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Preparation method of three-dimensional porous silica powder

A technology of three-dimensional porous and porous silicon, which is applied in electrical components, battery electrodes, nanotechnology, etc., can solve the problems of low production cost, harsh preparation process, and restrictions on the large-scale commercial application of powdery porous silicon, and achieve operational Ease, simple equipment effect

Active Publication Date: 2015-03-25
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the reaction process of preparing porous silicon by magnesia thermal reduction is simple, the reaction needs to be carried out in a high-temperature environment protected by an inert atmosphere. The harsh preparation process and low preparation cost greatly limit the large-scale commercialization of powdered porous silicon. application

Method used

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  • Preparation method of three-dimensional porous silica powder

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Embodiment 1

[0022] The preparation method of the three-dimensional porous silicon powder described in this embodiment specifically includes the following steps (such as figure 1 said):

[0023] (1) Pretreatment of silicon material: The bulk silicon material (metallurgical grade silicon, silicon purity: 98.8wt%) was crushed and ground (38~75μm), washed with deionized water for 5 times, and then washed with 5wt% HF Soak the cleaned silicon powder for 40min, and dry it for later use;

[0024] (2) Etching of silicon powder: A one-step metal nanoparticle-assisted etching method was used at 10 °C, and the silicon powder was placed in HF acid and AgNO. 3 In the mixed solution (the liquid-solid ratio of silicon material and etching solution is 5:1), the concentration of HF in the mixed solution is 0.1mol / L, AgNO 3 The concentration of silicon dioxide was 10 mol / L, and the reaction system was placed in a dark room and stirred (rotation speed: 120 rpm) for 50 min to obtain large-scale silicon par...

Embodiment 2

[0028] The preparation method of the three-dimensional porous silicon powder described in this embodiment specifically includes the following steps:

[0029] (1) Pretreatment of silicon material: The bulk silicon material (solar grade polysilicon, silicon purity: 99.99wt%) was crushed and ground (38~75μm), washed with deionized water for 5 times, and then washed with 20wt% HF Soak the cleaned silicon powder for 1min, and dry it for later use;

[0030] (2) Etching of silicon powder: a one-step metal nanoparticle-assisted etching method was used at 50 °C, and the silicon powder was placed in HF acid and KAuCl. 4 In the mixed solution (the liquid-solid ratio of silicon material and etching solution is 6:1), the concentration of HF in the mixed solution is 33mol / L, KAuCl 4 The concentration of silicon dioxide was 0.001 mol / L, and the reaction system was stirred (rotation speed: 120 rpm) for 600 min to obtain large-scale silicon particles containing nano-scale pores;

[0031] (3)...

Embodiment 3

[0034] The preparation method of the three-dimensional porous silicon powder described in this embodiment specifically includes the following steps:

[0035] (1) Pretreatment of silicon material: The bulk silicon material (single crystal silicon, silicon purity > 99.99999wt%) is crushed and ground (38~75μm), washed with deionized water for 5 times, and then washed with 30wt% HF Soak the cleaned silicon powder for 20min, and dry it for later use;

[0036] (2) Etching of silicon powder: a one-step metal nanoparticle-assisted etching method was used at 20 °C, and the silicon powder was placed in HF acid and H 2 PtCl 6 In the mixed solution (the liquid-solid ratio of silicon material and etching solution is 6:1), the concentration of HF in the mixed solution is 18mol / L, H 2 PtCl 6 The concentration of silicon dioxide was 4 mol / L, and the reaction system was stirred (rotation speed: 120 rpm) for 500 min to obtain large-scale silicon particles containing nano-scale pores;

[003...

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Abstract

The invention discloses a preparation method of three-dimensional porous silica powder, relates to a porous nanometer function material and belongs to the field of preparation of porous nanometer function materials. Silica powder with different purities fume is taken as a raw material, and metal nanoparticles (Ag, Au, Pd, Pt, Cu and the like) taken as catalysts are introduced on the surface of the silica Powder; in a reaction system with HF acid and an oxidizing agent, an MACE (metal-assisted chemical etching) method is adopted, and the porous silica powder with different pore structures and porosities is prepared under the room temperature condition. Compared with a traditional electrochemistry anode etching method, a magnesiothermic reduction method and the like, the method provided by the invention has the advantages of avoiding expensive single crystal silicon raw materials, harsh high-temperature reaction equipment and operation, being simple in equipment, easy in operation, low in cost, controllable in material structure and suitable for large-scale industrial production, and the like. The preparation method of the three-dimensional porous silica powder has wide application prospect in the fields of lithium ion batteries, photoelectric materials, biomedicine, sensors and the like.

Description

technical field [0001] The invention relates to a preparation method of three-dimensional porous silicon powder, which belongs to the field of preparation of porous nanometer functional materials. Background technique [0002] In 1956, Ulhir of Bell Labs in the United States discovered porous silicon by accident while studying the electrochemical polishing of silicon. Until 1990, British scientist Canham reported that the porous film exhibited strong and broad visible photoluminescence under UV excitation, which attracted extensive attention to porous silicon. As a new type of semiconductor material, porous silicon is widely used in photoluminescence devices, photodetectors, biomedicine and other fields due to its huge specific surface area, good biocompatibility, unique optoelectronic properties and active surface chemical structure. New energy materials and many other fields show broad application prospects. [0003] At present, the preparation methods of porous silicon ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/1395H01M4/38B82Y40/00
CPCH01M4/1395H01M4/386B82Y40/00Y02E60/10
Inventor 马文会李绍元周阳魏奎先于洁杨斌戴永年
Owner KUNMING UNIV OF SCI & TECH
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