CN101591192B - Reinforcement method for fibre-quartz ceramic-base composite material - Google Patents
Reinforcement method for fibre-quartz ceramic-base composite material Download PDFInfo
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- CN101591192B CN101591192B CN200810159027XA CN200810159027A CN101591192B CN 101591192 B CN101591192 B CN 101591192B CN 200810159027X A CN200810159027X A CN 200810159027XA CN 200810159027 A CN200810159027 A CN 200810159027A CN 101591192 B CN101591192 B CN 101591192B
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Abstract
The invention relates to a reinforcement method for a fibre-quartz ceramic-base composite material, and belongs to the technical field of inorganic materials. The composite material relates to a wave-transmitting material, and the finished product of the composite material is prepared by the following steps: carrying out sol reinforced infiltration treatment of a composite material body prepared through liquid-phase filtration-in situ solidifying molding; and finally, carrying out gel formation and solidification. The sol slurry comprises the following compositions by mol percentage: 10 to 50percent of analytically pure anhydrous ethanol, 6 to 20 percent of analytically pure tetraethyl orthosilicate, 30 to 70 percent of distilled water and 6 to 20 percent of acetylacetone or glycerol. The reinforcement method has the advantages that the method not only can increase material density and improve material density uniformity, but also can reinforce the bonding force among SiO2 powder granules, remarkably improve the overall performance of the composite material, and meet the requirements of a high Mach number antenna housing on material performance.
Description
Technical field
The present invention relates to a kind of Enhancement Method of fibre-quartz ceramic-base composite material, belong to technical field of inorganic material, be a kind of electromagnetic wave transparent material.
Background technology
As far back as 50～sixties of 20th century, abroad just begun fabric composite study and application successively are used widely in multinomial Aeronautics and Astronautics engineering parts such as nose cone, heat-protection layer, antenna windows, radome.The fiber that can be used for wave-penetrating composite material at present mainly is divided into silica fiber, sapphire whisker and boron nitride fibre etc., and the matrix of matrix material mainly contains inorganic and organic two big classes.Table 1 is the performance perameter of several radomes silica fiber composite inorganic material commonly used.
Table 1, several radome performance perameter table of silica fiber composite inorganic material
| Material | Density (g/cm 3) | Flexural strength (MPa) | Breaking strain (%) | Specific inductivity (ε) | Loss tangent (tg δ/10 -3) |
| Fabric/SiO 2 | 1.6～1.75 | 60～110 | 0.5～1 | 2.8～3.0 | 5～8 |
| 2.5DQ/ organosilicon | 1.6～1.70 | 50～110 | 0.4～1.7 | 3.2～3.4 | 7～8 |
| 2.5DQ/ phosphoric acid salt | 1.6～1.85 | 40～110 | 0.3～0.9 | 3.2～3.4 | 7～8 |
| 3DQ/SiO 2 | 1.70～1.85 | 60～110 | 0.2～0.7 | 3.0～3.4 | 5～8 |
Fibre reinforced composites can be applicable in antenna windows, the radome aerospace parts, and radome wherein is positioned at the head of various aerospacecrafts, and it is the structure-functional component that integrates ripple, carrying, solar heat protection.Along with the increase of aircraft Mach numbers such as guided missile, also more and more higher to the performance requriements of radome material, wish can satisfy when material has suitable dielectric properties and heat conductivility the requirement of mechanical property.
Because the mechanical property of original fibre-quartz ceramic-base composite material is relatively poor, limited its application on high Mach number large size missile-borne radome, therefore be badly in need of a kind of method that improves this composite materials property, enlarge its range of application, satisfy the demand of Aeronautics and Astronautics product the large-size antennae cover material.
Summary of the invention
The object of the present invention is to provide a kind of Enhancement Method of fibre-quartz ceramic-base composite material, improve the mechanical property of matrix material, make it satisfy the application requiring of high Mach number large-size antennae cover.
The Enhancement Method of fibre-quartz ceramic-base composite material of the present invention, the composite body of-in-situ solidifying moulding preparation long-pending to oozing through liquid phase is carried out the colloidal sol enhancing and is oozed long-pending the processing, is prepared into composite finished product through gel, curing, wherein, the batching mole percentage composition of colloidal sol slip is:
Analytical pure dehydrated alcohol 10～50%
Analytical pure tetraethoxy 6～20%
Distilled water 30～70%
Methyl ethyl diketone or glycerine 6～20%.
