CN112694093A - Low dielectric loss silicon dioxide microsphere and preparation method thereof - Google Patents
Low dielectric loss silicon dioxide microsphere and preparation method thereof Download PDFInfo
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- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
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Abstract
The invention discloses a low dielectric loss silicon dioxide microsphere and a preparation method thereof, wherein a silicon source precursor is slowly hydrolyzed and polycondensed under an acidic condition to form a copolymer, and the copolymer is converged on the surface of polystyrene powder particles to obtain silicon dioxide with a spherical morphology; drying and calcining the silicon dioxide with the spherical shape to obtain silicon dioxide hollow microspheres; and heating the silica hollow microspheres at high temperature to melt the silica hollow microspheres into spheres, and removing open pores to obtain the silica microspheres with low dielectric coefficient and low dielectric loss. According to the invention, the silicon dioxide microspheres are prepared by combining the template method and the flame fusion method, and due to the adoption of step-by-step synthesis, the requirement on quality control of products prepared by the template method is lowered, and even if the problems of poor open pore sphericity and the like exist, the hollow sphere structure with good sphericity and uniform granularity can be obtained after the balling process by the flame method, so that the prepared silicon dioxide hollow spheres have low dielectric constant and low dielectric loss.
Description
Technical Field
The invention relates to the technical field of preparation of inorganic nonmetallic materials, and particularly provides a low dielectric loss silicon dioxide microsphere and a preparation method thereof.
Background
The material is one of three major pillars of modern science and technology, and particularly, the importance of the material science is gradually highlighted nowadays when the science and technology in the world develops at a high speed. The silica material is an inorganic non-metallic material with stable chemical properties and no toxic pollution, and the silica is a raw material for manufacturing glass, quartz glass, water glass, optical fibers, important parts of the electronic industry, optical instruments, artware and refractory materials, and is an important material for scientific research. Has the characteristics of high heat conduction, low thermal expansion coefficient, low dielectric coefficient and the like.
The monodisperse spherical SiO2 has large specific surface area, small density, good dispersibility and good optical and mechanical properties, so the monodisperse spherical SiO2 has important application in the related materials and fields of biomedicine, catalysis, functional materials, high-performance ceramics, coatings, composite materials, recording materials, sensors, adsorbents, cosmetics, chromatographic column fillers, photoelectricity, data storage, medical diagnosis, immunoassay and the like
At present, various preparation methods of the silicon dioxide microspheres exist, such as a micro-emulsion method, a precipitation method, a hydrothermal method, a sol-gel method, a high-energy ball milling method and the like.
For the limitation that each preparation method is limited by respective raw materials and advantages and disadvantages, finding a preparation process of high-quality and high-efficiency silicon dioxide microspheres is still an important direction needing to be broken through and researched at present.
Disclosure of Invention
The template method takes a sphere raw material as a reagent for controlling the shape in the process, and the product is usually hollow or has a core-shell structure. The main process usually uses polystyrene microspheres as a template agent, coats the polystyrene microspheres with precursor nanoparticles, and washes the polystyrene microspheres with toluene to prepare hollow silica spheres, but the method has high requirements on the template agent, and the preparation process has many steps and is not easy to operate.
The technical task of the invention is to provide a silica microsphere with low dielectric loss and a preparation method thereof aiming at the problems.
A preparation method of silica microspheres with low dielectric loss utilizes a silicon source precursor to slowly hydrolyze and condense under an acidic condition to form a copolymer, and the copolymer is converged on the surface of polystyrene powder particles to obtain silica with a spherical morphology;
drying and calcining the silicon dioxide with the spherical shape to obtain silicon dioxide hollow microspheres;
and heating the silica hollow microspheres at high temperature to melt the silica hollow microspheres into spheres, and removing open pores to obtain the silica microspheres with low dielectric coefficient and low dielectric loss, wherein the prepared silica microspheres are good dielectric materials.
The precursor exists in a form before the target product is obtained, mostly exists in an organic-inorganic complex or mixture solid, and also exists in a sol form in part. "precursors" are specially processed batch materials used to synthesize and prepare other materials.
The flame melting method is to directly spray silicon oxide powder with irregular shape into flame to melt the silicon oxide powder into balls in the flame.
The method is realized by the following steps:
(1) preparing polystyrene powder into a template agent, adding a silicon source precursor, uniformly stirring, heating, hydrolyzing the silicon source precursor on polystyrene powder particles, and generating silicon dioxide to cover the silicon dioxide on the polystyrene powder particles;
(2) drying and calcining the reaction liquid prepared in the step (1) to prepare the silicon oxide hollow microspheres;
(3) the silicon oxide hollow microspheres are heated at the high temperature of 1700-2100 ℃, so that the hollow spheres have the appearance of good sphericity and uniform granularity.
The silicon source precursor is one or a mixture of more of tetramethoxysilane, tetraethoxysilane or calcium tetrachloride, and the concentration of the silicon source precursor is 0.01-1mol/L, and more preferably, the concentration of the silicon source precursor is 0.05-0.2 mol/L.
