CN108610047A - A kind of ultralow-temperature sintering microwave ceramic material and preparation method thereof - Google Patents

A kind of ultralow-temperature sintering microwave ceramic material and preparation method thereof Download PDF

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CN108610047A
CN108610047A CN201810507562.3A CN201810507562A CN108610047A CN 108610047 A CN108610047 A CN 108610047A CN 201810507562 A CN201810507562 A CN 201810507562A CN 108610047 A CN108610047 A CN 108610047A
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ceramic material
temperature
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sintering
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CN108610047B (en
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李波
田佳蔚
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University of Electronic Science and Technology of China
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    • 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
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
    • 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
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    • 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
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    • 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
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
    • 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
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof

Abstract

The invention belongs to electronic ceramics and its manufacturing technology fields, a kind of ultralow-temperature sintering microwave ceramic material and preparation method thereof is specifically provided, to overcome the universal higher disadvantage of microwave current ceramic material sintering temperature, the sintered at ultra low temperature at 700~750 DEG C is realized, optimal sintering temperature is 725 DEG C.Ceramic material of the present invention is single crystalline phase Ca5Zn4V6O24, chemical formula Ca5+aZn4+bV6O24, wherein 0<a<0.3,0<b<0.3；By adjusting the mode of non-chemical dose ratio, control the internal losses such as external losses and vanadium omission such as the stomata that vanadium volatile zone comes, excellent microwave dielectric property is obtained (under 9.9GHz frequencies, dielectric constant is 12.0, Q × f values are 61974GHz, temperature coefficient of resonance frequency is 91.2ppm/ DEG C), hence it is evident that it is better than chemical dosage ratio Ca5Zn4V6O24.Ceramic material of the present invention is raw materials used abundant, of low cost, is conducive to industrialized production, can be widely applied to the manufacture of the microwave devices such as low-temperature co-fired ceramics system, multilayer dielectricity resonator, filter, microwave base plate.

