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Preparation method of porous hollow micro-cube blocky tin dioxide

A tin dioxide and cubic technology is applied in the field of preparation of porous hollow micro-cube-shaped tin dioxide, which can solve the problem that the control of tin dioxide nanocrystals cannot be realized, the structure pulverization cannot be well solved, and the cycle performance is not good. and other problems, to achieve the effect of solving the problem of structure pulverization, large specific capacity and good product quality

Inactive Publication Date: 2013-11-20
ANHUI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When it is used as a lithium battery negative electrode material, it has a certain specific capacity and cycle performance, but the cycle performance is not good. This is mainly because, as can be seen from its scanning electron microscope photos, the nano-hollow nanorods composed of tin dioxide nanorods Balls, the cavity in the center of the material is not large, which cannot solve the problem of structural pulverization well, and also restricts its storage capacity
From the perspective of material synthesis, this method is still unable to achieve the control of the morphology and microstructure of tin dioxide nanocrystals

Method used

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  • Preparation method of porous hollow micro-cube blocky tin dioxide
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Embodiment 1

[0029] A preparation method of porous hollow micron cubic tin dioxide powder, the steps comprising:

[0030] A, mixing process: dissolving tin tetrachloride pentahydrate in water, then adjusting the pH of the solution to 12.5 with 5.0mol / L sodium hydroxide, preparing 30 milliliters of 0.0005mol / L sodium stannate solution; dissolving cobalt chloride Prepare 15 ml of 0.001mol / L cobalt chloride solution in water; mix the above-mentioned solutions and heat in a water bath at 60°C for 40 minutes, stir to obtain a cloudy solution; place the obtained cloudy solution at 25°C for aging After 12 hours, the precipitate was filtered, washed, and dried to obtain a solid cobalt hydroxystannate precursor in the form of micron cubes;

[0031] The stirring uses magnetic stirring, and the rotating speed is 15 rpm;

[0032] B. Conversion process: transform the precursor powder obtained in step A with 3 mol / L sodium hydroxide solution whose mass is 200 times that of the precursor powder at 10°C ...

Embodiment 2

[0036] A preparation method of porous hollow micron cubic tin dioxide powder, the steps comprising:

[0037] A, mixing process: sodium stannate is dissolved in water, and then the pH value of the solution is adjusted to 12.5 with 5.0mol / L potassium hydroxide to obtain 30 milliliters of 0.05mol / L sodium stannate solution; cobalt nitrate is dissolved in water to prepare 15 milliliters of 0.2mol / L cobalt chloride solution were obtained; the above-mentioned solution was mixed and heated in a water bath at 50°C for 80 minutes, and stirred to obtain a cloudy solution; the obtained cloudy solution was allowed to stand and age at 30°C for 4 hours, and then The precipitate is filtered, washed, and dried to obtain a solid micron cubic cobalt hydroxystannate precursor;

[0038] The stirring uses magnetic stirring, and the rotating speed is 80 rpm;

[0039] B. Transformation process: transform the precursor powder obtained in step A with a 4mol / L potassium hydroxide solution whose mass is ...

Embodiment 3

[0043] A preparation method of porous hollow micron cubic tin dioxide powder, the steps comprising:

[0044] A. Mixing process: Dissolve sodium stannate in water, then adjust the pH of the solution to 13.5 with 5.0mol / L sodium hydroxide to obtain 30 milliliters of 0.5 mol / L sodium stannate solution; dissolve cobalt chloride in water to prepare 15 milliliters of 1mol / L cobalt chloride solution were obtained; the above-mentioned solution was mixed and heated in a water bath at 60° C. for 50 minutes, and stirred to obtain a cloudy solution; the obtained cloudy solution was left to age at 80° C. for 6 hours, and then The precipitate is filtered, washed, and dried to obtain a solid micron cubic cobalt hydroxystannate precursor;

[0045] The stirring uses magnetic stirring, and the rotating speed is 50 rpm;

[0046] B. Conversion process: convert the precursor powder obtained in step A with a 5 mol / L sodium hydroxide solution whose mass is 100 times that of the precursor powder at ...

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Abstract

The invention discloses a preparation method of porous hollow micro-cube blocky tin dioxide. The preparation method comprises the following steps of: mixing and ageing procedure, conversion procedure, calcining procedure and acid washing procedure of tin salt and cobalt salt. The porous hollow micro-cube blocky tin dioxide powder product prepared by the preparation method is large in specific surface area (30-80m<2> / g) and high in purity, does not contain other shapes, is homogeneous in structure, uniform in size distribution and stable in performance, is not easily denatured in air and is good in quality; and the preparation method has the advantages of simple process and low cost.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, and in particular relates to a method for preparing porous hollow micron cubic tin dioxide. Background technique [0002] Tin dioxide is an important n-type broadband (Eg=3.6eV, 300K) semiconductor material, which is widely used in the field of lithium-ion batteries. Compared with the currently used graphite (372mAh / g) electrode, tin dioxide has a higher theoretical storage capacity (790mAh / g) when it is used as the negative electrode of lithium-ion batteries. However, when tin dioxide undergoes lithium intercalation and delithiation reactions, accompanied by huge volume expansion and contraction, the electrode will be pulverized and cracked, which will deteriorate the cycle performance of the battery. [0003] As we all know, at the nanometer scale, the shape, size, specific surface area of ​​materials and their performance are closely related. The performance determines the ap...

Claims

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Application Information

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IPC IPC(8): C01G19/02
Inventor 黄家锐史诚诚谷翠萍汪丽友
Owner ANHUI NORMAL UNIV
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