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Preparation method of manganous-manganic oxide-stannic oxide/cobaltosic oxide composite material

A technology of trimanganese tetraoxide and tricobalt tetraoxide, which is applied in the direction of secondary batteries, electrochemical generators, electrical components, etc., can solve the problems of difficult control of the preparation process, different sizes of products, and different shapes and products. Achieve the effect of uniform size, low cost and environmental friendliness

Active Publication Date: 2019-10-22
SHAANXI UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Currently, the preparation of SnO 2 The methods of core-shell composite materials include sol-gel method, co-precipitation method, solid-phase method, vapor-phase deposition method and hydrothermal method, etc., and the prepared morphology and products are also different, such as SnO 2 @PANI core-shell materials (Zhang F, Yang C, Gao X, et al. ACS Applied Materials & Interfaces, 2017, 9(11): 9620-9629), SnO 2 @C core-shell sphere (QiaoH, Zheng Z, Zhang L, et al. Journal of Materials Science, 2008, 43(8): 2778-2784), EG@SnO 2 @PANI core-shell materials (Yi L, Liu L, Guo G, et al. Electrochimica Acta, 2017, 240:63-71), etc., the preparation process is difficult to control, the product size is different and the dispersion is poor. Moreover, the hydrothermal method was used to prepare Mn 3 o 4 @SnO 2 / Co 3 o 4 Core-shell composites are rarely reported

Method used

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  • Preparation method of manganous-manganic oxide-stannic oxide/cobaltosic oxide composite material

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Experimental program
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Effect test

Embodiment 1

[0052] Step 1. Weigh 1mmol (158mg) of potassium permanganate (KMnO 4 ) Is dissolved in 30 mL of mixed solution (which contains N,N-dimethylformamide and deionized water, the volume ratio is 1:1), and mixes solution A of 33.3 mM under continuous stirring for 30 min.

[0053] Step 2: Transfer the obtained mixed solution A to a 50mL polytetrafluoroethylene lined hydrothermal kettle, the filling ratio is controlled at 50%, the hydrothermal temperature is 120°C, and the reaction time is 4h. After the reaction is completed, the product is centrifuged and washed three times with absolute ethanol and deionized water, and then dried in a vacuum drying oven at 40°C for 8 hours, and then ground to obtain Mn 3 O 4 Nanorod powder.

[0054] Step 3. Weigh 1.5 mmol of crystalline tin tetrachloride and dissolve it in 15 mL of deionized water to prepare a 0.1 M solution, and dropwise add 20 mL of 1.0 M sodium hydroxide solution under continuous stirring to form a mixed solution B.

[0055] Step 4. Wei...

Embodiment 2

[0058] Step 1. Weigh 2mmol (316mg) of potassium permanganate (KMnO 4 ) Dissolve in 30 mL of mixed solution (which contains N,N-dimethylformamide and deionized water, with a volume ratio of 1:1), and prepare 66.7 mM mixed solution A under continuous stirring for 30 minutes.

[0059] Step 2: Transfer the obtained mixed solution A to a 50mL polytetrafluoroethylene lined hydrothermal kettle, the filling ratio is controlled at 50%, the hydrothermal temperature is 120°C, and the reaction time is 6h. After the reaction is completed, the product is centrifuged and washed three times with absolute ethanol and deionized water, and then dried in a vacuum drying oven at 40°C for 8 hours, and then ground to obtain Mn 3 O 4 Nanorod powder.

[0060] Step 3. Weigh 3.0 mmol of crystalline tin tetrachloride and dissolve it in 15 mL of deionized water to prepare a 0.2M solution, and add 20 mL of 1.0M sodium hydroxide solution dropwise under continuous stirring to form a mixed solution B.

[0061] Step ...

Embodiment 3

[0064] Step 1. Weigh 3mmol (474mg) of potassium permanganate (KMnO 4 ) Dissolve in 30 mL of mixed solution (which contains N,N-dimethylformamide and deionized water, with a volume ratio of 1:1), and prepare a 100 mM mixed solution A under continuous stirring for 30 minutes.

[0065] Step 2: Transfer the obtained mixed solution A to a 50mL polytetrafluoroethylene lined hydrothermal kettle, the filling ratio is controlled at 50%, the hydrothermal temperature is 120°C, and the reaction time is 8h. After the reaction is completed, the product is centrifuged and washed three times with absolute ethanol and deionized water, and then dried in a vacuum drying oven at 40°C for 8 hours, and then ground to obtain Mn 3 O 4 Nanorod powder.

[0066] Step 3. Weigh 4.5 mmol of crystalline tin tetrachloride and dissolve it in 15 mL of deionized water to prepare a 0.3M solution, and add 20 mL of 1.0M sodium hydroxide solution dropwise under continuous stirring to form a mixed solution B.

[0067] Step...

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Abstract

The invention discloses a preparation method of manganous-manganic oxide-stannic oxide / cobaltosic oxide composite material. The method specifically comprises the following steps: firstly mixing potassium permanganate, N, N-dimethylformamide and deionized water, and carrying out hydrothermal reaction, washing, drying and grinding to obtain Mn3O4 nanorod powder; dissolving tin tetrachloride in deionized water; under the continuous stirring condition, dropwise adding a sodium hydroxide solution; dissolving the Mn3O4 nanorod powder into the mixed solution, stirring, carrying out ultrasonic treatment, carrying out hydrothermal reaction, washing, drying and grinding; and ispersing the Mn3O4@SnO2 core-shell structure material into the mixed solution, carrying out water bath reaction, washing, drying, grinding and calcining to obtain the Mn3O4@SnO2 / Co3O4 core-shell structure composite material for a lithium ion battery. The method is simple in preparation process, low in cost and environmentally friendly, and the obtained lithium ion battery composite material is uniform in size and good in dispersion and has excellent charging and discharging performance.

Description

Technical field [0001] The invention belongs to the technical field of composite material preparation methods, and specifically relates to a preparation method of trimanganese tetroxide-tin dioxide / cobalt tetraoxide composite material. Background technique [0002] Tin dioxide (Tin(Ⅳ)Oxide, SnO 2 ) As a widely used metal oxide semiconductor material, it is a white powder under normal conditions. Its powder is white, odorless, non-toxic, and tasteless, and its relative molecular weight is 150.69g / mol. It is a kind of semiconductor material with a wide range of uses, the specific gravity is about 6.17-7.02g / cm 2 , The melting point is about 1127℃, and it can be decomposed at higher temperature, and the boiling point is higher than 1900℃. High theoretical specific capacity 782mAh / g, compared to commercial graphite (372mAh / g), SnO 2 It has the advantages of low price, strong conductivity, good corrosion resistance and high lithium insertion capacity, and is used as a negative electro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/485H01M4/505H01M4/525H01M10/0525
CPCH01M4/364H01M4/485H01M4/505H01M4/525H01M10/0525H01M2004/021Y02E60/10
Inventor 刘辉宋洋航庞凌燕王少兰李军奇
Owner SHAANXI UNIV OF SCI & TECH