CN100465129C - Ceramic-base wave-permeation material and preparing process thereof - Google Patents
Ceramic-base wave-permeation material and preparing process thereof Download PDFInfo
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- CN100465129C CN100465129C CNB2007100162237A CN200710016223A CN100465129C CN 100465129 C CN100465129 C CN 100465129C CN B2007100162237 A CNB2007100162237 A CN B2007100162237A CN 200710016223 A CN200710016223 A CN 200710016223A CN 100465129 C CN100465129 C CN 100465129C
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- aluminium borate
- aluminum phosphate
- borate whisker
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Abstract
This invention relates to a ceramic-based wave-permeable material used for manufacturing antenna housing, and the preparing method therefore. The material is composed (by weight percentages) of: aluminium borate crystal whisker 15-65%, aluminium phosphate 35-85%. The preparation process comprises: ball-milling and raw materials mixing, drying, grinding, cold moulding, drying to obtain final products. In this invention, the crystal whisker of aluminium borate is used as reinforcement material, it has properties of neutral chemical properties, low dielectric constant, high elastricity modulus, excellent strength, heat-resistance, chemical-resistance, acid-resisting, electric insulation and neutron-absorbing and low cost, so, the inventive products containing the same have excellent mechanical properties and dielectric properties.
Description
One, technical field
The invention belongs to the features technical field of ceramic material, specially refer to a kind of ceramic-base wave-permeation material of making by radome and preparation method thereof that is used to.
Two, background technology
Electromagnetic wave transparent material is the basis of development radome, and the dielectric properties of material are to select the main foundation of material, require material to have low-k (ε＜10) and dielectric loss.Pneumatic heating meeting during the aircraft high-speed flight produces very big thermal stresses in that radome is inner, and therefore, radome material must have the ability of very low linear expansivity and good heat shock resistance.Simultaneously, the various stress that produce by overload when bearing the aircraft high-speed flight, it is high that selected radome material intensity is wanted, and have certain rigid.And material must have enough surface hardnesses and fracture toughness property, makes it have anti-weathering and desertification erosion ability.General material is under the hot operation condition, and obvious variation may take place for its dielectric characteristics and intensity, and therefore, the temperature variant influence of every performance of radome material is the smaller the better.
Developed countries has carried out a large amount of research to radome material and preparation technology thereof, makes remarkable progress, and some novel materials and preparation technology have reached the practicability level.The electromagnetic wave transparent material that is used to make radome mainly contains organic materials and ceramic two big classes.Intensity height, the material designability of organic class electromagnetic wave transparent material are strong, but its application is subjected to the restriction of the resistance toheat of matrix resin, can only be applied on the low mach aircraft.So various countries concentrate on the ceramic aspect to research gradually, comprise glass-ceramic, quartz-ceramics and silicon nitride ceramics etc., but this class material obviously exists, and fragility is big, mechanical strength low and dielectric properties are stablized shortcomings such as difference, and its application is very restricted.
Afterwards, various countries had invested the phosphate system electromagnetic wave transparent material to sight again.The phosphate system electromagnetic wave transparent material has dielectric properties excellence, production cost is low, moulding process is simple, with short production cycle characteristics, is the first-selection of radome material of new generation.What at present, phosphate composite material can obtain practical application mainly is siliceous fiber reinforcement aluminum phosphate, Plessy's green and chrome-alumina phosphate matrix material.During production,, use the phosphoric acid salt vacuum impregnation then, at last curing molding under certain temperature and pressure at first with the fabric pre-treatment.But, in preparation process, needing to control the synthetic suitable mol ratio of phosphoric acid salt, and select suitable pH value that fiber is protected processing, this has caused no small difficulty to actual production.
Three, summary of the invention
The object of the present invention is to provide the good ceramic matric composite of a kind of thermotolerance, ablation resistance, mechanical property and dielectric properties; Material preparation method is provided simultaneously.
Ceramic matric composite of the present invention is formulated by aluminium borate whisker and aluminum phosphate powder, and its raw material weight per-cent is: 15～65% aluminium borate whiskers, 35%～85% aluminum phosphate.The optimum material proportion of material of the present invention is: aluminium borate whisker 30～50%, aluminum phosphate 50%～70%.
