CN103288467B - A kind of composite ceramic substrate and preparation method thereof - Google Patents
A kind of composite ceramic substrate and preparation method thereof Download PDFInfo
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- CN103288467B CN103288467B CN201210050255.XA CN201210050255A CN103288467B CN 103288467 B CN103288467 B CN 103288467B CN 201210050255 A CN201210050255 A CN 201210050255A CN 103288467 B CN103288467 B CN 103288467B
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Abstract
The invention provides a kind of composite ceramic substrate and preparation method thereof, take silica fiber as supporter, the composite ceramic substrate prepared for filler of silica aerogel, this substrate not only high temperature resistant, specific inductivity is low, silica fiber is that supporter makes overall homogeneity better than common two-dimensional fiber, also can not reduce the intensity of substrate simultaneously.
Description
[technical field]
The present invention relates to Meta Materials field, particularly relate to a kind of composite ceramic substrate and preparation method thereof.
[background technology]
Meta Materials refers to some artificial composite structures with the extraordinary physical properties not available for natural materials or matrix material.By medium substrate and array, the multiple man-made microstructure on medium substrate form the basic structure of Meta Materials, the multiple man-made microstructure of array on medium substrate have specific electromagnetic property, electromagnetic response can be produced to electric field or magnetic field, by carrying out to the structure of man-made microstructure and arrangement regulation effective dielectric constant and the equivalent permeability that careful design can control each elementary cell of Meta Materials, thus the electromagnetic property making Meta Materials present various general material not have, if converge, disperse and deviation hertzian wave etc.
Existing Meta Materials man-made microstructure is generally metallic substance, and medium substrate generally adopts organic resin substrate, the specific inductivity of organic resin baseplate material is generally between 3-5, and for some application of Meta Materials, often need the material of more low-k as medium substrate, while meeting various mechanical property, be difficult to search out suitable material.
The main component of silica aerogel is SiO
2be, by sol-gel method, organic or inorganic silicon source is prepared into wet gel, then replace the liquid in gel with gas, by the control of drying control agent and drying process, keep its spacial framework substantially constant, thus obtain the silica aerogel material of nanoporous.Silica aerogel includes large quantity of air, and its porosity can reach 80% ~ 99%, and its pore size range is 1 ~ 100nm.Its nano-porous structure makes it possess many excellent electric properties, and as within the scope of 3-40GHz, can control within the scope of 1.008-2.27 by its specific inductivity by controlling its porosity, thermal expansivity is only common SiO
21/5, density is 5-200kg/m
3, can carrying capacity more than 28MPa, resistivity is for for SiO
21000 times.SiO
2the specific inductivity of aerogel is very low (1-2), thermally-stabilised good, also has insulation, lightweight, the performance such as nontoxic, fire-retardant, cheap.Good application prospect is had in low-k unleaded metamaterial substrate material.
During with pure silica aerogel for substrate, the intensity of substrate is less, can not meet processing request; Because general fibre is control of two-dimensional braided, the effect of enhancing well cannot played along the thickness direction of substrate; In addition, the specific inductivity of fiber strand and aperture sections jumps larger, and the homogeneity of whole substrate is bad.
[summary of the invention]
Technical problem to be solved by this invention is: prepare a kind of take silica fiber as supporter, that silica aerogel is filler is high temperature resistant, the composite ceramic substrate of low-k and the preparation method of composite ceramic substrate.
The technical scheme that the present invention realizes goal of the invention employing is that a kind of preparation method of composite ceramic substrate, comprises the following steps:
A, preparation hollow silica fiber: taken out after soaking paste in silicon sol by organic fibre cloth, organic fibre cloth is removed in dry, calcining, obtains the hollow silica fiber of porous surface;
B, solvent, drying control agent, performance additive are joined respectively in silicon source and form colloidal sol, add PH conditioning agent adjust ph, after colloidal sol is crosslinked, before gel, colloidal sol is injected in hollow silica fiber, then vacuumizes;
C, the silica fiber being injected with colloidal sol is left standstill, aging, then process silica fiber surface with displacer, coating materials, dry acquisition with silica fiber is the composite ceramic substrate containing aerosil of supporter.