Fiber comprises silica fiber, sapphire whisker and boron nitride fibre etc.
Operating process:
At first prepare the colloidal sol slip, with dehydrated alcohol, sequestrant and tetraethoxy thorough mixing, with acid solutions such as hydrochloric acid or nitric acid the pH value of distilled water is adjusted to 2～3, and slowly joins in the above-mentioned mixed solution, and then utilize ultrasonic wave to mix 15～30min can to form even colloidal sol.(vacuum pressure≤0.01MPa), make and ooze long-pending colloidal sol slip between fibre-quartz ceramic-base composite material matrix and fiber gets final product through gel and thermal treatment then with fibre-quartz ceramic-base composite material vacuum impregnation in the colloidal sol slip then.
Wherein:
The colloidal sol slip need utilize ultrasonic or alternate manner (as stirring) disperses, and makes its thorough mixing, forms even colloidal sol.
The gelling temp of colloidal sol slip is 60～80 ℃, and thermal treatment temp is 300～500 ℃, soaking time 2～6 hours.
Among the present invention:
Tetraethoxy has lower surface tension, can infiltrate composite inner, and hydrolysis generation silicon-dioxide, but the space of filled composite materials inside, improve its density and density uniformity, also can improve the intergranular bonding strength of fibre-quartz ceramic-base composite material simultaneously.
Sequestrant can play the effect that suppresses teos hydrolysis and improve the stability of colloidal sol slip.
H in the colloidal sol slip
+Be hydrolyst, the hydrolysis rate of may command tetraethoxy.
Matrix material of the present invention at room temperature has higher mechanical property, table 2 is to utilize this Enhancement Method to strengthen the mechanical property contrast of front and back fiber composite, can find to utilize matrix material after this method strengthens by this table, change in dielectric constant is little, but mechanical property has had significantly raising, compressive strength has improved 157%, and tensile strength has improved 77%.But the fiber reinforcement silica based matrix material of the present invention's preparation has material densification degree height, with short production cycle, characteristics such as cost is low, mass production simple to operate.
Table 2, utilize this method fibre composite performance comparison table before and after strengthening
The Enhancement Method of fibre-quartz ceramic-base composite material of the present invention, can not only improve material density, improve the density uniformity of material, can also strengthen SiO
2Bonding force between powder granule can also significantly improve the overall performance of this matrix material, can satisfy the requirement of high Mach number radome to material property.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
At first prepare the colloidal sol slip, compound method is as follows: with 2mol dehydrated alcohol, 1mol methyl ethyl diketone and 1mol tetraethoxy thorough mixing, utilize hydrochloric acid that the pH value of distilled water is adjusted to 2.5 then, and slowly join in the mixed solution, fully stir back ultrasonic 30min in ultrasonic wave.
Fabric is immersed in the quartzy slip, ooze long-pending-in-situ solidifying moulding through liquid phase, be prepared into composite body, then base substrate is immersed in the colloidal sol slip of method for preparing, vacuum impregnation (vacuum pressure is 0.01MPa) makes base substrate infiltrate the colloidal sol slip, then at 70 ℃ of following gels, thermal treatment under 350 ℃ of temperature, 2 hours must product.
Embodiment 2
At first prepare the colloidal sol slip: with 5mol dehydrated alcohol, 2mol glycerine and 3mol tetraethoxy thorough mixing, utilize nitric acid that the pH value of distilled water is adjusted to 2.2 then, and slowly join in the mixed solution, fully stir back ultrasonic mixing 30min in ultrasonic wave.
Fabric is immersed in the quartzy slip, to ooze long-pending-in-situ solidifying moulding through liquid phase then, the fibre reinforced composites base substrate that is prepared into immerses above-mentioned colloidal sol to be strengthened in the slip, vacuum impregnation (vacuum pressure is 0.008MPa), make and infiltrate the colloidal sol slip in the composite body, then at 75 ℃ of following gels, thermal treatment under 400 ℃ temperature, 2 hours product.
