CN106892655A - A kind of high-k temperature-stable ceramic capacitor dielectric material - Google Patents

A kind of high-k temperature-stable ceramic capacitor dielectric material Download PDF

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CN106892655A
CN106892655A CN201710206414.3A CN201710206414A CN106892655A CN 106892655 A CN106892655 A CN 106892655A CN 201710206414 A CN201710206414 A CN 201710206414A CN 106892655 A CN106892655 A CN 106892655A
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temperature
ceramic capacitor
dielectric material
capacitor dielectric
stable ceramic
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李玲霞
郭千瑜
张帅
孙正
张宁
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Tianjin University
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Tianjin University
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    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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    • C04B35/63404Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
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    • H01B3/00Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/02Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
    • H01B3/12Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances ceramics
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G4/00Fixed capacitors; Processes of their manufacture
    • H01G4/002Details
    • H01G4/018Dielectrics
    • H01G4/06Solid dielectrics
    • H01G4/08Inorganic dielectrics
    • H01G4/12Ceramic dielectrics
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    • H01G4/1254Ceramic dielectrics characterised by the ceramic dielectric material based on niobium or tungsteen, tantalum oxides or niobates, tantalates
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    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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Abstract

The invention discloses a kind of high-k temperature-stable ceramic capacitor dielectric material, chemical formula Bi2Mg2/3Nb16/ 15Zr4/15O7.First by raw material Bi2O3、Nb2O5、ZrO2, MgO press chemical formula and weigh dispensing, by ball milling, drying, sieving, in synthesis principal crystalline phase is calcined at 750 DEG C, shaping is made required ceramic capacitor dielectric material after 900~950 DEG C of sintering.Between 144~160, nearly zero temperature coefficient of capacitance is 55 × 10 for dielectric constant of the present invention‑6/ DEG C~42 × 10‑6/ DEG C in the range of, for the preparation of multiple-layer sheet ceramic capacitor, with relatively low sintering temperature, reduce the cost of multilayer device.