In the step (1), the granularity of the polystyrene powder particles is 1-10 microns, more preferably 3-8 microns, the heating temperature is 30-60 ℃, and more preferably, the reaction temperature is 40-50 ℃.
The calcination temperature in the step (2) is 500-700 ℃, and the calcination time is 2-8 h; the further preferred calcination temperature is 550-650 ℃ and the calcination time is 3-6 h.
And (4) spraying the silicon oxide hollow microspheres into a microwave plasma or oxyhydrogen flame heating facility from top to bottom to perform high-temperature heating in the step (3).
The reaction solution prepared in the step (1) is subjected to centrifugal treatment before drying and calcining;
washing with deionized water, drying, washing with toluene to remove template agent, drying, and calcining.
The process for preparing the polystyrene powder particles into the template agent in the step (1) is as follows:
and washing the polystyrene powder particles with ethanol and deionized water, dispersing the washed polystyrene powder particles in the deionized water, and adjusting the pH value to 0-6 to obtain the template agent of the polystyrene suspension.
The concentration of the polystyrene in the polystyrene suspension is 1-50mg/mL, and the concentration of the polystyrene in the polystyrene suspension is more preferably 5-20 mg/mL.
A silica microsphere with low dielectric loss, which is prepared by any one of the above methods.
Compared with the prior art, the low dielectric loss silicon dioxide microsphere and the preparation method thereof have the following outstanding beneficial effects:
according to the invention, the silicon dioxide microspheres are prepared by combining the template method and the flame fusion method, and due to the adoption of step-by-step synthesis, the requirement on quality control of products prepared by the template method is lowered, and even if the problems of poor open pore sphericity and the like exist, the hollow sphere structure with good sphericity and uniform granularity can be obtained after the balling process by the flame method, so that the prepared silicon dioxide hollow spheres have low dielectric constant and low dielectric loss.
Drawings
FIG. 1 is an electron microscope image of the hollow silica microsphere of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
A preparation method of low dielectric loss silica microspheres comprises the following steps:
(1) preparation of hollow silica particles using template method
Washing 1g of polystyrene powder with ethanol and deionized water, drying, dissolving into 30mL of deionized water, and performing ultrasonic dispersion for 30 min;
regulating the pH value of the obtained polystyrene powder dispersion to 3 by using hydrochloric acid solution, and uniformly stirring and diluting to 10 mg/mL;
adding tetramethoxysilane into the polystyrene suspension to enable the final concentration of tetramethoxysilane in the solution to reach 0.1mol/L, heating to 40 ℃, and stirring for reaction for 24 hours;
centrifuging the obtained reaction solution, washing with deionized water and drying;
and (3) washing with toluene to remove the polystyrene template, then washing with deionized water, drying, and calcining in a muffle furnace at 600 ℃ for 3h to obtain the silica particles with the hollow sphere morphology.
(2) Optimization of silica hollow spheres using flame fusion
The silicon dioxide hollow sphere particles are sprayed into microwave plasma heating equipment from top to bottom, the hollow sphere particles are rapidly cooled after being heated at 2050 ℃, defects such as open pores and the like are removed, the sphericity of the hollow sphere particles is better, and the silicon dioxide hollow microspheres with low dielectric loss, uniform granularity and good sphericity are obtained, as shown in figure 1.
Example 2
(1) Preparation of hollow silica particles using template method
Washing 1g of polystyrene powder with ethanol and deionized water, drying, dissolving into 20mL of deionized water, and performing ultrasonic dispersion for 30 min;
regulating the pH value of the obtained polystyrene powder dispersion to 5 by using hydrochloric acid solution, and uniformly stirring and diluting to 30 mg/mL;
adding tetraethoxysilane into the polystyrene suspension to enable the final concentration of the tetraethoxysilane in the solution to reach 0.15mol/L, heating to 50 ℃, and stirring for reaction for 24 hours;
centrifuging the obtained reaction solution, washing with deionized water and drying;
and (3) washing with toluene to remove the polystyrene template, washing with deionized water, drying, and calcining in a muffle furnace at 700 ℃ for 5 hours to obtain the silica particles with the hollow sphere morphology.
(2) Optimization of silica hollow spheres using flame fusion
The silicon dioxide hollow sphere particles are sprayed into microwave plasma heating equipment from top to bottom, the hollow sphere particles are rapidly cooled after being heated at 2100 ℃, defects such as open pores and the like are removed, the sphericity of the hollow sphere particles is better, and the silicon dioxide hollow microspheres with low dielectric loss, uniform granularity and good sphericity are obtained.