Dry in described step a, calcining is specifically: at 55 DEG C ~ 65 DEG C at dry 1.5 ~ 2.5 hours, 100 DEG C ~ 120 DEG C dry 1.5 ~ 2.5 hours, and then calcines 5 ~ 10 hours at 600 DEG C ~ 1000 DEG C.
Described silicon source is tetraethoxy, methyl silicate, acidity or alkaline silica sol or water glass.
Described solvent is deionized water and dehydrated alcohol mixing solutions.
Described drying control agent is methane amide or ethylene glycol.
Described performance additive is titanium dioxide powder or glass fibre.
Described pH adjusting agent is hydrochloric acid or acetic acid, and the pH value of adjustment is 10 ~ 13.
Described pH adjusting agent is ammoniacal liquor, and the pH value of adjustment is 3 ~ 5.
Described displacer is ethanol or acetone.
Described coating materials is silicane coating materials.
A kind of composite ceramic substrate, the composite ceramic substrate prepared by the method described in above any one.
The invention has the beneficial effects as follows: take silica fiber as supporter, the composite ceramic substrate prepared for filler of silica aerogel, this substrate not only high temperature resistant, specific inductivity is low, silica fiber is that supporter makes overall homogeneity better than common two-dimensional fiber, also can not reduce the intensity of substrate simultaneously.
[embodiment]
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
A preparation method for composite ceramic substrate, comprises the following steps:
A, preparation hollow silica fiber: organic fibre cloth is taken out after soaking paste in silicon sol, at 55 DEG C ~ 65 DEG C at dry 1.5 ~ 2.5 hours, 100 DEG C ~ 120 DEG C dry 1.5 ~ 2.5 hours, and then calcine 5 ~ 10 hours at 600 DEG C ~ 1000 DEG C, remove organic fibre cloth, obtain the hollow silica fiber of porous surface;
B, by solvent, methane amide or the agent of ethylene glycol drying control, titanium dioxide powder or glass fibre performance additive join tetraethoxy respectively, methyl silicate, colloidal sol is formed in acidity or the silicon such as alkaline silica sol or water glass source, add pH adjusting agent adjust ph, be 10 ~ 13 when pH adjusting agent is hydrochloric acid or acetic acid adjust ph, be 3 ~ 5 when pH adjusting agent is ammoniacal liquor adjust ph, after colloidal sol is crosslinked, before gel, colloidal sol is injected in hollow silica fiber, then vacuumize and make colloidal sol enter in hollow silica fiber, and remove the bubble introduced in casting process, described solvent is deionized water and dehydrated alcohol mixing solutions,
C, the substrate in step b is left standstill, aging, then process substrate surface with ethanol or acetone displacer, silicane coating materials, dry acquisition with silica fiber is the composite ceramic substrate containing aerosil of supporter.
Take silica fiber as supporter, the composite ceramic substrate prepared for filler of silica aerogel, this substrate not only high temperature resistant, specific inductivity is low, silica fiber is that supporter makes overall homogeneity better than common two-dimensional fiber, also can not reduce the intensity of substrate simultaneously.
Also following processing method can be adopted to prepare hollow silica fiber: first by tensio-active agent, hydrochloric acid and solvent are placed in container, stirred at ambient temperature evenly also leaves standstill, and then slowly positive silicic acid propyl ester or butyl silicate silicon source is instilled in mixing solutions, silicon source, tensio-active agent, the mol ratio of hydrochloric acid and solvent is 0.02 ~ 1: 0.7: 33 ~ 85: 2300 ~ 3100, then it is 35 DEG C ~ 65 DEG C in temperature, 24 hours are reacted under static conditions, after question response completes, the cotton-shaped floating matter on solution upper strata is drained out, washing, drying obtains flocculence product, product is placed in retort furnace, be warming up to 500 DEG C and constant temperature 5 hours, remove tensio-active agent and obtain hollow silica fiber.
