Preparation method of antimony/nitrogen doped graphene compound, and obtained material and application thereof

A nitrogen-doped graphene and composite technology, applied in electrical components, electrochemical generators, battery electrodes, etc., can solve the problem of poor cycle stability, loss of electrical contact between active materials and conductive additives, and reduced first-cycle Coulomb efficiency. and other problems, to achieve the effect of simple process, excellent electrochemical performance, and green raw materials

Active Publication Date: 2018-10-12
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Na can be formed between antimony and sodium 3 Sb alloys, but antimony-based materials undergo severe volume expansion (~390%) during the process of sodation and desodination, causing the active material to lose electrical contact with the conductive additive, resulting in rapid capacity fading
During the cycle, a thick, unstable, electronically insulating solid electrolyte film will be formed on the surface of antimony particles to hinder the progress of the reaction, reduce the first-cycle Coulombic efficiency, and make the cycle stability worse.

Method used

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  • Preparation method of antimony/nitrogen doped graphene compound, and obtained material and application thereof
  • Preparation method of antimony/nitrogen doped graphene compound, and obtained material and application thereof
  • Preparation method of antimony/nitrogen doped graphene compound, and obtained material and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Preparation of Sb / N-rGO composite

[0028] With 10mL graphene oxide dispersion (10mg mL) prepared by Hummers method -1 ), 300mg of purchased commercial antimony powder and 50mg of 1-ethyl-3-methylimidazolium dicyanamide were added into the ball mill jar, and ball milled at 800rpm for 24h. Add 10 mL of water to the ball-milled dispersion for dilution, take out the diluted mixture and ultrasonicate it in a digitally controlled ultrasonic cleaner for 5 minutes to form a uniform dispersion. The resulting solution was quickly frozen with liquid nitrogen and lyophilized for 2 days, and the resulting powder was placed in a single-temperature zone tube furnace under Ar / H 2 atmosphere (wherein H 2 Volume percentage is 5%), at 5°C min -1The speed was heated to 600 °C and kept at this temperature for 2 h to obtain the Sb / N-rGO composite.

[0029] (2) Characterization of antimony / nitrogen doped graphene composites

[0030] The size, morphology and microstructure of the obt...

Embodiment 2

[0047] With 10mL graphene oxide dispersion (10mg mL) prepared by Hummers method -1 ), 250 mg of purchased commercial antimony powder and 50 mg of 1-ethyl-3-methylimidazolium dicyanamide were added into a ball mill jar, and ball milled at 800 rpm for 24 hours. Add 10 mL of water to the ball-milled dispersion for dilution, take out the diluted mixture and ultrasonicate it in a digitally controlled ultrasonic cleaner for 5 minutes to form a uniform dispersion. The resulting solution was quickly frozen with liquid nitrogen and lyophilized for 2 days, and the resulting powder was placed in a single-temperature zone tube furnace under Ar / H 2 atmosphere (wherein H 2 5% by volume), at 4°C min -1 The speed was heated to 600 °C and kept at this temperature for 2 h to obtain the Sb / N-rGO-2 composite.

[0048] The structural characterization and electrochemical performance test of the prepared Sb / N-rGO-2 composite were carried out in the same manner as in Example 1, and the results wer...

Embodiment 3

[0050] With 10mL graphene oxide dispersion (10mg mL) prepared by Hummers method -1 ), 350mg of purchased commercial antimony powder and 50mg of 1-ethyl-3-methylimidazolium dicyanamide were added into the ball mill jar, and ball milled at 800rpm for 24h. Add 10 mL of water to the ball-milled dispersion for dilution, take out the diluted mixture and ultrasonicate it in a digitally controlled ultrasonic cleaner for 5 minutes to form a uniform dispersion. The resulting solution was quickly frozen with liquid nitrogen and lyophilized for 2 days, and the resulting powder was placed in a single-temperature zone tube furnace under Ar / H 2 atmosphere (wherein H 2 10% by volume), at 5°C min -1 The speed was heated to 600 °C and kept at this temperature for 3 h to obtain the Sb / N-rGO-3 composite.

[0051] According to the same method as in Example 1, the structural characterization and electrochemical performance test of the prepared Sb / N-rGO composite were carried out, and the results w...

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Abstract

The invention provides a preparation method of an antimony / nitrogen doped graphene compound, and an obtained composite material and an application of the composite material as a negative electrode material of a sodium ion battery. The preparation method comprises the following steps of 1) performing ball milling and mixing on graphene oxide, 1-ethyl-3-methylimidazole dicyanamide and antimony powder; 2) taking out the ball milled mixture, and enabling the mixture to be dispersed into distilling water, and performing ultrasonic dispersion and uniformizing and freezing and drying; and 3) performing carbonization on the product obtained in the step 2) in H<2> / Ar atmosphere to obtain the antimony / nitrogen doped graphene compound. Compared with the prior art, the method disclosed in the invention is simple in process, the used raw materials are green and environment friendly, the method is suitable for batch production, and the prepared antimony / nitrogen doped graphene compound has excellentelectrochemical performance and can be used as an ideal negative electrode material of the sodium ion battery to replace pure antimony of low reversible capacity to be applied to the sodium ion battery, so that that antimony / nitrogen doped graphene compound is a promising negative electrode material of the sodium ion battery.

Description

technical field [0001] The invention relates to a preparation method of an antimony / nitrogen-doped graphene compound and the obtained material and application thereof, belonging to the technical field of electrode materials. Background technique [0002] Lithium-ion batteries, as the most widely used energy storage system, dominate the power supply market for electric vehicles and portable electronic devices due to their high energy density and long life cycle. However, the scarcity and uneven geographical distribution of lithium resources have seriously hindered the large-scale application of lithium-ion batteries for energy storage. Na-ion batteries have physical and chemical properties comparable to those of lithium, and sodium is abundant and inexpensive, and is considered to be suitable for large-scale stationary energy storage. Recently, a large number of layered oxides and polyanionic compounds have been demonstrated as highly efficient cathode materials for Na-ion b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/38H01M4/583H01M4/62H01M10/054
CPCH01M4/362H01M4/38H01M4/583H01M4/62H01M4/625H01M10/054Y02E60/10
Inventor 周小四许欣
Owner NANJING NORMAL UNIVERSITY
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