Iron sesquioxide nanotube material as well as preparation method and application thereof
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A ferric oxide and nanotube technology, applied in nanotechnology, nanotechnology, secondary battery manufacturing, etc., can solve problems such as poor cycle life and low coulombic efficiency, achieve good reproducibility, improve coulombic efficiency, and be suitable for The effect of mass production
Active Publication Date: 2016-09-28
镇江微电智能科技有限公司
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[0004] The purpose of the present invention is to solve the technical problems of low coulombic efficiency and poor cycle life of the existing ferric oxi
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Embodiment 1
[0028] (1) Add 0.822g of ferric chloride and 1.234g of fumaric acid to a beaker containing 80ml of deionized water, and keep stirring at a speed of 800r / min until all are dissolved;
[0029] (2) Place the mixed aqueous solution in step (1) in a 100 mL autoclave, and then place it in an oven for hydrothermal treatment, keep it at 70°C for 24 hours, and then cool it naturally to room temperature;
[0030] (3) The sample after hydrothermal in step (2) is centrifuged at 6000r / min and washed with ethanol and deionized water for 3 times; finally, the precipitate is dried in a vacuum drying at 80°C to obtain iron Metal-based organic framework nanofibers.
[0031] (4) Put the iron-based metal-organic framework nanofibers dried in step (3) in a tube furnace, and pass air shielding gas at an air intake of 0.15L / min. The heating rate is 2℃ / min, and the temperature is increased to After being kept at 550°C for 4 hours, it is naturally cooled to room temperature to obtain the ferric oxide nanotu...
Embodiment 2
[0034] (1) Add 1.112g ferric nitrate and 1.112g fumaric acid to a beaker containing 80ml deionized water, and stir continuously at a speed of 700r / min until all are dissolved;
[0035] (2) Place the mixed aqueous solution in step (1) in a 100mL autoclave, and then place it in an oven for hydrothermal treatment, keep it at 80°C for 24 hours and then cool it naturally to room temperature;
[0036] The other steps are the same as in Example 1.
Embodiment 3
[0038] (1) Add 0.741g of iron sulfate and 1.334g of fumaric acid to a beaker containing 80ml of deionized water and stir continuously at a speed of 900r / min until all are dissolved;
[0039] (2) Place the mixed aqueous solution in step (1) in a 100mL autoclave, and then place it in an oven for hydrothermal treatment, keep it at 75°C for 24 hours, and then cool to room temperature naturally;
[0040] The other steps are the same as in Example 1.
[0041] Table 1 shows the capacity of the lithium ion batteries of Examples 1 to 3 in the first cycle and the 50th cycle of the charge-discharge test at a current of 0.1C.
[0042] Table 1
[0043]
[0044] It can be seen from Table 1 that the ferric oxide nanotubes prepared by this method are used as electrode materials and applied to lithium-ion batteries. After 50 cycles of cycles, the capacity retention rate is above 88.4%, which has good cycle performance and is still high. For the current commercial graphite anode material.
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Abstract
The invention discloses an iron sesquioxide nanotube cathode material, which is prepared from an iron salt, fumaric acid and deionized water. A preparation method comprises the following steps of first adding a trivalent iron salt and the fumaric acid into the deionized water, and agitating an obtained aqueous solution for 2 to 6 hours at a rotational speed of 600r/min to 1,000r/min; afterwards, transferring the mixed aqueous solution into a high-pressure reaction kettle to keep the mixed aqueous solution for 12 to 24 hours at 70 DEG C to 90 DEG C; naturally cooling the mixed aqueous solution to be at a room temperature, then carrying out centrifugal separation on a precipitate, which is generated in a low-temperature hydrothermal manner, at a rotational speed of 4,000r/min to 7,000r/min, and successively washing the precipitate for three times by using ethanol and the deionized water; subsequently, carrying out vacuum drying on the precipitate in a condition of 80 DEG C to 100 DEG C, so as to obtain an iron-based metal organic framework nanofiber; finally, placing the iron-based metal organic framework nanofiber in a tube furnace, introducing an air shielding gas into the tube furnace according to an inlet gas volume of 0.2L/min to 0.8L/min, raising a temperature to 550 DEG C to 600 DEG C according to a temperature raising rate of 0.5 DEG C per minute to 2 DEG C per minute, carrying out heat preservation for 2 to 6 hours, and naturally cooling the precipitate to the room temperature, so as to obtain an iron sesquioxide nanotube material. The iron sesquioxide nanotube material prepared by the invention is applied to a lithium ion battery; the initial coulombic efficiency of a lithium battery is improved, and the cycle life of the lithium battery is prolonged; the technique is simple; the reproducibility is good; the implementation is easy.
Description
Technical field [0001] The invention relates to the technical field of lithium ion battery negative electrode materials, in particular to a lithium ion battery ferric oxide nanotube material, and a preparation method and application thereof. Background technique [0002] Lithium-ion batteries have the advantages of high voltage, high capacity, small size, light weight, no memory effect, small self-discharge and long cycle life, making them a new type of chemical power source with great potential in the 21st century. At present, the theoretical capacity of the anode material graphite in commercial lithium batteries is only 372mAh / g, which cannot meet the application requirements of high-performance batteries. Therefore, the development of anode materials with higher capacity, long cycle life and high rate performance has become a goal pursued by domestic and foreign researchers. Among them, transition metal oxide ferric oxide (Fe 2 O 3 ) The theoretical capacity (1007mAh / g) is 3 ...
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