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Spherical nano-silica material with dual particle size distribution and preparation method thereof

A nano-silica, double-particle size technology, applied in the direction of silica, silicon oxide, nanotechnology for materials and surface science, etc., can solve the problems of ignoring the heterogeneity and importance of monodisperse nano-silica

Active Publication Date: 2014-06-18
SHENZHEN INST OF ADVANCED TECH
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Problems solved by technology

At present, people are often committed to further improving the particle size uniformity of the prepared single-size silica by improving various preparation methods, but there is no report about the one-step preparation of spherical nano-silica materials with a double particle size distribution. The research ignores the uniqueness and importance of monodisperse nano-silica with double particle size distribution when used as a filler

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  • Spherical nano-silica material with dual particle size distribution and preparation method thereof
  • Spherical nano-silica material with dual particle size distribution and preparation method thereof
  • Spherical nano-silica material with dual particle size distribution and preparation method thereof

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preparation example Construction

[0027] see figure 1 , the preparation method of spherical nano-silica material with double particle size distribution according to one embodiment, comprising the following steps S110 to S120.

[0028] Step S110: preparing an alcohol solution containing a silicon precursor.

[0029] The silicon precursor is preferably tetraethylorthosilicate, tetramethoxysilane, butyltrimethoxysilane, tetraethoxysilane, methyltriethoxysilane, amyltriethoxysilane, tetrapropoxy silane or tetrabutoxysilane.

[0030] The silicon precursor is dissolved in an alcohol solvent to prepare an alcohol solution containing the silicon precursor. The alcoholic solvent is preferably anhydrous methanol, anhydrous ethanol, isopropanol, n-propanol, n-butanol, isobutanol or pentanol.

[0031] Preferably, the silicon precursor is dissolved in an alcohol solvent, and then placed in an ultrasonic bath for 5 minutes to 30 minutes so that the silicon precursor is evenly dispersed.

[0032] Preferably, in the alcoh...

Embodiment 1

[0056] 1. Take 5mL of tetraethyl orthosilicate, add it to 45mL of absolute ethanol, and sonicate in an ultrasonic bath for 5 minutes to obtain a uniformly dispersed ethanol solution containing tetraethyl orthosilicate; among them, tetraethyl orthosilicate The concentration is 0.45mol / L;

[0057] 2. Take 2.5mL of deionized water and 4mL of ammonia water, add them to 41mL of absolute ethanol, and sonicate in an ultrasonic bath for 5 minutes to obtain a uniformly dispersed ethanol solution containing water and ammonia water; the concentration of water is 6.0mol / L, the concentration of ammonia is 1.1mol / L;

[0058] 3. Under mechanical stirring, inject the ethanol solution containing tetraethyl orthosilicate and the ethanol solution containing water and ammonia into the reactor at the same time at the feeding speed of 2mL / min and 4mL / min respectively, and react at 30°C After 10 hours of centrifugation, the lower precipitate was washed with absolute ethanol and repeated three time...

Embodiment 2

[0061] 1. Take 5mL of tetraethyl orthosilicate, add it to 45mL of absolute ethanol, and sonicate in an ultrasonic bath for 15 minutes to obtain a uniformly dispersed ethanol solution containing tetraethyl orthosilicate; among them, tetraethyl orthosilicate The concentration is 0.45mol / L;

[0062] 2. Take 6.5mL of deionized water and 4mL of ammonia water, add them to 39.5mL of absolute ethanol, and sonicate in an ultrasonic bath for 5 minutes to obtain a uniformly dispersed ethanol solution containing water and ammonia water; the concentration of water is 10.0mol / L, the concentration of ammonia is 1.0mol / L;

[0063] 3. Under mechanical stirring, inject the ethanol solution containing tetraethyl orthosilicate and the ethanol solution containing water and ammonia water into the reactor at the same time at the feeding speed of 1mL / min and 3mL / min respectively, and react at 60°C After 4 hours, filter and wash the filter cake with absolute ethanol, vacuum-dry the filter cake at 80...

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Abstract

The invention relates to a spherical nano-silica material with dual particle size distribution and a preparation method thereof. The preparation method of the spherical nano-silica material with dual particle size distribution comprises the following steps: preparing an alcoholic solution containing a silicon precursor; preparing an alcoholic solution containing water and a catalyst; and mixing the alcoholic solution containing the silicon precursor and the alcoholic solution containing water and the catalyst to obtain a mixture, stirring the mixture to react for 4-10 hours at 25-60 DEG C, and separating and purifying to obtain the spherical nano-silica material with dual particle size distribution. Experiments prove that the preparation method of the spherical nano-silica material with dual particle size distribution can be used for preparing the spherical nano-silica material with dual particle size distribution in situ. The preparation method disclosed by the invention is simple in process and capable of preparing the spherical nano-silica material with dual particle size distribution in a large scale, so that the thermomechanical performance of an electronically-packaged composite is improved.

Description

technical field [0001] The invention relates to the technical field of preparation of nano powder materials, in particular to a spherical nano silicon dioxide material with double particle size distribution and a preparation method thereof. Background technique [0002] Due to the low coefficient of thermal expansion, nano-silica spherical powder has excellent properties such as high heat resistance, high humidity resistance and high dielectric strength, and has been widely used as a filler to fill polymer and resin matrices to reduce the thermal expansion coefficient of composite materials. . The thermal expansion coefficient of the composite material is related to the filling amount of nano-silica filler, the higher the filling amount of nano-silica, the lower the thermal expansion coefficient of the composite material. However, with the increase of the nano-silica filling amount, the viscosity of the composite system also increases accordingly, which limits the further i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18B82Y30/00
Inventor 孙蓉郭倩朱朋莉李刚
Owner SHENZHEN INST OF ADVANCED TECH
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