Preparation method of low-cost nano-porous silica powder

A nanoporous, low-cost technology, applied in nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of poor controllability of pore structure, high heating temperature, small pores, etc., and achieve short reaction time and material structure. Control, low cost effect

Inactive Publication Date: 2017-05-17
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method is simpler than other methods, the heating temperature is higher, the pores are smaller, and the controllability of the pore structure is poor.

Method used

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  • Preparation method of low-cost nano-porous silica powder

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Embodiment 1

[0030] The preparation method of porous silicon described in this embodiment specifically includes the following steps:

[0031] (1) Pretreatment of silicon powder: Soak and clean silicon powder (metallurgical grade silicon, particle size less than or equal to 500 μm) with 5wt% hydrofluoric acid (that is, 5% HF aqueous solution) for 10 minutes, and filter with deionized water Wash 3 times and dry;

[0032] (2) Etching of silicon powder: place silicon powder in HF, Cu(NO 3 ) 2 , ethanol and water, the concentration of HF in the mixed solution is 5mol / L, Cu(NO 3 ) 2 The concentration of the mixture is 0.06mol / L, the mass percentage of ethanol is 1%, react at room temperature 25°C for 20min, and magnetically stir at the same time (stirring speed is 300r / min), to obtain porous silicon particles;

[0033] (3) processing of silicon powder: the porous silicon particles obtained in (2) step are placed in 10% nitric acid aqueous solution and soaked for 1 hour (the mass percentage o...

Embodiment 2

[0036] The preparation method of porous silicon described in this embodiment specifically includes the following steps:

[0037] (1) Pretreatment of silicon powder: soak and clean silicon powder (metallurgical grade silicon) with 5wt% HF for 10 minutes, wash with deionized water for 3 times after filtering, and dry;

[0038] (2) Etching of silicon powder: place silicon powder in HF, Cu(NO 3 ) 2 , ethanol and water, the concentration of HF in the mixed solution is 5mol / L, Cu(NO 3 ) 2 The concentration is 0.12mol / L, ethanol is 10%, react at room temperature 25°C for 20min, and magnetic stirring is carried out at the same time (stirring speed is 300r / min), to obtain porous silicon particles;

[0039] (3) Treatment of silicon powder: soak the porous silicon particles obtained in step (2) in 10% nitric acid solution for 1 hour, and at the same time perform ultrasonic cleaning on the porous silicon to remove impurities to obtain porous silicon.

[0040](4) Cleaning of porous sil...

Embodiment 3

[0042] The preparation method of porous silicon described in this embodiment specifically includes the following steps:

[0043] (1) Pretreatment of silicon powder: soak and clean silicon powder (metallurgical grade silicon) with 5wt% HF for 10 minutes, wash with deionized water for 3 times after filtering, and dry;

[0044] (2) Etching of silicon powder: place silicon powder in HF, Fe(NO 3 ) 3 , ethanol and water, the concentration of HF in the mixed solution is 5mol / L, Fe(NO 3 ) 3 The concentration is 0.24mol / L, ethanol is 15%, react at normal temperature 25 ℃ for 30min, carry out magnetic stirring simultaneously (stirring speed is 300r / min), obtain porous silicon particle;

[0045] (3) Treatment of silicon powder: soak the porous silicon particles obtained in step (2) in 10% nitric acid aqueous solution for 1 hour, and ultrasonically clean the porous silicon to remove impurities to obtain porous silicon.

[0046] (4) Cleaning of porous silicon: the porous silicon obtain...

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Abstract

The invention discloses a preparation method of low-cost nano-porous silica powder. The method comprises the following steps of etching of silica powder, namely etching the pretreated silica powder by using an etchant, etching for 1-600 minutes to obtain porous silicon containing nanoscale channels, wherein the apertures are 1-1,000nm and the etchant is a mixed solution prepared from HF, a metal salt, ethanol and water; and treatment of the silica powder, soaking the porous silicon containing nanoscale channels into an acid solution for soaking, and cleaning and removing impurities to obtain the nano-porous silica powder. According to the preparation method, the metal salt is introduced as the etchant, and the shape and form, the aperture, the pore-forming speed and the like of the porous silica powder can be controlled through controlling the concentration of a corrosive solution. Preparation of porous silicon is achieved by using reaction heat release at a room temperature, heating equipment is avoided, meanwhile, the reaction speed is high and the porous silicon can be prepared within a few of minutes in general.

Description

technical field [0001] The invention relates to the technical field of porous nano functional materials, in particular to a preparation method of low-cost nano porous silicon powder. Background technique [0002] As early as 1956, Uhlir of Bell Laboratories in the United States first discovered and reported that porous silicon films could be formed by electrochemical corrosion. Since the discovery of porous silicon, porous silicon has been widely used in biological and chemical sensors, photocatalysis, energy, supercapacitors, bioimaging, drug delivery and other fields. [0003] At present, there are many methods for preparing porous silicon at home and abroad, but they can be generally classified into electrochemical methods, photochemical etching methods, etching methods and hydrothermal etching methods. At present, the relatively mature preparation methods of porous silicon include anodic electrochemical etching method, magnesia thermal reduction method, and hydrothermal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/021B82Y30/00
CPCC01B33/021C01P2004/03C01P2004/61C01P2006/16
Inventor 汪雷唐勋刘友博张军娜蔡辉杨德仁
Owner ZHEJIANG UNIV
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