Description

A kind of ultralow-temperature sintering microwave ceramic material and preparation method thereof
Technical field
The invention belongs to electronic ceramics and its manufacturing technology field, especially a kind of ultralow-temperature sintering microwave ceramic material and Preparation method.
Background technology
It is corresponding to be with the fast development of modern wireless telecommunications industry, Internet of Things, wearable electronic, intelligent transportation system System and device develop to the direction of multi-functional, miniaturization, flexibility, light weight, low cost and high frequency, to the performance of dielectric material It is further proposed that new requirement, the demand of the microwave dielectric ceramic material to haveing excellent performance is continuously increased.Low-temperature co-fired ceramics skill The hybrid integrated of high density integrated circuit and passive device and active device may be implemented in art (L TCC), and then realizes device Miniaturization with system and multifunction.
The major requirement that LTCC technology proposes dielectric material has：(1) have suitable dielectric constant, low dielectric material can be with As baseplate material etc., the delay of signal transmission is reduced；(2) it is strong to be conducive to reduction device loss, raising signal for low-dielectric loss Degree；(3) frequency-temperature coefficient nearly zero ensures the temperature stability of dielectric constant and resonant frequency；(4) it is less than the burning of electrode material Junction temperature；(5) good thermomechanical property, such as high heat conductance, the linear expansion coefficient that matches with composite material.
With the fast development of the flexible devices such as wearable electronic, it is desirable that ceramic material can with eutectic point electrode, partly lead The integrated cofiring such as body material, polymer-based substrate；Although having in document and reporting a large amount of ceramics as low-loss microwave medium material Material, however wherein most of materials have high sintering temperature.Therefore, one of research hotspot is 750 DEG C below ultralow at present The exploitation of ceramic (ULTCC) material of temperature sintering, advantageously reduces energy consumption, prevents the volatilization of volatile components and same other materials Reaction.There is the dielectric material of most of high quality factors (Q × f) high sintering temperature, generally use to add low melting point oxygen The method of compound reduces material sintering temperature, but often causes deterioration and the mechanical strength of its microwave dielectric property Reduction.Common low melting point additive has TeO2、Bi2O3、B2O3、Li2O、V2O5And MoO3Deng.On the other hand, from material science The microwave dielectric ceramic materials of angle design and exploitation with intrinsic ultra-low sintering temperature, it is not only simple at phase, and also performance is excellent It is good.
Vanadate system microwave ceramic material because of its intrinsic sintering temperature and low and excellent microwave dielectric property, by Greatly concern, becomes the important research direction of ultralow temperature microwave ceramic material.In Ceramics International periodicals Report Ca5N i4(VO4)6Ceramics are sintered at 875 DEG C and obtain excellent dielectric properties：εr=9.5GHz, Q × f= 54100GHz, τf=-60pp m/ DEG C (in 10.5GHz), however its higher sintering temperature still limits its further development (43:334–338(2017)).Ca is reported on Ceramics International periodicals5Zn4(VO4)6Ceramics pass through 725 DEG C sintering, microwave dielectric property is：εr=11.7, Q × f=49400GHz, τf=-81ppm/ DEG C (9.7GHz), although realizing Sintered at ultra low temperature, but Q × f values also need to further increase (96 [6]:1691–1693(2013)).In actual production process It was found that since v element is Volatile Elements, uncontrollable loss is will produce in pre-burning and sintering process, causes stomata etc. outer Portion is lost and the internal losses such as vanadium omission, to limit the raising of vanadate microwave ceramics Q × f values.
To sum up, the present invention proposes a kind of ultralow-temperature sintering microwave ceramic material and preparation method thereof.
Invention content
The purpose of the present invention is to provide a kind of ultralow-temperature sintering microwave ceramic materials and preparation method thereof, to overcome mesh The universal higher disadvantage of preceding microwave ceramic material sintering temperature, realizes the sintered at ultra low temperature at 700~750 DEG C, best to be sintered Temperature is 725 DEG C.Ceramic material of the present invention is single crystalline phase Ca5Zn4V6O24, chemical formula Ca5+aZn4+bV6O24, wherein 0<a <0.3,0<b<0.3；By adjusting the mode of non-chemical dose ratio, control the external losses such as the stomata that vanadium volatile zone comes and The internal losses such as vanadium omission, obtain excellent microwave dielectric property (under 9.9GHz frequencies, dielectric constant 12.0, Q × f values For 61974GHz, temperature coefficient of resonance frequency is -91.2ppm/ DEG C), hence it is evident that it is better than chemical dosage ratio Ca5Zn4V6O24.The present invention Ceramic material is raw materials used abundant, of low cost, is conducive to industrialized production, can be widely applied to low-temperature co-fired ceramics system, The manufacture of the microwave devices such as multilayer dielectricity resonator, filter, microwave base plate.