The preparation technology of this invention material is as follows:
(1) by proportioning weighing aluminium borate whisker, aluminum phosphate raw material, be mixed into slurry with an amount of distilled water then, carry out ball mill mixing;
(2) pellet is leached from the mixture of aluminium borate whisker, aluminum phosphate and distilled water, mixed raw material is put into loft drier dry, temperature is 60～90 ℃;
(3) dried raw material is put into mortar and smash to pieces, and dropwise add polyvinyl alcohol solution, constantly grind simultaneously, put into 30～40 purpose standard sieves then and sieve, will tail over and deposit, not granulated continuation is ground, to whole granulating, afterwards raw material is put into old 24 hours of the sample bag of sealing;
(4) with the raw material coldmoulding after old, pressure is 100～300MPa, and the dwell time is 1～5 minute;
(5) sample that suppresses is put into loft drier and be heated to 60～90 ℃ of temperature, dry 24 hours;
(6) with dried sample sintering under normal pressure, the equipment choosing high temperature resistance furnace, sintering temperature is 850～1400 ℃, is incubated 1～3 hour, naturally cooling is reduced to room temperature in stove then, is prepared into the ceramic-base wave-permeation matrix material.
The preparation method of the invention described above, in the described step (1), ball-grinding machine is selected high-energy planetary formula ball mill for use, and the used pellet of ball milling is the corundum ball, and the ball milling time is 5～60 minutes, and drum's speed of rotation is 200～400 rev/mins.
The preparation method of the invention described above, in the described step (3), the concentration expressed in percentage by weight of polyvinyl alcohol solution is 5%, add-on is 3～15% of a raw material gross weight.
After testing, the technical performance index of material of the present invention is:
Density: 1.50～2.35g/cm
3, room temperature bending strength: 100～300MPa, Vickers' hardness: 30～300MPa, thermal expansivity: 3～5 * 10
-6/ ℃, specific inductivity: 2.7～4.3, tangent of the dielectric loss angle value tg θ: 0.008～0.03.
The present invention selects for use aluminium borate whisker as strengthening body, and the chemical property of this whisker is neutral substantially, is insoluble to substantially in acid, the alkaline solution.Aluminium borate whisker has lower specific inductivity, high Young's modulus, good intensity, thermotolerance, chemical proofing, acid resistance, electrical insulating property and neutron absorptive character, meet requirement, and its price is relatively low, helps reducing production costs as material wild phase of the present invention.Material of the present invention has good mechanical performance and dielectric properties, can satisfy the ripple application requiring.
Preparation method of the present invention is simple, is convenient to produce implement.
Four, embodiment
Below in conjunction with specific embodiment the present invention is made specific description, as do not have other explanation, form proportioning and all be weight percentage.
Invention example 1
The composition proportioning of present embodiment material is: 30% aluminium borate whisker, all the other are aluminum phosphate and other unavoidable impurities.
Become to be grouped into proportioning and step of preparation process according to the present invention, aluminium borate whisker, aluminum phosphate and an amount of distilled water are mixed into slurry, carry out ball mill mixing, the ball milling time is 10 minutes, and drum's speed of rotation is 300 rev/mins; Then pellet is leached from the mixture of aluminium borate whisker, aluminum phosphate and distilled water, mixed raw material is put into loft drier, dried in 60～90 ℃ of temperature; Dried raw material is smashed to pieces, and dropwise to add concentration expressed in percentage by weight be 5% polyvinyl alcohol solution, and the add-on of polyvinyl alcohol solution is 10% of a raw material gross weight, constantly grinds simultaneously, put into 35 mesh standard sieves then and sieve, afterwards raw material is put into old 24 hours of the sample bag of sealing; With the raw material coldmoulding after old, pressure is 100MPa, and the dwell time is 2 minutes; The sample that suppresses is put into loft drier be warmed to 80 ℃ of dryings 24 hours; With dried sample sintering under normal pressure, sintering temperature is 1050 ℃, and soaking time is 1 hour, and naturally cooling is reduced to room temperature in stove then.Through above technological process, make aluminium borate whisker-aluminum phosphate ceramic matric composite.
The measuring technology index of this material is: density 2.22g/cm
3, Vickers' hardness 231MPa, bending strength 235MPa, specific inductivity 4.24, tangent of the dielectric loss angle value 0.02383.
Invention example 2:
The composition proportioning of present embodiment material is: 40% aluminium borate whisker, all the other are aluminum phosphate and other unavoidable impurities.
Carry out ball milling, drying, granulation, moulding, sintering according to this composition proportioning and same step of preparation process and the parameter of embodiment, sintering temperature is 1200 ℃.Through above technological process, make aluminium borate whisker-aluminum phosphate ceramic matric composite.
The measuring technology index of this material is: density 2.02g/cm
3, Vickers' hardness 155MPa, bending strength 187MPa, specific inductivity 3.38, tangent of the dielectric loss angle value 0.02158.
Invention example 3:
The composition proportioning of present embodiment material is: 50% aluminium borate whisker, all the other are aluminum phosphate and other unavoidable impurities.