Embodiment one
A, preparation hollow silica fiber: organic fibre cloth is taken out after soaking paste in silicon sol, at 55 DEG C at dry 1.5 hours, 120 DEG C dry 2.5 hours, and then calcine 8 hours at 800 DEG C, remove organic fibre cloth, obtain the hollow silica fiber of porous surface;
B, by methyl silicate: deionized water: dehydrated alcohol: HCl is by 1: 3.5: 8: 8.4 × 10
-4mixed in molar ratio obtain mixing solutions, for improving the mechanical property of aerosil, add appropriate titanium dioxide powder or glass fibre as performance additive, for improving void content, also can add methane amide or ethylene glycol as drying control agent, 60 DEG C of waters bath with thermostatic control are incubated 2 hours, instillation weight fraction is the ammoniacal liquor of 1.5%, adjust ph forms colloidal sol to 3.0-3.5, after colloidal sol is crosslinked, before gel, colloidal sol is injected in hollow silica fiber, then vacuumize and make colloidal sol enter in hollow silica fiber, and remove the bubble introduced in casting process,
C, by the substrate in step b at room temperature leave standstill within 6 hours, make collosol and gel, aging 5 days in acetone, period adopts acetone displacer to carry out solvent exchange three times, remove the water in gel, then with trimethylchlorosilane coating materials, hydrophobic treatment is carried out to gel, again to dry under substrate normal temperature and pressure, remove acetone, obtaining with silica fiber is the composite ceramic substrate containing aerosil of supporter.
Embodiment two
A, preparation hollow silica fiber: organic fibre cloth is taken out after soaking paste in silicon sol, at 60 DEG C at dry 2 hours, 100 DEG C dry 2 hours, and then calcine 7 hours at 1000 DEG C, remove organic fibre cloth, obtain the hollow silica fiber of porous surface;
B, by methyl silicate: deionized water: dehydrated alcohol: HCl is by 1: 3.5: 8: 8.4 × 10
-4mixed in molar ratio obtain mixing solutions, for improving the mechanical property of aerosil, add appropriate titanium dioxide powder or glass fibre as performance additive, for improving void content, also can add methane amide or ethylene glycol as drying control agent, 70 DEG C of waters bath with thermostatic control are incubated 2.5 hours, instillation weight fraction is the ammoniacal liquor of 1.5%, adjust ph forms colloidal sol to 3.0-3.5, after colloidal sol is crosslinked, before gel, colloidal sol is injected in hollow silica fiber, then vacuumize and make colloidal sol enter in hollow silica fiber, and remove the bubble introduced in casting process,
C, by the substrate in step b at room temperature leave standstill within 6 hours, make collosol and gel, aging 5 days in acetone, period adopts acetone displacer to carry out solvent exchange three times, remove the water in gel, then with trimethylchlorosilane coating materials, hydrophobic treatment is carried out to gel, dry at normal temperatures and pressures to substrate again, remove acetone, obtain with silica fiber be supporter containing the composite ceramic substrate of aerosil.
Embodiment three
A, preparation hollow silica fiber: organic fibre cloth is taken out after soaking paste in silicon sol, at 65 DEG C at dry 2.5 hours, 110 DEG C dry 1.5 hours, and then calcine 10 hours at 600 DEG C, remove organic fibre cloth, obtain the hollow silica fiber of porous surface;
B, by methyl silicate: deionized water: dehydrated alcohol: HCl is by 1: 3.5: 8: 8.4 × 10
-4mixed in molar ratio obtain mixing solutions, for improving the mechanical property of aerosil, add appropriate titanium dioxide powder or glass fibre as performance additive, for improving void content, also can add methane amide or ethylene glycol as drying control agent, 60 DEG C of waters bath with thermostatic control are incubated 2 hours, instillation weight fraction is the ammoniacal liquor of 1.5%, adjust ph forms colloidal sol to 3.0-3.5, after colloidal sol is crosslinked, before gel, colloidal sol is injected in hollow silica fiber, then vacuumize and make colloidal sol enter in hollow silica fiber, and remove the bubble introduced in casting process,
C, by the substrate in step b at room temperature leave standstill within 6 hours, make collosol and gel, aging 5 days in acetone, period adopts acetone displacer to carry out solvent exchange three times, remove the water in gel, then with trimethylchlorosilane coating materials, hydrophobic treatment is carried out to gel, again to dry under substrate normal temperature and pressure, remove acetone, obtaining with silica fiber is the composite ceramic substrate containing aerosil of supporter.
