CN111302808A - Wave-transparent high-dielectric ceramic material and preparation method and application thereof - Google Patents

Wave-transparent high-dielectric ceramic material and preparation method and application thereof Download PDF

Info

Publication number
CN111302808A
CN111302808A CN201811515780.8A CN201811515780A CN111302808A CN 111302808 A CN111302808 A CN 111302808A CN 201811515780 A CN201811515780 A CN 201811515780A CN 111302808 A CN111302808 A CN 111302808A
Authority
CN
China
Prior art keywords
wave
ceramic material
dielectric ceramic
transparent high
dielectric
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201811515780.8A
Other languages
Chinese (zh)
Inventor
张萍萍
王洪升
韦其红
朱保鑫
盖莹
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shandong Industrial Ceramics Research and Design Institute Co Ltd
Original Assignee
Shandong Industrial Ceramics Research and Design Institute Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shandong Industrial Ceramics Research and Design Institute Co Ltd filed Critical Shandong Industrial Ceramics Research and Design Institute Co Ltd
Priority to CN201811515780.8A priority Critical patent/CN111302808A/en
Publication of CN111302808A publication Critical patent/CN111302808A/en
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron

Abstract

The invention discloses a wave-transparent high-dielectric ceramic material and a preparation method and application thereof, wherein the wave-transparent high-dielectric ceramic material is prepared from the following raw materials in parts by weight: 80-95% of silicon nitride and 5-20% of sintering aid, and the addition amount of the high dielectric component is 5-30% of the total weight of the silicon nitride and the sintering aid. The wave-transparent high-dielectric ceramic material disclosed by the embodiment of the invention has good mechanical properties (the bending strength is more than or equal to 150MPa), and also has excellent dielectric properties, the dielectric constant epsilon is 7.5-10.0, the dielectric loss is less than 0.02 (X/Ku/Ka wave band tested by a short-circuit waveguide method), and the use requirement of the multifunctional antenna housing on the wave-transparent high-dielectric ceramic material can be met.