Example 3
(1) Preparation of hollow silica particles using template method
Washing 1g of polystyrene powder with ethanol and deionized water, drying, dissolving into 50mL of deionized water, and performing ultrasonic dispersion for 30 min;
regulating the pH value of the obtained polystyrene powder dispersion to 2 by using hydrochloric acid solution, and uniformly stirring and diluting to 50 mg/mL;
adding silicon tetrachloride into the polystyrene suspension to enable the final concentration of the silicon tetrachloride in the solution to reach 0.05mol/L, heating to 30 ℃, and stirring for reacting for 24 hours;
centrifuging the obtained reaction solution, washing with deionized water and drying;
and (3) washing with toluene to remove the polystyrene template, then washing with deionized water, drying, and calcining in a muffle furnace at 500 ℃ for 3h to obtain the silica particles with the hollow sphere morphology.
(2) Optimization of silica hollow spheres using flame fusion
The silicon dioxide hollow sphere particles are sprayed into microwave plasma heating equipment from top to bottom, the hollow sphere particles are rapidly cooled after being heated at 1800 ℃, defects such as open pores and the like are removed, the sphericity of the hollow sphere particles is better, and the silicon dioxide hollow microspheres with low dielectric loss, uniform granularity and good sphericity are obtained.
The above description is only exemplary of the present application and should not be taken as limiting the present application, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (10)
1. A preparation method of silica microspheres with low dielectric loss is characterized in that a silicon source precursor is hydrolyzed and polycondensed under acidic conditions to form a copolymer, and the copolymer is converged on the surfaces of polystyrene powder particles to obtain silica with spherical morphology;
drying and calcining the silicon dioxide with the spherical shape to obtain silicon dioxide hollow microspheres;
heating the silica hollow microspheres at high temperature to melt the silica hollow microspheres into spheres and removing open pores.
2. The method for preparing silica microspheres with low dielectric loss according to claim 1, wherein the method is realized by the following steps:
(1) preparing polystyrene powder into a template agent, adding a silicon source precursor, uniformly stirring, heating, hydrolyzing the silicon source precursor on polystyrene powder particles, and generating silicon dioxide to cover the silicon dioxide on the polystyrene powder particles;
(2) drying and calcining the reaction liquid prepared in the step (1) to prepare the silicon oxide hollow microspheres;
(3) the silicon oxide hollow microspheres are heated at the temperature of 1700-2100 ℃, so that the hollow spheres have the appearance of good sphericity and uniform granularity.
3. The method of claim 2, wherein the silicon source precursor is a mixture of one or more of tetramethoxysilane, tetraethoxysilane or calcium tetrachloride, and the concentration is 0.01-1 mol/L.
4. The method for preparing silica microspheres with low dielectric loss according to claim 2, wherein the polystyrene powder particles in the step (1) have a particle size of 1-10 μm and a heating temperature of 30-60 ℃.
5. The method as claimed in claim 2, wherein the calcination temperature in step (2) is 500-700 ℃ and the calcination time is 2-8 h.
6. The method for preparing silica microspheres with low dielectric loss according to claim 3, wherein the silica hollow microspheres in step (3) are sprayed from top to bottom into a microwave plasma or oxyhydrogen flame heating facility for high temperature heating.
7. The method for preparing silica microspheres with low dielectric loss according to any one of claims 2 to 6, wherein the reaction solution obtained in the step (1) is subjected to centrifugation treatment before drying and calcining;
washing with deionized water, drying, washing with toluene to remove template agent, drying, and calcining.
8. The method for preparing silica microspheres with low dielectric loss according to claim 7, wherein the step (1) of preparing the polystyrene powder particles into the template comprises the following steps:
and washing the polystyrene powder particles with ethanol and deionized water, dispersing the washed polystyrene powder particles in the deionized water, and adjusting the pH value to 0-6 to obtain the template agent of the polystyrene suspension.
9. The method of claim 7, wherein the polystyrene suspension contains polystyrene at a concentration of 1-50 mg/mL.
10. Silica microspheres with low dielectric losses, characterized in that they are prepared by a process according to any of the preceding claims.
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| CN113416066A (en) * | 2021-07-02 | 2021-09-21 | 广东风华高新科技股份有限公司 | LTCC substrate and preparation method and application thereof |
| CN113428867A (en) * | 2021-07-15 | 2021-09-24 | 深圳先进技术研究院 | Hollow silicon dioxide spherical particle and preparation method and application thereof |
| WO2023016242A1 (en) * | 2021-08-12 | 2023-02-16 | 广东生益科技股份有限公司 | Fluorine-containing resin-based resin composition and application thereof |
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| CN113416066A (en) * | 2021-07-02 | 2021-09-21 | 广东风华高新科技股份有限公司 | LTCC substrate and preparation method and application thereof |
| CN113428867A (en) * | 2021-07-15 | 2021-09-24 | 深圳先进技术研究院 | Hollow silicon dioxide spherical particle and preparation method and application thereof |
| WO2023016242A1 (en) * | 2021-08-12 | 2023-02-16 | 广东生益科技股份有限公司 | Fluorine-containing resin-based resin composition and application thereof |
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