In order to achieve the above objectives, the technical solution adopted by the present invention is；
A kind of ultralow-temperature sintering microwave ceramic material, which is characterized in that the ceramic material has cubic garnet type knot Structure, single crystalline phase are Ca5Zn4V6O24, chemical general formula Ca5+aZn4+bV6O24, wherein 0<a<0.3、0<b<0.3.
The preparation method of above-mentioned ultralow-temperature sintering microwave ceramic material, which is characterized in that include the following steps：
Step 1：Using CaCO3、ZnO、V2O5For raw material, according to Ca：Zn：V=5+a：4+b：6 mol ratio is matched Material obtains mixture, wherein 0<a<0.3、0<b<0.3；
Step 2：Mixture obtained by step 1 is subjected to ball milling, obtains ball milling material；
Step 3：Step 2 gained ball milling material is dried and is sieved to obtain evenly dispersed powder；
Step 4：It is placed in 2~5h of pre-burning under 680~720 DEG C of temperature conditions by evenly dispersed powder is obtained obtained by step 3 Obtain pre-burning powder；
Step 5：It is dry-pressing formed to obtain green compact after step 4 gained pre-burning powder is granulated；
Step 6：Step 5 gained green compact are placed in 3~5h of sintering under 700~750 DEG C of temperature conditions, obtain the ultralow temperature Sintered microwave ceramic material.
The beneficial effects of the present invention are：
1. microwave ceramic material provided by the invention can complete sintering under 700~750 DEG C of ultra low temperatures, belong to ultralow Warm sintered microwave ceramic material, ultralow sintering temperature can not only substantially reduce energy consumption and production cost, and can prevent The only volatilization of volatile components and the reaction with other materials；
2. microwave ceramic material provided by the invention has ultralow intrinsic sintering temperature, any sintering need not be added and helped Agent causes the consistency and strength reduction of dielectric material penalty and porcelain body so as to avoid sintering aid；It avoids and helps burning The cumbersome preparation process of agent, such as glass smelting；
3. microwave ceramic material provided by the invention keeps single crystalline phase Ca5Zn4V6O24, by adjusting non-chemical dose ratio Mode, control the internal losses such as external losses and vanadium omission such as stomata that vanadium volatile zone comes, substantially increase dielectricity Can, dielectric constant about 12, Q × f values are higher than 60000GHz, about -90ppm/ DEG C of temperature coefficient of resonance frequency；
4. the preparation process that the present invention provides ceramic material is simple, raw materials used abundant, of low cost, be conducive to industrialize Production, can be widely applied to the microwave devices such as low-temperature co-fired ceramics system, multilayer dielectricity resonator, filter, microwave base plate Manufacture.
Description of the drawings
Fig. 1 is the SEM figures that the embodiment of the present invention 1 is prepared into ultralow-temperature sintering microwave ceramic material.
Fig. 2 is the XRD diagram that the embodiment of the present invention 1 is prepared into ultralow-temperature sintering microwave ceramic material.
Specific implementation mode
The present invention is described in further details with reference to the accompanying drawings and examples.
5 embodiments are provided in the present invention, respectively number 1~5；Each embodiment provides ultralow-temperature sintering microwave ceramics material It is Ca that material, which has cubic garnet type structure, single crystalline phase,5Zn4V6O24, chemical general formula Ca5+aZn4+bV6O24, wherein 0< a<0.3、0<b<0.3。
The preparation method of above-mentioned ultralow-temperature sintering microwave ceramic material, includes the following steps：
Step 1：Using CaCO3、ZnO、V2O5For raw material, carries out dispensing according to the stoicheiometry of chemical formula and obtains mixture,
Step 2：Mixture obtained by step 1 is subjected to ball milling, obtains ball milling material；
Step 3：Step 2 gained ball milling material is dried and is sieved to obtain evenly dispersed powder；
Step 4：It is placed in 2~5h of pre-burning under 680~720 DEG C of temperature conditions by evenly dispersed powder is obtained obtained by step 3 Obtain pre-burning powder；
Step 5：Step 4 gained pre-burning powder addition polyvinyl alcohol water solution is granulated, the dry-pressing under 20Mpa pressure Molding, obtains a diameter of 15mm, and thickness is the cylinder green compact of 6~7mm；
Step 6：Step 5 gained green compact are placed in 3~5h of sintering under 700~750 DEG C of temperature conditions, obtain the ultralow temperature Sintered microwave ceramic material.
The specific of above-mentioned 5 embodiments discloses parameter and is prepared into ultralow-temperature sintering microwave ceramic material microwave dielectric properties As shown in the table：
Wherein, embodiment 1 be prepared into ultralow-temperature sintering microwave ceramic material SEM figures and XRD diagram respectively such as Fig. 1 and Fig. 2 Locked, as seen from the figure, which is that single crystalline phase is Ca5Zn4V6O24, there is cubic garnet type structure.
The above description is merely a specific embodiment, any feature disclosed in this specification, except non-specifically Narration, can be replaced by other alternative features that are equivalent or have similar purpose；Disclosed all features or all sides Method or in the process the step of, other than mutually exclusive feature and/or step, can be combined in any way.