Embodiment 3
The Enhancement Method of fibre-quartz ceramic-base composite material of the present invention is carried out the colloidal sol enhancing with fibre-quartz ceramic-base composite material and is oozed long-pending the processing, is prepared into composite finished product through gel, curing, and wherein, the batching mole percentage composition of colloidal sol slip is:
Analytical pure dehydrated alcohol 30%
Analytical pure tetraethoxy 10%
Distilled water 45%
Methyl ethyl diketone 15%.
With dehydrated alcohol, glycerine or methyl ethyl diketone and tetraethoxy thorough mixing, utilize hydrochloric acid or nitric acid that the pH value of distilled water is adjusted to 2.5 then, and slowly join in the mixed solution, it is standby fully to stir back ultrasonic mixing 18min in ultrasonic wave.
The fibre-quartz ceramic-base composite material base substrate is immersed above-mentioned colloidal sol to be strengthened in the slip, vacuum impregnation (vacuum pressure is 0.009MPa) makes and infiltrates the colloidal sol slip in the composite body, then at 70 ℃ of following gels, thermal treatment under 450 ℃ temperature, 4 hours must product.
Embodiment 4
The Enhancement Method of fibre-quartz ceramic-base composite material of the present invention is carried out the colloidal sol enhancing with fibre-quartz ceramic-base composite material and is oozed long-pending the processing, is prepared into composite finished product through gel, curing, and wherein, the batching mole percentage composition of colloidal sol slip is:
Analytical pure dehydrated alcohol 45%
Analytical pure tetraethoxy 15%
Distilled water 30%
Glycerine 10%.
With dehydrated alcohol, glycerine or methyl ethyl diketone and tetraethoxy thorough mixing, utilize hydrochloric acid or nitric acid that the pH value of distilled water is adjusted to 2 then, and slowly join in the mixed solution, it is standby fully to stir back ultrasonic mixing 20min in ultrasonic wave.
The fibre-quartz ceramic-base composite material base substrate is immersed above-mentioned colloidal sol to be strengthened in the slip, vacuum impregnation (vacuum pressure is 0.007MPa) makes and infiltrates the colloidal sol slip in the composite body, then at 75 ℃ of following gels, thermal treatment under 400 ℃ temperature, 5 hours must product.
Embodiment 5
The Enhancement Method of fibre-quartz ceramic-base composite material of the present invention is carried out the colloidal sol enhancing with fibre-quartz ceramic-base composite material and is oozed long-pending the processing, is prepared into composite finished product through gel, curing, and wherein, the batching mole percentage composition of colloidal sol slip is:
Analytical pure dehydrated alcohol 15%
Analytical pure tetraethoxy 16%
Distilled water 57%
Methyl ethyl diketone 12%.
With dehydrated alcohol, glycerine or methyl ethyl diketone and tetraethoxy thorough mixing, utilize hydrochloric acid or nitric acid that the pH value of distilled water is adjusted to 3 then, and slowly join in the mixed solution, it is standby fully to stir back ultrasonic mixing 28min in ultrasonic wave.
The fibre-quartz ceramic-base composite material base substrate is immersed above-mentioned colloidal sol to be strengthened in the slip, vacuum impregnation (vacuum pressure is 0.009MPa) makes and infiltrates the colloidal sol slip in the composite body, then at 70 ℃ of following gels, thermal treatment under 300 ℃ temperature, 6 hours must product.
Embodiment 6
The Enhancement Method of fibre-quartz ceramic-base composite material of the present invention is carried out the colloidal sol enhancing with fibre-quartz ceramic-base composite material and is oozed long-pending the processing, is prepared into composite finished product through gel, curing, and wherein, the batching mole percentage composition of colloidal sol slip is:
Analytical pure dehydrated alcohol 34%
Analytical pure tetraethoxy 15%
Distilled water 35%
Methyl ethyl diketone 16%.
With dehydrated alcohol, glycerine or methyl ethyl diketone and tetraethoxy thorough mixing, utilize hydrochloric acid or nitric acid that the pH value of distilled water is adjusted to 2.5 then, and slowly join in the mixed solution, it is standby fully to stir back ultrasonic mixing 22min in ultrasonic wave.
