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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 lithium storage capacity, which greatly reduces the volume specific capacitance of the negative electrode.

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
Comparison scheme
Effect test

Embodiment 1

[0022] In a nitrogen-protected glove box, add 1g of cetyltrimethylammonium chloride, 4g of analytically pure iodine and 4ml of ethylenediamine to 6ml of toluene in sequence, stir for 10 minutes, and put the mixture into a volume of 15ml In a stainless steel reaction kettle, seal it; then place the reaction kettle in a crucible boiler, heat it at 300°C for 6 hours, then wait for the reaction kettle to cool down to room temperature naturally, and take out the mixture. The above mixture was washed three times successively with absolute ethanol, dilute hydrochloric acid and distilled water, filtered, and then vacuum-dried at 60°C and 0.1MPa vacuum for 12 hours 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 surface of the microsphere is smooth and spherical, and its length is between 1 micron and 4 microns.

[0024] Such as figure 2 It can be seen that the ...

Embodiment 2

[0026] In a nitrogen-protected glove box, 1.8 grams of cetyltrimethylammonium bromide, 2.1 grams of analytically pure ammonium iodide and 9 ml of pyrrole were added to 6 ml of benzene in turn, stirred for 20 minutes, and the mixture was put into a volume of 45ml stainless steel reaction kettle, sealed; then the reaction kettle was placed in a crucible boiler, heated at 600 ° C for 24 hours, and then the reaction kettle was naturally cooled to room temperature, and the mixture was taken out. The above mixture was washed 5 times with absolute ethanol, dilute hydrochloric acid and distilled water successively, filtered, and then vacuum-dried at 80°C and 0.1MPa vacuum for 10 hours to obtain iodine-nitrogen-doped carbon microparticles with high volume specific capacitance. ball.

[0027] Such as image 3 As shown, the carbon microspheres co-doped with iodine and nitrogen are used as the cyclic voltammetry curves of the first three cycles of the negative electrode of the lithium-io...

Embodiment 3

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

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

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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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