Claims (2)

1. a kind of ultralow-temperature sintering microwave ceramic material, which is characterized in that the ceramic material has cubic garnet type structure, Its single crystalline phase is Ca5Zn4V6O24, chemical general formula Ca5+aZn4+bV6O24, wherein 0<a<0.3、0<b<0.3.
2. by the preparation method of ultralow-temperature sintering microwave ceramic material described in claim 1, which is characterized in that including following step Suddenly：
Step 1：Using CaCO3、ZnO、V2O5For raw material, according to Ca：Zn：V=5+a：4+b：6 mol ratio carries out dispensing and obtains To mixture, wherein 0<a<0.3、0<b<0.3；
Step 2：Mixture obtained by step 1 is subjected to ball milling, obtains ball milling material；
Step 3：Step 2 gained ball milling material is dried and is sieved to obtain evenly dispersed powder；
Step 4：Evenly dispersed powder will be obtained obtained by step 3 and is placed in 2~5h of pre-burning under 680~720 DEG C of temperature conditions obtaining Pre-burning powder；
Step 5：It is dry-pressing formed to obtain green compact after step 4 gained pre-burning powder is granulated；
Step 6：Step 5 gained green compact are placed in 3~5h of sintering under 700~750 DEG C of temperature conditions, obtain the sintered at ultra low temperature Microwave ceramic material.
CN201810507562.3A 2018-05-24 2018-05-24 Ultralow temperature sintered microwave ceramic material and preparation method thereof Active CN108610047B (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110002874A (en) * 2019-04-30 2019-07-12 电子科技大学 A kind of ultralow temperature-sintered microwave dielectric ceramic material and preparation method thereof
CN110330334A (en) * 2019-08-01 2019-10-15 电子科技大学 Low-temperature sintering microwave medium material C a5Ni4-xZnxV6O24And preparation method thereof
CN110395984A (en) * 2019-08-01 2019-11-01 电子科技大学 A kind of low temperature sintering microwave ceramic material and preparation method thereof
CN111908920A (en) * 2020-07-31 2020-11-10 东莞市翔通光电技术有限公司 Barium-cobalt-zinc-niobium-based microwave dielectric ceramic and preparation method thereof
CN113582690A (en) * 2021-07-09 2021-11-02 电子科技大学 Ultralow temperature sintered microwave dielectric material Zn2V2O7And method for preparing the same
CN114550977A (en) * 2022-03-03 2022-05-27 太原理工大学 Low-temperature co-fired ceramic dielectric material and preparation method thereof
CN115872740A (en) * 2022-12-28 2023-03-31 北京工业大学 Ultralow temperature sintered low dielectric microwave dielectric ceramic and preparation method thereof

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110002874A (en) * 2019-04-30 2019-07-12 电子科技大学 A kind of ultralow temperature-sintered microwave dielectric ceramic material and preparation method thereof
CN110330334A (en) * 2019-08-01 2019-10-15 电子科技大学 Low-temperature sintering microwave medium material C a5Ni4-xZnxV6O24And preparation method thereof
CN110395984A (en) * 2019-08-01 2019-11-01 电子科技大学 A kind of low temperature sintering microwave ceramic material and preparation method thereof
CN111908920A (en) * 2020-07-31 2020-11-10 东莞市翔通光电技术有限公司 Barium-cobalt-zinc-niobium-based microwave dielectric ceramic and preparation method thereof
CN113582690A (en) * 2021-07-09 2021-11-02 电子科技大学 Ultralow temperature sintered microwave dielectric material Zn2V2O7And method for preparing the same
CN114550977A (en) * 2022-03-03 2022-05-27 太原理工大学 Low-temperature co-fired ceramic dielectric material and preparation method thereof
CN114550977B (en) * 2022-03-03 2024-01-30 太原理工大学 Low-temperature co-fired ceramic dielectric material and preparation method thereof
CN115872740A (en) * 2022-12-28 2023-03-31 北京工业大学 Ultralow temperature sintered low dielectric microwave dielectric ceramic and preparation method thereof
CN115872740B (en) * 2022-12-28 2023-10-27 北京工业大学 Ultralow-temperature sintered low-dielectric microwave dielectric ceramic and preparation method thereof

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