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A method for preparing nano-silicon based on halloysite raw material

A technology of nano-silicon and nano-silicon dioxide, applied in the direction of nanotechnology, nanotechnology, nanotechnology, etc. for materials and surface science, can solve the unfavorable large-scale production of nano-silicon materials, the inability to obtain nano-silicon materials, high Toxicity and other issues can be achieved to improve the nano-silicon morphology, uniform pore size distribution, and reduce the reaction temperature

Active Publication Date: 2018-03-30
湖南宸宇富基新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These preparation methods generally have the disadvantages of high cost, high toxicity and low yield, which are not conducive to large-scale production of nano-silicon materials.
Metallurgical silicon prepared by traditional carbothermal reduction cannot obtain nano-silicon materials due to high temperature

Method used

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  • A method for preparing nano-silicon based on halloysite raw material
  • A method for preparing nano-silicon based on halloysite raw material
  • A method for preparing nano-silicon based on halloysite raw material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] (1) Take 5g of halloysite and add it to 500mL of sulfuric acid solution with a concentration of 2mol / L, react at 100°C for 10h, filter and wash with water until neutral, and dry in an oven at 80°C to obtain the desired silica intermediate product .

[0052] (2) Take the above 1g of silicon dioxide, mix it with 10g of sodium chloride, add 0.9g of metal magnesium powder, place it in a sealed tube furnace, raise the temperature to 700°C at 5°C / min and keep it for 10h under an argon atmosphere. After cooling, the product was treated in 1mol / L hydrochloric acid for 6h, filtered and then treated in 5wt% hydrofluoric acid for 0.5h, filtered and washed to neutrality, and dried at 80°C to obtain a nano-silicon material. The X-ray diffraction pattern is as follows Figure 4 As shown, the scanning electron microscope as Figure 5 As shown, the transmission electron microscope is shown as Figure 6 As shown, the pore size distribution is as Figure 7 As shown, the nitrogen adsor...

Embodiment 2

[0055] (1) Take 5g of halloysite and add it to 500mL of hydrochloric acid solution with a concentration of 1mol / L, react at 90°C for 12h, filter and wash with water until neutral, and dry in an oven at 80°C to obtain the desired silica intermediate product .

[0056] (2) Take the above 1g of silicon dioxide, mix it with 5g of sodium chloride and 5g of potassium chloride, then add 0.8g of metal magnesium powder, place it in a sealed tube furnace, and raise the temperature at 2°C / min to Insulate at 650°C for 10h, after cooling, the product is treated in 2mol / L hydrochloric acid for 6h, filtered and then treated in 10wt% hydrofluoric acid for 0.5h, filtered and washed with water until neutral, dried at 80°C to obtain the morphology of Example 1 The same nano-silicon material.

[0057] The prepared material was made into a negative electrode sheet of a lithium ion battery according to the method in Example 1, and a simulated battery was assembled. Under the current density of 20...

Embodiment 3

[0059] (1) Add 5g of halloysite to 300mL of sulfuric acid solution with a concentration of 3mol / L, react at 120°C for 5h, filter and wash with water until neutral, and dry in an oven at 80°C to obtain the desired silica intermediate product .

[0060] (2) Take the above 1g of silicon dioxide, mix it with 20g of potassium chloride, add 1g of metal magnesium powder, put it in a sealed tube furnace, heat it up to 1000°C at 10°C / min under an argon atmosphere and keep it warm for 6h, then cool The final product was treated in 1mol / L sulfuric acid for 12h, filtered and then treated in 5wt% hydrofluoric acid for 1h, filtered and washed with water until neutral, and dried at 80°C to obtain a nano-silicon material with the same appearance as Example 1.

[0061] The prepared material was made into a negative electrode sheet of a lithium ion battery according to the method in Example 1, and a simulated battery was assembled. Under the current density of 200mA / g, the prepared battery com...

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Abstract

The invention discloses a method of preparing nano silicon on the basis of a halloysite raw material. The method includes the steps of: with halloysite clay as a raw material, acid-pickling the halloysite clay to obtain nano silicon dioxide, and mixing the nano silicon dioxide as a precursor with magnesium powder, and performing magnesiothermic reduction to prepare nano silicon particles having regular morphology with reaction conditions controlled. The halloysite has a nano tubular structure, so that an acid solution is easy to permeate the halloysite, thereby accelerating the acid pickling reaction. The magnesiothermic reduction process has low temperature, so that the micro-structure of a reaction product can be maintained. The nano silicon particle has uniform appearance and morphology, uniform pore diameter distribution, high specific surface are and low production cost. The method, with the natural halloysite clay as the raw material, is low in cost, is easy to amplified in production and has a wide application prospect in the fields such as lithium ion battery materials.

Description

technical field [0001] The invention belongs to the field of inorganic nanometer materials, and in particular relates to a method for preparing nanometer silicon based on halloysite raw materials. Background technique [0002] Halloysite (Al 2 Si 2 o 5 (OH) 4 2H 2 O) is a natural nanomaterial that can be mined from ore deposits, and halloysite presents a nanotube structure in microscopic appearance. Compared with kaolin, halloysite has an extra layer of water molecules between the alumina layer and the silica layer, resulting in a tubular structure of halloysite, so halloysite is also called halloysite. Traditionally, halloysite is mainly used in the production of ceramic products. In recent years, with the rapid development of nanoscience and technology, the application fields of natural halloysite nanotubes have been continuously expanded. For example, researchers have made good achievements in using halloysite in sewage treatment and biopharmaceutical fields. Natur...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/021C01B33/023B82Y30/00
CPCB82Y30/00C01B33/021C01B33/023C01P2002/72C01P2004/03C01P2004/04C01P2004/64C01P2006/12C01P2006/16
Inventor 杨娟周向阳吴李力唐晶晶席利华王标
Owner 湖南宸宇富基新能源科技有限公司
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