Description

Wave-transparent high-dielectric ceramic material and preparation method and application thereof
Technical Field
The invention relates to the technical field of material preparation, in particular to a preparation method of a wave-transparent high-dielectric ceramic material used for a multifunctional antenna housing.
Background
In recent years, with the rapid development of science and technology, the increasingly complex battlefield environment of modern war has made higher requirements for the accurate guidance and anti-interference capability of missiles. At present, a single guidance mode is difficult to complete a combat mission, and a multimode composite guidance mode must be developed, so that greater challenges are provided for the design and material selection of the key components of the radome. At present, although silicon nitride ceramic materials have excellent force, heat, electricity, thermal shock resistance and ablation resistance, and are also called as the most promising antenna housing materials by the American society of Zongzhi sciences, the requirements of wave-transparent high-dielectric ceramic materials used by multifunctional antenna housings cannot be met due to the lower dielectric properties (the dielectric constant epsilon is less than or equal to 7.5). At present, no preparation method of the wave-transparent high-dielectric ceramic material used by the multifunctional antenna housing exists.
Disclosure of Invention
Based on the prior art, the invention aims to provide a wave-transparent high-dielectric ceramic material, and a preparation method and application thereof.
In a first aspect, an embodiment of the present application provides a wave-transparent high-dielectric ceramic material, which is prepared from the following raw materials in parts by weight: 80-95% of silicon nitride and 5-20% of sintering aid, and the addition amount of the high dielectric component is 5-30% of the total weight of the silicon nitride and the sintering aid.
Preferably: the high dielectric component comprises titanium dioxide or titanate, wherein the titanate comprises more than one of calcium titanate, barium titanate, magnesium titanate and the like, and the chemical reagent grade is analytically pure.
Preferably, the grain diameter of the silicon nitride is 0.5-1.5 μm, and the α phase content is more than or equal to 93%.
Preferably: the particle size of the sintering aid is less than 1.5 mu m, the sintering aid contains more than one of alumina and rare earth oxide, wherein the rare earth oxide is more than one of neodymium oxide, yttrium oxide, lanthanum oxide, samarium oxide and the like.
In a second aspect, embodiments of the present application provide an application of the above-mentioned transparent-wave high-dielectric ceramic material in preparing a multifunctional radome.
In a third aspect, an embodiment of the present application provides a method for preparing the wave-transparent high-dielectric ceramic material, including the following steps: material preparation, ball milling, molding and sintering.
Preferably: the ingredient also comprises a dispersion medium, and the weight ratio of the dosage of the dispersion medium to the total weight of all the powder can be (1-2.5): 1, the dispersion medium may be absolute ethanol.
Preferably: the forming mode is cold isostatic pressing. Further: the pressure of the cold isostatic pressing is 40-200 MPa.
Preferably: the sintering is carried out in a nitrogen atmosphere, the atmosphere pressure is 0.1-6.0MPa, the sintering temperature is 1650-1850 ℃, and the high-temperature heat preservation time is 60-300 min.
Compared with the prior art, the invention has the following beneficial effects:
1. the wave-transparent high-dielectric ceramic material disclosed by the embodiment of the invention has good mechanical properties (the bending strength is more than or equal to 150MPa), and also has excellent dielectric properties, the dielectric constant epsilon is 7.5-10.0, the dielectric loss is less than 0.02 (X/Ku/Ka wave band tested by a short-circuit waveguide method), and the use requirement of the multifunctional antenna housing on the wave-transparent high-dielectric ceramic material can be met.
2. The preparation method of the wave-transparent high-dielectric ceramic material disclosed by the embodiment of the invention has the advantages of simple steps, low technical requirements on operators, labor cost saving and suitability for industrial production.
Detailed Description
In order to better understand the technical solution of the present invention, the following embodiments are provided to further explain the present invention.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
Example one
A wave-transparent high-dielectric ceramic material is prepared from the following raw materials in parts by weight: 80 percent of silicon nitride with the grain diameter of 0.5 mu m, 20 percent of sintering aid alumina with the grain diameter of 1.0 mu m, and 5 percent of high dielectric component titanium dioxide by weight of the total weight of the silicon nitride and the alumina.
The preparation method of the wave-transparent high-dielectric ceramic material comprises the following steps:
adding a dispersion medium which is 2.5 times of the amount of all the raw materials into the raw materials, then batching, carrying out ball milling, forming and firing treatment to obtain the catalyst.
Example two
In this embodiment, the silicon nitride has a particle size of 1.5 μm and a weight fraction of 95%, the sintering aid is a rare earth oxide, yttria, has a particle size of 0.5 μm and a weight fraction of 5%, and the high dielectric component is calcium titanate, which is used in an amount of 30% of the total weight of the silicon nitride and the rare earth oxide.
The forming mode is cold isostatic pressing, and the pressure of the cold isostatic pressing is 40 MPa.
The sintering is carried out in a nitrogen atmosphere, the atmosphere pressure is 0.1MPa, the sintering temperature is 1650 ℃, and the high-temperature heat preservation time is 60 min.
Other technical features are the same as those of the embodiment.
EXAMPLE III
In the embodiment, the particle size of the silicon nitride is 1.0 μm, the weight fraction of the silicon nitride is 90%, the sintering aid is rare earth oxide lanthanum oxide, the particle size is 1.2 μm, the weight fraction of the sintering aid is 10%, and the high dielectric component is barium titanate, and the usage amount of the high dielectric component is 10% of the total weight of the silicon nitride and the rare earth oxide.
The forming mode is cold isostatic pressing, and the pressure of the cold isostatic pressing is 200 MPa.
The sintering is carried out in a nitrogen atmosphere, the atmosphere pressure is 6.0MPa, the sintering temperature is 1850 ℃, and the high-temperature heat preservation time is 300 min.
Other technical features are the same as those of the first embodiment or the second embodiment.
Example four
In the embodiment, the particle size of the silicon nitride is 0.8 μm, the weight fraction of the silicon nitride is 85%, the sintering aid is rare earth oxide samarium oxide, the particle size is 1.0 μm, the weight fraction of the sintering aid is 15%, and the high dielectric component is magnesium titanate, and the usage amount of the high dielectric component is 20% of the total weight of the silicon nitride and the rare earth oxide.
The forming mode is cold isostatic pressing, and the pressure of the cold isostatic pressing is 80 MPa.
The sintering is carried out in a nitrogen atmosphere, the atmosphere pressure is 3.0MPa, the sintering temperature is 1750 ℃, and the high-temperature heat preservation time is 150 min.
Other technical features are the same as those of any one of the first to third embodiments.
EXAMPLE five
In the embodiment, the particle size of the silicon nitride is 1.1 μm, the weight fraction of the silicon nitride is 90%, the sintering aid is aluminum oxide and rare earth oxide samarium oxide, the particle size is 0.3 μm, the weight fraction of the sintering aid is 10%, and the high dielectric component is magnesium titanate and barium titanate, and the using amount of the high dielectric component is 8% of the total weight of the silicon nitride and the sintering aid.
The forming mode is cold isostatic pressing, and the pressure of the cold isostatic pressing is 150 MPa.
The sintering is carried out in a nitrogen atmosphere, the atmosphere pressure is 1.0MPa, the sintering temperature is 1700 ℃, and the high-temperature heat preservation time is 250 min.
Other technical features are the same as those of any one of the first to fourth embodiments.
EXAMPLE six
The dispersion medium described in this example was absolute ethanol, which was used in an amount of 2.5 times the weight of all the raw materials.
Other technical features are the same as those of any one of the first to fifth embodiments.
EXAMPLE seven
The dispersion medium described in this example was absolute ethanol, which was used in an amount of 2 times the weight of all the raw materials.
Other technical features are the same as those of any one of the first to fifth embodiments.
Example eight
Weight fraction of each raw material Si in the present example3N492％，Y2O38％，TiO2Is Si3N4And Y2O320% of the mass.
Other technical features are the same as those of the first to seventh embodiments.
Example nine
Weight fraction of each raw material Si in the present example3N490％，Y2O34％，Al2O36％，BaTiO3Is Si3N4、Al2O3And Y2O320% of the mass.
Other technical features are the same as those of the first to seventh embodiments.
Example ten
Weight fraction of each raw material Si in the present example3N490％，Y2O310％，MgTiO3Is Si3N4And Y2O35% by mass.
Other technical features are the same as those of the first to seventh embodiments.
EXAMPLE eleven
Weight fraction of each raw material Si in the present example3N485％，Y2O36％，Al2O39％，CaTiO3Is Si3N4、Al2O3And Y2O35% by mass.
Other technical features are the same as those of the first to seventh embodiments.
Example twelve
Weight fraction of each raw material Si in the present example3N490％，Y2O34％，Al2O36％，TiO2Is Si3N4、Al2O3And Y2O320% of the mass.
Other technical features are the same as those of the first to seventh embodiments.
Test examples
The performance parameters of the wave-transparent high-dielectric ceramic materials prepared in the eight to twelve examples are shown in the following table:
numbering Material composition Bending strength (MPa) Dielectric constant Dielectric loss
1 Example eight 308.1 8.44 -0.0091
2 Example nine 732.3 8.98 -0.0165
3 Example ten 421 7.75 -0.0052
4 EXAMPLE eleven 340.1 8.89 -0.0157
5 Example twelve 285.5 9.98 -0.0149
The above description is only a preferred embodiment of the application and is illustrative of the principles of the technology employed. It will be appreciated by a person skilled in the art that the scope of the invention as referred to in the present application is not limited to the embodiments with a specific combination of the above-mentioned features, but also covers other embodiments with any combination of the above-mentioned features or their equivalents without departing from the inventive concept. For example, the above features may be replaced with (but not limited to) features having similar functions disclosed in the present application.