Carry out ball milling, drying, granulation, moulding, sintering according to this composition proportioning and same step of preparation process and the parameter of embodiment, sintering temperature is 1200 ℃.Through above technological process, make aluminium borate whisker-aluminum phosphate ceramic matric composite.
The measuring technology index of this material is: density 1.68g/cm
3, Vickers' hardness 57MPa, bending strength 112MPa, specific inductivity 2.8, tangent of the dielectric loss angle value 0.01036.
Claims (5)
1, a kind of ceramic-base wave-permeation material is characterized in that: be compound formulated by aluminium borate whisker and aluminum phosphate powder, its raw material weight per distribution ratio is: aluminium borate whisker 15～65%, aluminum phosphate 35%～85%.
2, ceramic-base wave-permeation material according to claim 1 is characterized in that: the weight percent proportioning of described raw material is: aluminium borate whisker 30～50%, aluminum phosphate 50%～70%.
3, the preparation method of the described ceramic-base wave-permeation material of a kind of claim 1 is characterized in that adopting following steps:
(1) by proportioning weighing aluminium borate whisker, aluminum phosphate raw material, is mixed into slurry with distilled water then, carries out ball mill mixing;
(2) pellet is leached from the mixture of aluminium borate whisker, aluminum phosphate and distilled water, mixed raw material is put into loft drier dry, temperature is 60～90 ℃;
(3) dried raw material is put into mortar and smash to pieces, and dropwise add polyvinyl alcohol solution, constantly grind simultaneously, put into 30～40 purpose standard sieves then and sieve, will tail over and deposit, not granulated continuation is ground, to whole granulating, afterwards raw material is put into old 24 hours of the sample bag of sealing;
(4) with the raw material coldmoulding after old, pressure is 100～300MPa, and the dwell time is 1～5 minute;
(5) sample that suppresses is put into loft drier and be heated to 60～90 ℃ of temperature, dry 24 hours;
(6) with dried sample sintering under normal pressure, the equipment choosing high temperature resistance furnace, sintering temperature is 850～1400 ℃, is incubated 1～3 hour, naturally cooling is reduced to room temperature in stove then, is prepared into the ceramic-base wave-permeation matrix material.
4. preparation method according to claim 3 is characterized in that: in the described step (1), ball-grinding machine is selected high-energy planetary formula ball mill for use, and the used pellet of ball milling is the corundum ball, and the ball milling time is 5～60 minutes, and drum's speed of rotation is 200～400 rev/mins.
5. preparation method according to claim 3 is characterized in that: in the described step (3), the concentration expressed in percentage by weight of polyvinyl alcohol solution is 5%, and add-on is 3～15% of a raw material gross weight.
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| CN100465129C true CN100465129C (en) | 2009-03-04 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101402797B (en) * | 2008-10-27 | 2010-12-08 | 苏州大学 | Aluminum orthophosphate/heat convertible resin compound system and method of producing the same |
| CN101817690B (en) * | 2010-02-09 | 2012-08-29 | 济南大学 | Borate whisker reinforced aluminum phosphate ceramic wave-transparent material and preparation method thereof |
| CN102432323B (en) * | 2011-09-15 | 2013-07-03 | 济南大学 | Wave-transmitting material and preparation method thereof |
| CN108455995A (en) * | 2018-02-09 | 2018-08-28 | 青海大学 | A kind of silicon carbide fibre enhancing aluminum phosphate ceramic matric composite and preparation method thereof |
| CN109251041B (en) * | 2018-11-19 | 2021-05-18 | 中国民航大学 | Preparation method of mullite whisker in-situ growth self-toughening aluminum phosphate-based high-temperature-resistant adhesive |
| CN111205067B (en) * | 2020-01-15 | 2022-04-01 | 武汉科技大学 | Glass-ceramic material for cooperative protection of neutrons and gamma rays and preparation method thereof |
| CN115974524A (en) * | 2022-12-19 | 2023-04-18 | 湖北中烟工业有限责任公司 | Preparation method of low-dielectric-constant insulating ceramic |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1676617A (en) * | 2005-04-17 | 2005-10-05 | 上海师范大学 | Method for preparing high temperature resistant wave-permeable material special for steel-smelting furnace |
| CN1793014A (en) * | 2005-10-27 | 2006-06-28 | 中材高新材料股份有限公司 | Low dielectric, wave-transparent porous ceramic material and preparation process thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1676617A (en) * | 2005-04-17 | 2005-10-05 | 上海师范大学 | Method for preparing high temperature resistant wave-permeable material special for steel-smelting furnace |
| CN1793014A (en) * | 2005-10-27 | 2006-06-28 | 中材高新材料股份有限公司 | Low dielectric, wave-transparent porous ceramic material and preparation process thereof |
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