The fibre-quartz ceramic-base composite material base substrate is immersed above-mentioned colloidal sol to be strengthened in the slip, vacuum impregnation (vacuum pressure is 0.01MPa) makes and infiltrates the colloidal sol slip in the composite body, then at 60 ℃ of following gels, thermal treatment under 500 ℃ temperature, 2 hours must product.
Claims (2)
1. the Enhancement Method of a fibre-quartz ceramic-base composite material, the composite body that it is characterized in that-in-situ solidifying moulding preparation long-pending to oozing through liquid phase, carry out the colloidal sol enhancing and ooze long-pending the processing, be prepared into composite finished product through gel, curing, wherein, the batching mole percentage composition of colloidal sol slip is:
Fiber comprises silica fiber, sapphire whisker and boron nitride fibre;
Operating process:
At first prepare the colloidal sol slip, with dehydrated alcohol, sequestrant and tetraethoxy thorough mixing, with hydrochloric acid acid solution or nitric acid acid solution the pH value of distilled water is adjusted to 2～3, and slowly join in the mixed solution, and then utilize ultrasonic wave mixing 15～30min to form even colloidal sol, then with fibre-quartz ceramic-base composite material vacuum impregnation in the colloidal sol slip, vacuum pressure≤0.01MPa, make and ooze long-pending colloidal sol slip between fibre-quartz ceramic-base composite material matrix and fiber, get final product through gel and thermal treatment then.
2. the Enhancement Method of fibre-quartz ceramic-base composite material according to claim 1, the gelling temp that it is characterized in that the colloidal sol slip is 60～80 ℃, thermal treatment temp is 300～500 ℃, soaking time 2～6 hours.
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| CN101591192B true CN101591192B (en) | 2011-12-28 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102167609B (en) * | 2010-12-23 | 2012-10-10 | 中国人民解放军国防科学技术大学 | Quartz/quartz-boron nitride high-temperature wave-permeable material |
| CN103787684B (en) * | 2014-01-23 | 2015-09-30 | 湖北三江航天江北机械工程有限公司 | The preparation method of high temperature resistant nitride based ceramic penetrating wave composite material forming thing |
| CN104909791B (en) * | 2015-05-27 | 2016-10-12 | 山东工业陶瓷研究设计院有限公司 | Quartz fibre strengthens the densifying method of quartz-ceramics composite |
| CN106810287B (en) * | 2015-11-30 | 2020-06-16 | 航天特种材料及工艺技术研究所 | Method for improving density of large-thickness fiber reinforced quartz composite material |
| CN109553431B (en) * | 2018-12-11 | 2021-08-31 | 哈尔滨工业大学 | Preparation method of hollow quartz fiber fabric tough ceramic matrix composite material |
| CN109761628B (en) * | 2019-03-19 | 2022-06-07 | 江西嘉捷信达新材料科技有限公司 | Chopped fiber reinforced wave-transmitting ceramic matrix composite material for radar antenna window/antenna housing and preparation method thereof |
| CN110015892A (en) * | 2019-04-16 | 2019-07-16 | 山东工业陶瓷研究设计院有限公司 | A kind of quartz-ceramics densification maceration extract and preparation method thereof, application method |
| CN112851384B (en) * | 2021-01-29 | 2022-07-08 | 中南大学 | Preparation method of low-temperature sintered ceramic matrix composite based on silicon carbide fiber reinforcement |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5082810A (en) * | 1990-02-28 | 1992-01-21 | E. I. Du Pont De Nemours And Company | Ceramic dielectric composition and method for preparation |
| CN1854105A (en) * | 2004-12-31 | 2006-11-01 | 电子科技大学 | Nanometer ceramic-material doping agent, ceramic capacitor media material and production thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5082810A (en) * | 1990-02-28 | 1992-01-21 | E. I. Du Pont De Nemours And Company | Ceramic dielectric composition and method for preparation |
| CN1854105A (en) * | 2004-12-31 | 2006-11-01 | 电子科技大学 | Nanometer ceramic-material doping agent, ceramic capacitor media material and production thereof |
Non-Patent Citations (1)
| Title |
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| JP平2-296764A 1990.12.07 |
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