCl 2 ·6H 2 O and 332mg of terephthalic acid were put into 32ml of N,N-dimethylformamide solvent, stirred for 10 minutes, added 2mL of dilute ammonia water with a concentration of 0.5mol / L, mixed well, and put into a 50ml Teflon kettle , the filling amount was 70%, sealed, and reacted at 100°C for 24 hours. After the kettle was naturally cooled, the mixture was washed by centrifugation with absolute ethanol three times, and vacuum-dried at 60°C for 6 hours to obtain a cobalt-based MOF stacked by layers.

[0030] (2) According to the ratio of adding 1 mg butyl titanate per 1 mL of anhydrous methanol solution, prepare A solution, disperse 200 mg of cobalt-based MOF into 20 mL of anhydrous methanol solution, ultrasonically disperse it for 10 minutes, and prepare B solution ; Then add 15ml of solution A to solution B, stir for 10 minutes, then transfer the dispersion to a Teflon reactor with a filling capacity of 70%. Airtightly heat at 100°C and react for 10 h...

Embodiment 2

[0035] (1) 355mg CoCl 2 ·6H 2O and 162mg of 2-methylimidazole were put into 22ml of absolute ethanol, stirred for 30 minutes, and 3mL of dilute ammonia water with a concentration of 0.5mol / L was added. %, sealed, and reacted at 130°C for 16 hours. After the kettle was naturally cooled, the mixture was centrifuged and washed 3 times with absolute ethanol, and vacuum-dried at 60°C for 12 hours to obtain a cobalt-based MOF stacked in layers.

[0036] (2) According to the ratio of adding 1 mg butyl titanate to every 1 mL of anhydrous methanol solution, A solution was prepared, 200 mg of cobalt-based MOF was dispersed in 17.5 mL of anhydrous methanol solution, and ultrasonically dispersed for 10 minutes to prepare B solution solution; then add solution A to solution B, stir for 20 minutes, then transfer the dispersion to a Teflon reaction kettle with a filling capacity of 70%, heat in a closed manner at 160°C, and react for 6 hours. After cooling, wash with absolute ethanol After...

Embodiment 3

[0041] (1) 237mg CoCl 2 ·6H 2 Put O and 210mg of trimesic acid into 26ml of anhydrous methanol, stir for 20 minutes, add 4mL of dilute ammonia water with a concentration of 0.5mol / L, mix well, and put it into a 50ml Teflon kettle with a filling capacity of 60%. , sealed, and reacted at 180°C for 12 hours. After the kettle was naturally cooled, the mixture was centrifuged and washed three times with absolute ethanol, and vacuum-dried at 60°C for 10 hours to obtain a cobalt-based MOF.

[0042] (2) According to the ratio of adding 1 mg butyl titanate per 1 mL of anhydrous methanol solution, prepare solution A, disperse 200 mg of cobalt-based MOF into 15 mL of anhydrous methanol solution, and disperse it uniformly by ultrasonication for 10 minutes, and prepare solution B ; After that, add 20mL of A solution to B solution, stir for 30 minutes, then transfer the dispersion to a Teflon reactor with a filling capacity of 70%, heat in a closed manner at 180°C, and react for 4 hours. A...

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Abstract

The invention provides a synthesis method for preparing a carbon-coated CoTiO3 nanocrystalline material through MOF derivation. The synthesis method mainly comprises the steps of dissolving CoCl2.6H2Oand a ligand (trimesic acid, 2-methylimidazole or terephthalic acid) into a solvent (N,N-dimethylformamide, anhydrous methanol or anhydrous ethanol) and preparing cobalt-based MOF by using a Teflon reactor and a solvothermal method; dispersing the cobalt-based MOF into an anhydrous methanol solution, adding the anhydrous methanol solution of butyl titanate, and carrying out the solvothermal method once again to compound titanium oxide on the cobalt-based MOF to obtain a precursor; and finally carrying out alloying reaction in a closed manner by using a special stainless steel kettle under protective atmosphere and generating the carbon-coated CoTiO3 nanocrystalline material. The synthesis method is low in synthesis cost, mild in reaction condition and high in repeatability; the prepared nanocrystalline material is small in particle size, carbon coating on CoTiO3 nanocrystalline is uniform and the prepared carbon-coated CoTiO3 nanocrystalline material is good in electrochemical properties.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to a preparation method of battery negative electrode materials. Background technique [0002] Lithium-ion secondary batteries have the advantages of high specific energy, high working voltage, long cycle life, safety and pollution-free, and have become the fastest-growing and most valued high-energy batteries. Commercial graphitic carbon anode materials have good cycle performance, but the specific capacity (300mAhg -1 -350mAhg -1 ) is low, which cannot meet the development requirements of high specific energy batteries, and there is an urgent need for research and exploration of new high-capacity negative electrode materials. [0003] In recent years, metal oxides, especially transition metal oxides such as (Fe, Co, Ni), have been reported more and more as anode materials for lithium-ion batteries. Transition metal oxides are applied to the negative electrode of l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/583H01M4/52H01M10/0525B82Y30/00
CPCB82Y30/00H01M4/366H01M4/52H01M4/583H01M10/0525Y02E60/10
Inventor 高发明李俊凯王栋周军双
Owner YANSHAN UNIV
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