Preparation method of iodine-nitrogen co-doped carbon microspheres

A carbon microsphere, co-doping technology, applied in electrical components, electrochemical generators, battery electrodes, etc., can solve the problems of negative electrode volume discount, reduce material density, etc., achieve good sphericity, avoid density reduction, preparation process Simple and gentle effect

Inactive Publication Date: 2018-04-17
YANSHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these defects and voids greatly reduce the density of the material while increasing the lith

Method used

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  • Preparation method of iodine-nitrogen co-doped carbon microspheres
  • Preparation method of iodine-nitrogen co-doped carbon microspheres
  • Preparation method of iodine-nitrogen co-doped carbon microspheres

Examples

Experimental program
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Example Embodiment

[0021] Example 1

[0022] In a glove box protected by nitrogen, add 1g of cetyltrimethylammonium chloride, 4g of analytically pure iodine and 4ml of ethylenediamine to 6ml of toluene, stir for 10 minutes, and put the mixture into a volume of 15ml In a stainless steel reaction kettle, seal; then put the reaction kettle in a crucible boiler and heat it at 300°C for 6 hours, then let the reaction kettle cool to room temperature naturally, and then take out the mixture. Wash the above mixture with absolute ethanol, dilute hydrochloric acid and distilled water successively for 3 times, filter, and then vacuum dry for 12 hours at 60℃ and 0.1MPa vacuum to obtain iodine-nitrogen co-doped carbon microparticles with high volume specific capacitance. ball.

[0023] Such as figure 1 As shown, it can be clearly seen that the microspheres have a smooth surface and good sphericity, and their length is between 1 micron and 4 microns.

[0024] Such as figure 2 As shown, it can be seen that the syn...

Example Embodiment

[0025] Example 2

[0026] In a glove box protected by nitrogen, 1.8 grams of cetyltrimethylammonium bromide, 2.1 grams of analytically pure ammonium iodide, and 9ml of pyrrole were added to 6ml of benzene, stirred for 20 minutes, and the mixture was put into In a 45ml stainless steel reaction kettle, seal it; place the reaction kettle in a crucible boiler and heat it at 600°C for 24 hours, and then let the reaction kettle cool to room temperature naturally, and then take out the mixture. Wash the above mixture with absolute ethanol, dilute hydrochloric acid and distilled water for 5 times, filter, and then vacuum dry at 80°C and 0.1MPa vacuum for 10 hours to obtain iodine-nitrogen-doped carbon microstructures with high volume specific capacitance. ball.

[0027] Such as image 3 As shown, carbon microspheres co-doped with iodine and nitrogen are used as the cyclic voltammetry curve of the first three circles of the negative electrode of the lithium ion battery. It can be seen that...

Example Embodiment

[0028] Example 3

[0029] In a glove box protected by nitrogen, add 1 g of cetyltrimethylammonium bromide, 2 g of analytically pure hydroiodic acid, and 28 ml of acetonitrile to 4 ml of xylene, stir for 30 minutes, and put the mixture into the volume In a 45ml stainless steel reaction kettle, seal it; place the reaction kettle in a crucible boiler and heat it at 450°C for 48 hours, and then let the reaction kettle cool to room temperature naturally, and then take out the mixture. The above mixture was washed with absolute ethanol, dilute hydrochloric acid and distilled water 6 times, filtered, and then vacuum dried at 100°C and 0.1MPa vacuum for 6 hours to obtain iodine-nitrogen co-doped carbon microstructures with high volumetric capacitance. ball.

[0030] Such as Figure 4 As shown, it can be seen that the carbon microspheres have good dispersion, and the surface of the microspheres is smooth, with a diameter between 2 microns and 6 microns, and a good sphericity.

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Abstract

The invention discloses a preparation method of iodine-nitrogen co-doped carbon microspheres. The method mainly comprises the steps of sequentially adding the following raw materials in percentages bymass (wt%): 12-60% of a carbon source, 26-76% of a nitrogen source, 3-28% of an iodine source and 1-10% of a surfactant to a stainless steel reactor, stirring for 10-30min and sealing the reactor; putting the stainless steel reactor into a crucible furnace, heating the crucible furnace at 300-600 DEG C for 6-48h, naturally cooling the reactor to room temperature and taking out a mixture; and washing the mixture by using absolute ethyl alcohol, diluted hydrochloric acid and distilled water in sequence for 3-6 times, filtering and putting obtained powder into a vacuum drying oven for drying at60-100 DEG C for 6-12h, wherein the vacuum degree is 0.1MPa, thereby preparing the iodine-nitrogen co-doped carbon microspheres. The iodine-nitrogen co-doped carbon microspheres are simple in synthetic process, mild in reaction condition and high in repeatability and have relatively high volumetric specific capacitance as a negative electrode of a lithium-ion battery.

Description

technical field [0001] The invention relates to a preparation method of a battery negative pole, in particular to a preparation method of a lithium ion battery negative pole. Background technique [0002] Facing the ever-increasing demand for energy and the depletion of fossil fuels, we urgently need to utilize sustainable energy alternatives. However, current renewable energy sources such as solar energy, tidal energy, wind energy, and geothermal energy are generally indirect and decentralized and cannot be directly applied. This requires a complete energy storage and conversion system. Among them, the rechargeable battery has received extensive attention and research because of its ability to store electrical energy as chemical energy and then convert chemical energy into low-voltage DC electrical energy. In the current rechargeable batteries, lithium-ion batteries have higher working voltage (about 3.7V), greater specific energy (100Wh kg -1 ), small self-discharge, lo...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/587H01M4/62H01M10/0525
CPCH01M4/362H01M4/587H01M4/62H01M10/0525Y02E60/10
Inventor 高发明王栋周军双李俊凯
Owner YANSHAN UNIV
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