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Preparation method of low-dielectric hollow silicon dioxide microspheres

A hollow silica, low dielectric technology, applied in the field of non-metallic materials, can solve the problems of many influencing factors, complicated structure control, difficult to obtain particle size, etc., to reduce energy consumption, not easily deformed and cracked, and the surface dense effect

Active Publication Date: 2021-12-21
SUZHOU GINET NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because of its too many influencing factors, its structure control is complicated
Therefore, it is difficult to obtain hollow microspheres with uniform particle size and uniform wall thickness by this method.

Method used

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  • Preparation method of low-dielectric hollow silicon dioxide microspheres
  • Preparation method of low-dielectric hollow silicon dioxide microspheres
  • Preparation method of low-dielectric hollow silicon dioxide microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Step 1.1, 1.5g polyvinylpyrrolidone, 45g ethanol, 5g distilled water, 15g styrene, 0.29g initiator azobisisobutyronitrile were dissolved for 10min and then loaded into a 250mL three-necked flask (including nitrogen inlet, stirring paddle inlet and condensation mouth), stirred at room temperature to form a homogeneous solution;

[0042] Step 1.2, deoxidize the homogeneous solution by bubbling nitrogen gas at room temperature for 30 minutes, then heat to 70°C and continue stirring for 24 hours to obtain a polystyrene sphere dispersion;

[0043] In step 1.3, add 10 g of methyltrimethoxysilane to 50 ml of water and mix evenly, then add hydrochloric acid after heating up to 35°C, adjust the pH to 3, and continue stirring for 3 hours to obtain the hydrolyzed solution of the organosilane precursor;

[0044] Step 1.4, add 2g of cetyltrimethylammonium bromide (CTAB) and 3ml of ammonia water to the polystyrene sphere dispersion obtained in step 1.2, stir for 6min, add the organos...

Embodiment 2

[0048] Step 2.1, after ultrasonically dissolving 1.5g polyvinylpyrrolidone, 45g ethanol, 5g distilled water, 15g styrene, 0.29g initiator azobisisobutyronitrile and cationic comonomer acryloxyethyltrimethylammonium chloride for 10min Pack into a 250 mL three-necked flask (including nitrogen inlet, stirring paddle inlet and condensation outlet), and stir at room temperature to form a homogeneous solution;

[0049] Step 2.2, deoxidize the homogeneous solution by bubbling nitrogen gas at room temperature for 30 minutes, then heat to 70°C and continue stirring for 24 hours to obtain a positively charged polystyrene sphere dispersion;

[0050] In step 2.3, add 5 g of methyltrimethoxysilane to 50 ml of water and mix evenly. After heating up to 35° C., add hydrochloric acid, adjust the pH to 3, and continue stirring for 3 hours to obtain the hydrolyzed solution of the organosilane precursor;

[0051] Step 2.4, add 3ml of ammonia water to the polystyrene sphere dispersion obtained in ...

Embodiment 3

[0055] Step 3.1, 1.5g polyvinylpyrrolidone, 45g ethanol, 5g distilled water, 15g styrene, 0.29g initiator azobisisobutyronitrile and cationic comonomer acryloxyethyltrimethylammonium chloride were ultrasonically dissolved for 10min Pack into a 250 mL three-necked flask (including nitrogen inlet, stirring paddle inlet and condensation outlet), and stir at room temperature to form a homogeneous solution;

[0056] Step 3.2, deoxidize the homogeneous solution by bubbling nitrogen gas at room temperature for 30 minutes, then heat to 70°C and continue stirring for 24 hours to obtain a positively charged polystyrene sphere dispersion;

[0057] In step 3.3, add 8 g of methyltrimethoxysilane to 50 ml of water and mix evenly, then add hydrochloric acid after heating up to 35° C., adjust the pH to 3, and continue stirring for 3 hours to obtain the hydrolyzed liquid of the organosilane precursor;

[0058] Step 3.4, add 3ml of ammonia water to the polystyrene sphere dispersion obtained in ...

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Abstract

The invention provides a preparation method of a low-dielectric hollow silicon dioxide microsphere, which comprises the following steps: taking polystyrene as a template of a hollow microsphere, adding a cationic comonomer acryloyloxyethyl trimethyl ammonium chloride (DAC), and introducing a positive charge group to a polymer chain to prepare a positively charged polystyrene sphere. The method does not need to add an activating agent, so that the surface of the sphere is positively charged to attract the silicon source to uniformly coat the template. Through the calcining method provided by the invention, a compact sphere structure can be obtained. According to the method for preparing the silicon dioxide microspheres through the template method, the prepared microspheres are high in pelletizing rate, compact, not prone to being broken and low in dielectric constant, and the modulus and heat resistance of a substrate are improved, so that the silicon dioxide microspheres are particularly suitable for the requirements of the copper-clad plate industry.

Description

technical field [0001] The invention relates to the technical field of non-metallic materials, in particular to a method for preparing hollow silicon dioxide microspheres by using styrene polymerization to prepare polystyrene microspheres as a template body. Background technique [0002] Hollow silica microspheres are composed of nanoparticles, with a size ranging from nanometers to micrometers, and a multi-scale and multi-level nanostructure with hollow cavities. Compared with corresponding bulk materials, it has larger specific surface area, lower density, special mechanical, optical, electrical and other physical properties and application value. [0003] As a nano-scale inorganic material, silica microspheres have excellent characteristics such as low density, low thermal expansion coefficient, high insulation, low dielectric constant, and stable chemical properties in the fillers used in copper clad laminates, and have a very broad application field. Especially in the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18
CPCC01B33/18C01P2004/34C01P2004/64C01P2004/62C01P2004/61C01P2004/03C01P2006/40C01B33/12
Inventor 尹亚玲郑海涛沈晓燕
Owner SUZHOU GINET NEW MATERIAL TECH CO LTD
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