Description

A kind of high-k temperature-stable ceramic capacitor dielectric material
Technical field
The invention belongs to a kind of ceramic composition being characterized with composition, more particularly to a kind of high-k temperature stabilization Type ceramic capacitor dielectric material and preparation method.
Background technology
With continuing to develop for modern communication technology, especially mobile communication and satellite communication towards highly reliable and small size Direction is developed, and requirement higher is proposed to microwave dielectric material.Microwave dielectric material refers to be applied to microwave frequency (mainly 300MHz~300GHz frequency ranges) as dielectric material and one or more dielectric material of function is completed in circuit.It is low temperature co-fired Ceramic technology is a kind of integrated assembly technology of multi-crossed disciplines for attracting people's attention of rising in recent years, because its excellent electronics, The characteristics such as thermodynamics have turned into future electronic component integration, modular preferred manner.However, research of the China to the technology The starting stage is still in, the material system and electronic device for possessing independent intellectual property right are considerably less, LTCC (LowTemperature Co-fired Ceramic LTCC, LTCC) raw material band still relied on from the import of the foreign vendor such as Ferro, Du Pont. Therefore, finding has relatively low sintering temperature, dielectric constant in interior seriation in a big way, the new LTCC of temperature coefficient adjustable control Material system turns into the focus of research.
Bi-based pyrochlor dielectric material is used as the emerging low-temperature co-burning ceramic material of a class, and its dielectric constant is high, and dielectric is damaged Consumption is small, and sintering temperature is low, and temperature coefficient of capacitance is adjustable and without Pb, is applied in high-frequency element.The system sintering temperature Less than 950 DEG C, temperature coefficient of capacitance is adjustable, permittivity εr>=80, dielectric loss is low, is not reacted with Ag electrode slurrys, can Using the silver-colored palladium slurry of low palladium content as interior electrode, the preparation of LTCC (LTCC) is can be applied to, while reducing many The cost of layer device
The content of the invention
The purpose of the present invention, is very low (TCC ≈ -400 × 10 of temperature coefficient of capacitance for overcoming current material-6/℃)、 It is unfavorable for the shortcoming of practical application, there is provided a kind of temperature-stable ceramic capacitor dielectric material and system with high-k Preparation Method.
The present invention is achieved by following technical solution.
A kind of high-k temperature-stable ceramic capacitor dielectric material, chemical formula is Bi2Mg2/3Nb16/15Zr4/ 15O7
The preparation method of the temperature-stable ceramic capacitor dielectric material of the high-k, with following steps:
(1) by raw material Bi2O3、Nb2O5、ZrO2, MgO press Bi2Mg2/3Nb16/15Zr4/15O7Chemical formula weighs dispensing;
(2) powder that step (1) is prepared is put into ball grinder, adds zirconia ball and deionized water, ball milling 4 hours; Raw material after ball milling is placed in infrared drying oven and is dried, 40 mesh sieves are crossed after drying, obtain evengranular powder;
(3) the evengranular powder after step (2) treatment is synthesized into principal crystalline phase in being calcined 4 hours at 750 DEG C;
(4) additional mass percent is 0.75% polyethylene in the powder of the synthesis principal crystalline phase after step (3) treatment Alcohol, is put into ball grinder, adds zirconia ball and deionized water, and ball milling 12 hours crosses 80 mesh sieves, then use pressed powder after drying It is base substrate that machine is compressing;
(5) base substrate after step (4) is molded is incubated 4 hours in 900~950 DEG C of sintering, is made high-k temperature Stabilization type ceramic capacitor dielectric material.
The drying temperature of the step (2) or step (4) is 100 DEG C.
The ceramic powder of the step (2) or step (4) is 1: 1: 2 with the mass ratio of zirconia ball, deionized water.
The base substrate of the step (4) is the disk of Φ 10mm × 1mm.
The pressure of the tablet press machine of the step (4) is 4MPa.
The sintering temperature of the step (5) is 925 DEG C.
The invention provides a kind of high-k temperature-stable ceramic capacitor dielectric material and preparation method thereof, system The Bi for obtaining2Mg2/3Nb16/15Zr4/15O7Material, is 900~950 DEG C with relatively low sintering temperature, dielectric constant high 144~ Between 160, nearly zero temperature coefficient of capacitance is -55 × 10-6/ DEG C~-42 × 10-6/ DEG C in the range of, can be used for multilayer sheet type The preparation of ceramic capacitor (MLCC), while material has relatively low sintering temperature, can substantially reduce the cost of multilayer device.
Specific embodiment
Below by specific embodiment, the invention will be further described, raw materials used in example to be the commercially available pure examination of analysis Agent, specific embodiment is as follows.
Embodiment 1
(1) by raw material Bi2O3、Nb2O5、ZrO2, MgO press Bi2Mg2/3Nb16/15Zr4/15O7Chemical formula weighs dispensing;
(2) powder by above-mentioned preparation is put into ball grinder, adds zirconia ball and deionized water, ball milling 4 hours, powder It is 1: 1: 2 with the mass ratio of zirconia ball, deionized water;Raw material after ball milling is placed in infrared drying oven in baking at 100 DEG C It is dry, 40 mesh sieves are crossed after drying, obtain evengranular powder;
(3) above-mentioned well mixed powder is synthesized into principal crystalline phase in being calcined 4 hours at 750 DEG C;
(4) additional mass percent is 0.75% polyvinyl alcohol in powder after firing, is put into ball grinder, is added Zirconia ball and deionized water, powder are 1: 1: 2, ball milling 12 hours, mistake after drying with the mass ratio of zirconia ball, deionized water 80 mesh sieves, then the base substrate of Φ 10mm × 1mm is pressed into the pressure of 4MPa with powder compressing machine;
(5) base substrate after above-mentioned shaping is incubated 4 hours in 925 DEG C of sintering, is made the low-temperature sintering temperature of high-k Degree stabilization type ceramic capacitor dielectric material;
(6) its dielectric properties, under 1MHz, ε are tested using Agilent 4278A electric impedance analyzersr=160, tan δ= 9.1, TCC=-42 × 10-6/℃。
Embodiment 2~4
Embodiment 2~4 is essentially identical with the preparation method of embodiment 1, is only different sintering temperature.
The sintering temperature and its dielectric properties of specific embodiment refer to table 1.
Table 1
The present invention is not limited to above-described embodiment, and the change of some details is possible, but therefore this do not run counter to this hair Bright scope and spirit.