Claims (10)

1. A wave-transparent high-dielectric ceramic material is characterized in that: the feed is prepared from the following raw materials in parts by weight: 80-95% of silicon nitride and 5-20% of sintering aid, and the addition amount of the high dielectric component is 5-30% of the total weight of the silicon nitride and the sintering aid.
2. The wave-transparent high-dielectric ceramic material of claim 1, wherein: the high dielectric component comprises titanium dioxide or a titanate.
3. The wave-transparent high-dielectric ceramic material of claim 2, wherein: the titanate includes one or more of calcium titanate, barium titanate, magnesium titanate, and the like.
4. The wave-transparent high-dielectric ceramic material as claimed in claim 1, wherein the silicon nitride has a particle size of 0.5-1.5 μm and a α phase content of 93% or more.
5. The wave-transparent high-dielectric ceramic material of claim 1, wherein: the grain size of the sintering aid is less than 1.5 mu m, and the sintering aid can be more than one of aluminum oxide and rare earth oxide.
6. The wave-transparent high-dielectric ceramic material of claim 5, wherein: the rare earth oxide is more than one of neodymium oxide, yttrium oxide, lanthanum oxide, samarium oxide and the like.
7. Use of the wave-transparent high-dielectric ceramic material according to any one of claims 1 to 6 for the preparation of a multifunctional radome.
8. A method for preparing the wave-transparent high-dielectric ceramic material according to any one of claims 1 to 6, which is characterized by comprising the following steps: the method comprises the following steps: material preparation, ball milling, molding and sintering.
9. The method for preparing the wave-transparent high-dielectric ceramic material according to claim 8, wherein: the ingredient also comprises a dispersion medium, and the weight ratio of the dosage of the dispersion medium to the total weight of all the powders can be (1-2.5): 1.
10. the method for preparing the wave-transparent high-dielectric ceramic material according to claim 8, wherein: the forming mode is cold isostatic pressing, the pressure of the cold isostatic pressing is 40-200MPa, the sintering is sintering in a nitrogen atmosphere, the atmosphere pressure is 0.1-6.0MPa, the sintering temperature is 1650-1850 ℃, and the high-temperature heat preservation time is 60-300 min.
CN201811515780.8A 2018-12-12 2018-12-12 Wave-transparent high-dielectric ceramic material and preparation method and application thereof Pending CN111302808A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811515780.8A CN111302808A (en) 2018-12-12 2018-12-12 Wave-transparent high-dielectric ceramic material and preparation method and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811515780.8A CN111302808A (en) 2018-12-12 2018-12-12 Wave-transparent high-dielectric ceramic material and preparation method and application thereof

