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Method for preparing nanometer manganous-manganic oxide/carbon composite energy storage material

A technology of trimanganese tetraoxide and energy storage materials, which is applied in the field of preparation of nanometer trimanganese tetraoxide/carbon composite energy storage materials, can solve the problems of high energy consumption, high temperature requirement, environmental pollution, etc., and achieve low energy consumption and excellent The effect of supercapacitor performance

Inactive Publication Date: 2013-12-11
TIANJIN POLYTECHNIC UNIV
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Problems solved by technology

Yin Longwei et al. (ACS Applied Materials & Interfaces, 2012, 4: 1636-1642) reported a two-step synthesis of manganese tetraoxide / carbon composites using manganese acetate monohydrate as a precursor, ethylene glycol as a nucleating agent, and polyvinylpyrrolidone as a carbon source. Material: First, hydrothermal reaction at 180°C for 48 hours, and then sintering in nitrogen atmosphere at 700°C for 4 hours. The disadvantage is that the process is complicated, high temperature is required, and energy consumption is large.
Chinese patent CN101901916A reports a preparation method of carbon-supported trimanganese tetraoxide: first, carbon black is used to absorb manganese nitrate in water, after drying, the temperature is kept at 400°C for 3 hours, and the carbon-supported trimanganese tetraoxide composite material is obtained after grinding. The disadvantages are Manganese nitrate is decomposed to generate nitrogen oxide gas, which is easy to pollute the environment and requires high energy consumption
Wang Zhilin et al. (Chemistry-A European Journal, 2013, 19, 7084-7089) reported using manganese trioxide as a precursor and glucose as a carbon source for hydrothermal reaction at 180°C for 12 hours, and then in an argon atmosphere at 400°C for 30 minutes The shortcoming of synthesizing trimanganese tetraoxide / carbon composite material is also high temperature, and the specific capacity of the trimanganese tetraoxide / carbon composite supercapacitor material synthesized by this method is only 174F / g at 1A / g

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Embodiment 1

[0016] Embodiment 1: the preparation of nano trimanganese tetraoxide / carbon (20%) composite material

[0017] Slowly add 50 milliliters of oleic acid into 1.5 liters of 0.04 mol / L potassium permanganate solution under stirring. After reacting at room temperature for 24 hours, the obtained solid was filtered, washed and dried. Weigh 0.3 g of the above product, add 100 ml of absolute ethanol, and ultrasonically disperse. Then the solution was transferred to a reaction kettle and reacted at 160° C. for 24 hours. Centrifuge, wash and dry to obtain the product. Product X-ray powder diffraction spectrum ( figure 1 ) is consistent with the standard spectrogram (JCPDS No.24-0734) of manganese ore type trimanganese tetroxide, but a broad diffraction peak of amorphous carbon appears near 20 °; the diffraction peak is wider, indicating that the crystal grains are smaller. The average particle size calculated by the formula is about 11.4nm. From the scanning electron microscope image...

Embodiment 2

[0018] Embodiment 2: the preparation of nanometer trimanganese tetraoxide / carbon (7%) composite material

[0019] Weigh 0.3 g of the solid intermediate product obtained in Example 1, add 100 ml of absolute ethanol, and ultrasonically disperse. According to the mass ratio of iodine / manganese dioxide of 1:1, 0.3 g of elemental iodine was added and dissolved. Then the solution was transferred to a reaction kettle and reacted at 160° C. for 24 hours. Centrifugal separation, washing and drying to obtain nanometer trimanganese tetraoxide / carbon composite material. X-ray powder diffraction spectrum ( image 3 ) is consistent with the standard spectrogram (JCPDS No.24-0734) of manganese ore type trimanganese tetroxide; compared with the product of Example 1, the sharpness of the diffraction peak changes shows that crystallinity improves, and the average particle diameter is calculated by Scherrer's formula 27nm. This is because the carbon generated in the reaction is reduced, whic...

Embodiment 3

[0020] Embodiment 3: Electrochemical performance test of trimanganese tetraoxide and trimanganese tetraoxide / carbon composite material

[0021] The electrochemical properties of pure trimanganese tetraoxide and trimanganese tetraoxide / carbon composite were tested at room temperature with a three-electrode system, in which the reference electrode was a saturated calomel electrode and the auxiliary electrode was a platinum electrode. The electrolyte is 1mol / L sodium sulfate solution. The constant current charge and discharge test is carried out with the Blue Electric CT2001A battery test system, and the voltage range is 0-1.0V. The result is as follows:

[0022] (1) by Figure 5 It can be seen that, with a current density of 0.2A / g, the specific capacities of manganese tetraoxide / carbon with 7% and 20% carbon content are 218.2F / g and 207.8F / g, respectively. The curve of voltage versus time has a good mirror symmetry, indicating that the material has good electrochemical rever...

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Abstract

The invention discloses a method for preparing a nanometer manganous-manganic oxide / carbon composite energy storage material. The method comprises the steps that potassium permanganate is reacted with oleic acid in the ratio of 100:1 (g / L) in an aqueous solution, obtained solid substances are dispersed in alcohol solvent, single substance iodine is added into the aqueous solution according to the mass ratio of 0-2:1, and the solid substances are dissolved. The solution reaction time is 12 hours-48 hours in a reaction kettle at the temperature of 120 DEG C to 200 DEG C. After centrifugal separation, washing and drying are conducted, the manganous-manganic oxide / carbon composite energy storage material is obtained. The method can be conducted on the low temperature and non-alkaline conditions and is simple in technology and low in energy consumption. Meanwhile, the super capacitive property of the manganous-manganic oxide / carbon composite energy storage material obtained according to the method is remarkably improved.

Description

technical field [0001] The invention relates to the technical field of inorganic non-metallic composite materials, in particular to a preparation method of a nanometer trimanganese tetraoxide / carbon composite energy storage material. Background technique [0002] Compared with carbon materials, manganese tetraoxide energy storage materials have the advantages of large specific capacity, high energy density, and corrosion resistance. attention. However, the conductivity of trimanganese tetroxide is low, and the electron transfer resistance is large when the redox reaction occurs in the electrolyte, so that its actual specific capacity is much lower than the theoretical specific capacity. Manganese tetraoxide is usually compounded with carbon materials to increase the electrical conductivity of the material, thereby greatly improving the specific capacity and cycle performance (Journal of Power Sources, 2002, 104: 52-61). Yin Longwei et al. (ACS Applied Materials & Interface...

Claims

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Application Information

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IPC IPC(8): H01G11/30H01G11/46H01G11/86B82Y30/00B82Y40/00
Inventor 解勤兴于泽张国庆张宗杰解超张宇峰
Owner TIANJIN POLYTECHNIC UNIV
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