Claims (6)

1. a kind of high-k temperature-stable ceramic capacitor dielectric material, chemical formula is Bi2Mg2/3Nb16/15Zr4/15O7
The preparation method of the high-k temperature-stable ceramic capacitor dielectric material, with following steps:
(1) by raw material Bi2O3、Nb2O5、ZrO2, MgO press Bi2Mg2/3Nb16/15Zr4/15O7Chemical formula weighs dispensing;
(2) powder that step (1) is prepared is put into ball grinder, adds zirconia ball and deionized water, ball milling 4 hours;By ball Raw material after mill is placed in infrared drying oven and dries, and 40 mesh sieves are crossed after drying, obtains evengranular powder;
(3) the evengranular powder after step (2) treatment is synthesized into principal crystalline phase in being calcined 4 hours at 750 DEG C;
(4) additional mass percent is 0.75% polyvinyl alcohol in the powder of the synthesis principal crystalline phase after step (3) treatment, is put Enter in ball grinder, add zirconia ball and deionized water, ball milling 12 hours crosses 80 mesh sieves, then use powder compressing machine pressure after drying System is shaped to base substrate;
(5) base substrate after step (4) is molded is incubated 4 hours in 900~950 DEG C of sintering, is made high-k temperature stabilization Type ceramic capacitor dielectric material.
2. a kind of temperature-stable ceramic capacitor dielectric material with high dielectric constant according to claim 1, Characterized in that, the drying temperature of the step (2) or step (4) is 100 DEG C.
3. a kind of high-k temperature-stable ceramic capacitor dielectric material according to claim 1, its feature exists In ceramic powder and the mass ratio of zirconia ball, deionized water of the step (2) or step (4) are 1: 1: 2.
4. a kind of high-k temperature-stable ceramic capacitor dielectric material according to claim 1, its feature exists In the base substrate of the step (4) is the disk of Φ 10mm × 1mm.
5. a kind of high-k temperature-stable ceramic capacitor dielectric material according to claim 1, its feature exists In the pressure of the tablet press machine of the step (4) is 4MPa.
6. a kind of high-k temperature-stable ceramic capacitor dielectric material according to claim 1, its feature exists In the sintering temperature of the step (5) is 925 DEG C.
CN201710206414.3A 2017-03-31 2017-03-31 A kind of high-k temperature-stable ceramic capacitor dielectric material Pending CN106892655A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108929110A (en) * 2018-08-13 2018-12-04 安徽长容电子有限公司 A kind of high pressure resistant temperature-stable ceramic capacitor dielectric material and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN101318815A (en) * 2008-05-30 2008-12-10 西安交通大学 Bismuth-based molybdenum-based microwave dielectric ceramic material sintered at ultra low temperature and manufacture of the same
CN104310986A (en) * 2014-10-09 2015-01-28 天津大学 High dielectric constant stable-temperature ceramic capacitor dielectric material
CN105801104A (en) * 2016-02-23 2016-07-27 天津大学 High dielectric constant temperature stable type ceramic capacitor dielectric material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101318815A (en) * 2008-05-30 2008-12-10 西安交通大学 Bismuth-based molybdenum-based microwave dielectric ceramic material sintered at ultra low temperature and manufacture of the same
CN104310986A (en) * 2014-10-09 2015-01-28 天津大学 High dielectric constant stable-temperature ceramic capacitor dielectric material
CN105801104A (en) * 2016-02-23 2016-07-27 天津大学 High dielectric constant temperature stable type ceramic capacitor dielectric material

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XINYOU HUANG ETAL.: "Influence of Titanium Ion Doped Amount on the Dielectric Property of BMNT Ceramics", 《ADVANCED MATERIALS RESEARCH VOLS.》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108929110A (en) * 2018-08-13 2018-12-04 安徽长容电子有限公司 A kind of high pressure resistant temperature-stable ceramic capacitor dielectric material and preparation method thereof

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Application publication date: 20170627