Publications (1)

Publication Number Publication Date
CN111302808A true CN111302808A (en) 2020-06-19

Family

ID=71158082

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811515780.8A Pending CN111302808A (en) 2018-12-12 2018-12-12 Wave-transparent high-dielectric ceramic material and preparation method and application thereof

Country Status (1)

Country Link
CN (1) CN111302808A (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104926290A (en) * 2014-03-21 2015-09-23 中国石油化工股份有限公司 Composite material and its application
CN105541341A (en) * 2016-01-12 2016-05-04 河北高富氮化硅材料有限公司 Method for preparing high-compactness silicon nitride ceramic by adding composite additives
CN106631042A (en) * 2017-01-23 2017-05-10 威海圆环先进陶瓷有限公司 Manufacturing process of preparing silicon nitride ceramic circuit board
CN108203302A (en) * 2016-12-16 2018-06-26 中国科学院上海硅酸盐研究所 A kind of adjustable middle low-k silicon nitride ceramics of dielectric constant and preparation method thereof
CN108546131A (en) * 2018-06-29 2018-09-18 芜湖市元奎新材料科技有限公司 The preparation method of porous SiN ceramic

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104926290A (en) * 2014-03-21 2015-09-23 中国石油化工股份有限公司 Composite material and its application
CN105541341A (en) * 2016-01-12 2016-05-04 河北高富氮化硅材料有限公司 Method for preparing high-compactness silicon nitride ceramic by adding composite additives
CN108203302A (en) * 2016-12-16 2018-06-26 中国科学院上海硅酸盐研究所 A kind of adjustable middle low-k silicon nitride ceramics of dielectric constant and preparation method thereof
CN106631042A (en) * 2017-01-23 2017-05-10 威海圆环先进陶瓷有限公司 Manufacturing process of preparing silicon nitride ceramic circuit board
CN108546131A (en) * 2018-06-29 2018-09-18 芜湖市元奎新材料科技有限公司 The preparation method of porous SiN ceramic

Similar Documents

Publication Publication Date Title
CN109231967B (en) Bi2O3-B2O3Binary system microwave dielectric ceramic material and preparation method thereof
CN113004028A (en) Silicon-based low-dielectric microwave dielectric ceramic and preparation method thereof
CN110937892A (en) High-temperature absorbent, ultrathin high-temperature wave-absorbing material and preparation method thereof
CN113213894A (en) High-purity alumina ceramic substrate and preparation process thereof
CN102815928B (en) Preparation method of rare earth ions-doped hexaaluminate high-emissivity material
CN100522875C (en) Dielectric adjustable low-temperature co-fired composite microwave ceramic material and preparation method thereof
CN111302808A (en) Wave-transparent high-dielectric ceramic material and preparation method and application thereof
CN106977210B (en) High-thermal-conductivity microwave attenuation ceramic material and preparation method thereof
CN104446439B (en) Dielectric constant microwave dielectric ceramic In6mgTi5o20and preparation method thereof
CN109320236B (en) Composite material with high energy storage density and charge-discharge performance and preparation method thereof
CN106830919A (en) Low-temperature sintering wolframite structure microwave-medium ceramics and preparation method thereof
CN106830923A (en) High quality factor microwave dielectric ceramic Bi3Y2Ga3O12
CN107226700A (en) A kind of Si3N4BN MAS ceramic composites and preparation method thereof
CN103981384A (en) Preparation method of tungsten-aluminum nitride-hafnium boride composite material
CN112898031A (en) High-thermal-conductivity high-toughness silicon nitride ceramic material containing rare earth elements and preparation method thereof
CN100404458C (en) Zirconium dioxide mixed modified barium strontium phthalate-magnesium oxide base composite and preparation process thereof
US5677252A (en) Sion low dielectric constant ceramic nanocomposite
CN109320263B (en) Sintering aid, quartz ceramic, and preparation and application methods thereof
CN104446433B (en) Temperature-stable ultralow dielectric microwave dielectric ceramic Li3al2p3o12
CN117616917B (en) B-sandwich-structure ceramic radome material and preparation method thereof
CN107010924A (en) A kind of temperature-stable gallate microwave dielectric ceramic
CN112408990B (en) Ceramic wave-transmitting material matched with infrared material in performance, radome and preparation method
CN111302795A (en) Lithium-magnesium-niobium-aluminum-tungsten microwave dielectric ceramic and preparation method thereof
CN108218438B (en) Silicon nitride broadband wave-transparent material
CN114855113B (en) Low-absorption-ratio high-emissivity coating material and preparation process thereof, and coating system and preparation process thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination