Preparation method of amorphous monodisperse nano silicon dioxide powder with controllable granularity

A nano-silicon dioxide and silicon dioxide technology, applied in the direction of silicon dioxide, silicon oxide, chemical instruments and methods, etc., can solve problems such as difficult dispersion, failure to meet the requirements of nano-scale products, poor compatibility, etc., and achieve production The effect of short cycle time, low production cost, and improved dispersion

Inactive Publication Date: 2017-05-31
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, nano-SiO 2 There are hydroxyl groups on the surface of the powder, which has strong hydrophilicity, poor compatibility when mixed with organic systems, and is difficult to disperse; SiO with a particle size as small as 10-30nm 2 The powder has a higher surface energy, and the bonding strength of the agglomeration is greater. Once agglomerated, it is more difficult

Method used

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  • Preparation method of amorphous monodisperse nano silicon dioxide powder with controllable granularity
  • Preparation method of amorphous monodisperse nano silicon dioxide powder with controllable granularity
  • Preparation method of amorphous monodisperse nano silicon dioxide powder with controllable granularity

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Experimental program
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Effect test

Embodiment 1

[0031] At a constant temperature of 25°C, add 0.1g sodium dodecylsulfonate, 2.5mL ammonia water and 15mL deionized water to 50mL methanol solvent to prepare solution A; add 5mL MTMS to 50mL methanol solvent to prepare solution B Stir the above two solutions for 1 hour respectively, after mixing evenly, slowly add solution B dropwise to solution A and stir for 10 hours to form a silica sol; age the obtained silica sol in air for 24 hours to obtain a gel , dried in a freeze dryer at -40°C for 48h; the obtained product was mixed with 20mL of ethanol to form a slurry, ball milled for 5h, and dried in an oven at 50°C for 5h to finally obtain white amorphous monodisperse nano-silica with a particle size of 100nm Powder. Utilize scanning electron microscope to observe the dispersion situation of product powder, see figure 1 , indicating that the silicon dioxide silicon dioxide powder has good dispersibility.

Embodiment 2

[0033] At a constant temperature of 35°C, add 0.5mL polyethylene glycol, 2.5mL ammonia water and 10mL deionized water to 50mL methanol solvent to prepare solution A; add 5mL TMOS to 50mL methanol solvent to prepare solution B; The two solutions were stirred for 1 hour respectively, and after mixing evenly, solution B was slowly added dropwise to solution A and stirred for 10 hours to form a silica sol; the obtained silica sol was aged in the air for 24 hours to obtain a gel, which was then frozen Dry in a dryer at -40°C for 48h; mix the obtained product with 20mL of ethanol to form a slurry, ball mill for 5h, and dry in an oven at 50°C for 5h to finally obtain a white amorphous monodisperse nano-silica powder with a particle size of 50nm. Utilize scanning electron microscope to observe the dispersion situation of product powder, see figure 2 , indicating that the silica powder has good dispersibility.

Embodiment 3

[0035] At a constant temperature of 45°C, add 0.5mL CO-520, 2.5mL ammonia water and 3mL deionized water to 50mL methanol solvent to prepare solution A; add 5mL TEOS to 50mL methanol solvent to prepare solution B; The two solutions were stirred for 1 hour respectively, and after mixing evenly, solution B was slowly added dropwise to solution A and stirred for 10 hours to form a silica sol; the obtained silica sol was aged in the air for 24 hours to obtain a gel, which was then freeze-dried Dry in a machine at -40°C for 48h; mix the obtained product with 20mL of ethanol to form a slurry, ball mill for 5h, and dry in an oven at 50°C for 5h to finally obtain a white amorphous monodisperse nano-silica powder with a particle size of 30nm. Utilize scanning electron microscope to observe the dispersion situation of product powder, see image 3 , indicating that the silica powder has good dispersibility.

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Abstract

The invention discloses a preparation method of amorphous monodisperse nano silicon dioxide powder with controllable granularity and belongs to the field of an inorganic non-metal powder material. The preparation method comprises the specific steps: in a methanol solvent, selecting a silicon-containing organic matter as a silicon source and synthesizing silicon dioxide sol by utilizing an ammonia water catalyzed Stober method; ageing to obtain silicon dioxide gel; freezing and drying the gel to obtain silicon dioxide powder; mixing the powder and ethanol to form slurry and carrying out ball milling for 1h to 24h; drying in a drying oven at 50 DEG C to obtain the monodisperse amorphous silicon dioxide powder with the granularity in a range of 10nm to 100nm. A preparation process of the silicon dioxide powder is simple and the cost of the raw materials is low; large-scale industrial production of the silicon dioxide powder is easy to realize.

Description

technical field [0001] The invention belongs to the field of inorganic non-metallic powder materials, and in particular relates to a preparation method of amorphous monodisperse nano-silica powder with controllable particle size. Background technique [0002] Monodisperse nano-SiO 2 Due to its unique properties, powder is currently widely used in industrial production fields such as rubber, engineering plastics, adhesives, coatings, packaging materials, and cosmetics. In particular, 10-100nm monodisperse nano-SiO 2 The powder can be used as the precursor of lithium battery anode silicon material; while 10-30nm monodisperse nano-SiO 2 The powder has the characteristics of good insulation performance, good dispersibility, and high reflectivity to infrared light, making it an ideal material for the spacer layer of all-solid-state solar cells. [0003] Preparation of nano-SiO with high purity, narrow particle size distribution and high activity 2 Powder is the goal pursued b...

Claims

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Application Information

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IPC IPC(8): C01B33/145C01B33/12
CPCC01B33/145C01B33/126C01P2002/72C01P2004/04C01P2004/64
Inventor 谢志鹏孙思源葛一瑶田兆波张杰
Owner TSINGHUA UNIV
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