Controllable preparation method of porous silicon material by using reducing agent

A technology of porous silicon and reducing agent, applied in chemical instruments and methods, silicon compounds, hybrid/electric double layer capacitor manufacturing, etc., can solve the problems of increasing costs and achieve the effect of reducing the preparation process

Pending Publication Date: 2022-02-15
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Publication No. CN112850716A discloses a method for preparing nanoporous silicon by magnesia thermal reduction. Although the purity of the porous s...

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  • Controllable preparation method of porous silicon material by using reducing agent
  • Controllable preparation method of porous silicon material by using reducing agent
  • Controllable preparation method of porous silicon material by using reducing agent

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Embodiment 1

[0042] In this embodiment, a reducing agent can controlly prepare porous silicon material, and the steps are as follows:

[0043](1) Commercial micro-SiO and MgB with a particle size of 1-2 μm 2 Mix evenly, SiO and MgB in the mixture 2 The mass ratio is 1:1;

[0044] (2) Heat the mixture prepared in the step (1) to 800°C in an inert atmosphere of nitrogen or argon, and keep it at a constant temperature for 6h to perform a reduction reaction; then cool to room temperature under an inert atmosphere to obtain a solid product ;

[0045] (3) Etching the solid product obtained in the step (2) with dilute hydrochloric acid with a concentration of 20% by mass for 12 hours, then repeatedly washing with deionized water, and then drying to obtain a porous silicon material. Its morphology is as figure 1 shown.

Embodiment 2

[0047] This embodiment is basically the same as Embodiment 1, and the special features are:

[0048] In this embodiment, a reducing agent can controlly prepare porous silicon material, and the steps are as follows:

[0049] (1) Commercial micro-SiO and MgB with a particle size of 1-2 μm 2 Mix evenly, SiO and MgB in the mixture 2 The mass ratio is 2:1;

[0050] (2) Heat the mixture prepared in the step (1) to 900°C in an inert atmosphere of nitrogen or argon, and keep it at a constant temperature for 6h to perform a reduction reaction; then cool to room temperature under an inert atmosphere to obtain a solid product ;

[0051] (3) Etching the solid product obtained in the step (2) with dilute hydrochloric acid with a concentration of 20% by mass for 12 hours, then repeatedly washing with deionized water, and then drying to obtain a porous silicon material. Due to the insufficient amount of magnesium boride, in this embodiment only the outer layer has a porous structure, and...

Embodiment 3

[0053] This embodiment is basically the same as the previous embodiment, and the special features are:

[0054] In this embodiment, a reducing agent can controlly prepare porous silicon material, and the steps are as follows:

[0055] (1) Nano-SiO with a particle size of 200-500nm 2 with MgB 2 Evenly mixed, SiO in the mixture 2 with MgB 2 The mass ratio is 2:3;

[0056] (2) Heat the mixture prepared in the step (1) to 800°C in an inert atmosphere of nitrogen or argon, and keep it at a constant temperature for 6h to perform a reduction reaction; then cool to room temperature under an inert atmosphere to obtain a solid product ;

[0057] (3) Etching the solid product obtained in the step (2) with dilute hydrochloric acid with a concentration of 20% by mass for 12 hours, then repeatedly washing with deionized water, and then drying to obtain a porous silicon material. Its morphology is as figure 2 shown.

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Abstract

The invention relates to a controllable preparation method of a porous silicon material, which comprises the following steps: by taking silicon oxide SiOx as a main raw material and magnesium boride as a reducing agent, carrying out magnesiothermic reduction reaction to obtain a mixture of monatomic silicon, magnesium oxide and the like, and pickling to obtain the porous silicon material. The porous silicon material prepared by the preparation method disclosed by the invention retains typical morphological characteristics of an original material and shows a rich mesoporous structure. The unique adjustable porous structure not only can effectively relieve mechanical strain caused by volume change, but also is beneficial to improving transmission kinetics in an electrochemical reaction process. Meanwhile, the method has the advantages of being simple in preparation process, controllable in reaction, universal in strategy and the like. The micron/nano porous silicon material prepared by the method has potential application prospects in the field of new energy such as lithium ion batteries and the like.

Description

technical field [0001] The invention relates to a reducing agent controllable preparation of a porous silicon material and a synthesis method thereof. Background technique [0002] As an important branch of the material field, porous silicon materials have been widely used in adsorption and separation, energy storage, etc. and transformation, biomedicine and other fields. [0003] In recent years, there are many preparation methods for porous silicon, but different preparation methods and experimental conditions have a great impact on the structure and properties of porous silicon. In 1956, Uhlir of Bell Laboratories in the United States first discovered and reported the preparation of porous silicon films by electrochemical corrosion. However, the electrochemical etching method uses simple silicon as a precursor, and the manufacturing cost is high. Subsequently, researchers have successively developed a series of preparation methods for porous silicon, including chemical...

Claims

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Application Information

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IPC IPC(8): C01B33/021C01B33/023H01G11/30H01G11/86H01M4/38
CPCC01B33/023C01B33/021H01M4/38H01G11/30H01G11/86Y02E60/10
Inventor 张海娇朱冠家成慧
Owner SHANGHAI UNIV
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