Preparation method of high-nitrogen-doped graphene nanoparticles and application of high-nitrogen-doped graphene nanoparticles as negative material of lithium ion battery

A lithium-ion battery and nanoparticle technology, applied in battery electrodes, nanotechnology, nanotechnology, etc., can solve the problems of complex process, long reaction time, high temperature, etc., achieve simple and efficient preparation process, increase nitrogen doping amount, The effect of short synthesis cycle

Active Publication Date: 2014-12-10
UNIV OF SCI & TECH OF CHINA
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Problems solved by technology

However, the current methods for preparing nitrogen-doped carbon materials are mainly limited to high-temperature solid-state methods, and these methods require higher temperatures and longer reaction times, and will introduce a large number of toxic small molecules (such as ammonia, melamine, etc.)
In addition, the nitrogen content in the obtained nitrogen-doped carbon materials is low, and the process in the preparation process is often complicated, and it is difficult to obtain large-scale promotion and industrial application.

Method used

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  • Preparation method of high-nitrogen-doped graphene nanoparticles and application of high-nitrogen-doped graphene nanoparticles as negative material of lithium ion battery
  • Preparation method of high-nitrogen-doped graphene nanoparticles and application of high-nitrogen-doped graphene nanoparticles as negative material of lithium ion battery
  • Preparation method of high-nitrogen-doped graphene nanoparticles and application of high-nitrogen-doped graphene nanoparticles as negative material of lithium ion battery

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1, prepare uniform ZIF-8 nanoparticles

[0025] At room temperature, 50mL containing 105mg zinc nitrate (Zn(NO 3 )) methanol solution was slowly dripped into 50mL containing 120mg of 2-methylimidazole (C 4 h 6 N 2 ) and 1.5 g of polyvinylpyrrolidone (PVP) in methanol solution, magnetically stirred and left to stand for 10 hours, centrifuged to obtain the precursor ZIF-8 (complex formed by zinc and 2-methylimidazole) nanoparticles.

[0026] Such as figure 1 Shown, the X-ray diffraction of precursor ZIF-8 in the present embodiment ( ) figure, all diffraction peaks are consistent with the simulated ZIF-8 crystal data, showing that the product is ZIF-8 with good crystallinity. figure 2 are scanning electron microscope (SEM) photos and transmission electron microscope (TEM) photos of the product. From figure 2 (a) In the SEM image, it can be seen that ZIF-8 exists in the form of nanoparticles, and the particles have a uniform shape, a polyhedral shape, a...

Embodiment 2

[0027] Embodiment 2, preparation of high nitrogen-doped graphene-like nanoparticles

[0028]The precursor ZIF-8 nanoparticles obtained in Implementation 1 were placed in a crucible, and the temperature was raised to 800° C. at a rate of 5° C. / min in a nitrogen atmosphere, where the gas flow was 400 ml / min. Then calcining at this temperature for 8 hours, after naturally cooling to room temperature, immerse the obtained sample with 35% hydrochloric acid with a mass fraction to remove impurities such as zinc oxide remaining on the sample, then wash the obtained sample with water and ethanol successively for three times, Highly nitrogen-doped graphene-like nanoparticles (N-C-800) can be obtained.

[0029] The chemical composition of the particles can be determined by X-ray diffraction. Such as image 3 Shown, the X-ray diffraction ( )picture. The broad front at around 24° corresponds to the (002) crystal plane of the graphite-type carbon material, indicating that the sample i...

Embodiment 3

[0033] Embodiment 3, the influence of calcining temperature on product

[0034] Same as other conditions in Example 2, the precursor ZIF-8 was calcined at 900°C and 700°C respectively to obtain black products N-C-900 and N-C-700. Like the sample calcined at 800°C, the broad front at around 24° corresponds to the (002) crystal plane of the graphite-type carbon material, indicating that the sample is a graphite-type carbon material with low crystallinity. Figure 6 middle Figure 6 (a) and Figure 6 (b) Scanning electron micrographs corresponding to N-C-900 and N-C-700, respectively, where the inset is the transmission electron micrograph of the corresponding sample. It can be seen from the figure that when the calcination temperature rises from 700 °C to 900 °C, the morphology of the product changes little. However, nitrogen adsorption and desorption data show (as shown in Table 1), the specific surface area from 730.1m 2 / g(N-C-700) becomes 657.2m 2 / g(N-C-900), the space...

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Abstract

The invention provides a preparation method of high-nitrogen-doped graphene nanoparticles and application of the high-nitrogen-doped graphene nanoparticles as a negative material of a lithium ion battery. The corresponding method comprises the following steps: slowly dropwise adding a preset quantity of zinc nitrate (Zn(NO3)) methanol solution into a methanol mixed solution which is prepared from a preset amount of 2-methylimidazole (C4H6N2) and a preset amount of polyvinylpyrrolidone (PVP), magnetically stirring and standing for preset time, carrying out centrifugal separation to obtain ZIF-8(a complex formed by zinc and 2-methylimidazole) nanoparticles; and putting the obtained ZIF-8 nanoparticles in a high-temperature furnace and calcining at 600-1,000 DEG C for preset time in the nitrogen atmosphere to obtain the high-nitrogen-doped graphene nanoparticles. The preparation process of the high-nitrogen-doped graphene nanoparticles is simple, and the high-nitrogen-doped graphene nanoparticles are uniform in shape, relatively large in specific surface and high in content of nitrogen, and have great application potentials in aspects of lithium ion batteries, electrochemical energy storage, catalysis and the like. The preparation method of the high-nitrogen-doped graphene nanoparticles is simple and efficient, safe and liable to implement, short in synthesis cycle, is capable of preparing a large quantity of high-nitrogen-doped graphene nanoparticles and is expected to be popularized and industrially applied.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, and in particular relates to a preparation method of high nitrogen-doped graphene-like nanoparticles and its application in negative electrode materials of lithium-ion batteries. Background technique [0002] Nitrogen-doped graphene is a new type of material with a wide range of uses. Because it contains nitrogen atom doping and has a special two-dimensional planar structure, it has great applications in electronics, catalysis, energy conversion and storage, etc. prospect. In 2014, the U.S. "Nano Letters" magazine (Nano Letters, 2014, the 14th volume, page 1164) reported the preparation of nitrogen-doped graphene in argon, and when the material was used as a lithium-ion battery negative electrode material, the performance A better performance. In 2011, the Journal of Material Chemistry of the Royal Society of Chemistry (Journal of Material Chemistry, 2011, Vol. 21, p. 5430) rep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/583
CPCB82Y30/00H01M4/583H01M4/587H01M10/0525Y02E60/10
Inventor 陈乾旺郑方才
Owner UNIV OF SCI & TECH OF CHINA
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