In the above-described embodiments, only to invention has been exemplary description, but those skilled in the art can carry out various amendment to the present invention without departing from the spirit and scope of the present invention after reading present patent application.
Claims (11)
1. a preparation method for composite ceramic substrate, is characterized in that: comprise the following steps:
A, preparation hollow silica fiber: taken out after soaking paste in silicon sol by organic fibre cloth, organic fibre cloth is removed in dry, calcining, obtains the hollow silica fiber of porous surface;
B, solvent, drying control agent, performance additive are joined respectively in silicon source and form colloidal sol, add pH adjusting agent adjust ph, after colloidal sol is crosslinked, before gel, colloidal sol is injected in hollow silica fiber, then vacuumizes and make colloidal sol enter in hollow silica fiber;
C, the silica fiber being injected with colloidal sol is left standstill, aging, then process silica fiber surface with displacer, coating materials, dry acquisition with silica fiber is the composite ceramic substrate containing aerosil of supporter.
2. the preparation method of composite ceramic substrate according to claim 1, it is characterized in that: dry in described step a, calcining specifically: at 55 DEG C ~ 65 DEG C at dry 1.5 ~ 2.5 hours, 100 DEG C ~ 120 DEG C dry 1.5 ~ 2.5 hours, and then calcine 5 ~ 10 hours at 600 DEG C ~ 1000 DEG C.
3. the preparation method of composite ceramic substrate according to claim 1, is characterized in that: described silicon source is tetraethoxy, methyl silicate, acidity or alkaline silica sol or water glass.
4. the preparation method of composite ceramic substrate according to claim 1, is characterized in that: described solvent is deionized water and dehydrated alcohol mixing solutions.
5. the preparation method of composite ceramic substrate according to claim 1, is characterized in that: described drying control agent is methane amide or ethylene glycol.
6. the preparation method of composite ceramic substrate according to claim 1, is characterized in that: described performance additive is titanium dioxide powder or glass fibre.
7. the preparation method of composite ceramic substrate according to claim 1, is characterized in that: described pH adjusting agent is hydrochloric acid or acetic acid, and the pH value of adjustment is 10 ~ 13.
8. the preparation method of composite ceramic substrate according to claim 1, is characterized in that: described pH adjusting agent is ammoniacal liquor, and the pH value of adjustment is 3 ~ 5.
9. the preparation method of composite ceramic substrate according to claim 1, is characterized in that: described displacer is ethanol or acetone.
10. the preparation method of composite ceramic substrate according to claim 1, is characterized in that: described coating materials is silicane coating materials.
11. 1 kinds of composite ceramic substrates, is characterized in that: comprise composite ceramic substrate prepared by the method described in claim 1-10 any one.
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| CN1749214A (en) * | 2005-08-01 | 2006-03-22 | 中国人民解放军国防科学技术大学 | Aerogel heat insulation composite material and its preparing method |
| CN101698584A (en) * | 2009-11-13 | 2010-04-28 | 航天特种材料及工艺技术研究所 | Fiber-reinforcement silicon dioxide aerogel continuous felt and preparation method thereof |
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| CN1749214A (en) * | 2005-08-01 | 2006-03-22 | 中国人民解放军国防科学技术大学 | Aerogel heat insulation composite material and its preparing method |
| CN101698584A (en) * | 2009-11-13 | 2010-04-28 | 航天特种材料及工艺技术研究所 | Fiber-reinforcement silicon dioxide aerogel continuous felt and preparation method thereof |
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Effective date of registration: 20210414 Address after: 2 / F, software building, No.9, Gaoxin Zhongyi Road, Nanshan District, Shenzhen City, Guangdong Province Patentee after: KUANG-CHI INSTITUTE OF ADVANCED TECHNOLOGY Address before: 18B, building a, CIC international business center, 1061 Xiangmei Road, Futian District, Shenzhen, Guangdong 518034 Patentee before: KUANG-CHI INNOVATIVE TECHNOLOGY Ltd. |
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