CN105801104B - A kind of high dielectric constant temperature-stable ceramic capacitor dielectric material - Google Patents
A kind of high dielectric constant temperature-stable ceramic capacitor dielectric material Download PDFInfo
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- C04B35/453—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 zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
Abstract
The invention discloses a kind of high dielectric constant temperature-stable ceramic capacitor dielectric material, chemical formula Bi2Mg1/3Mn1/ 3Nb4/3O7.First by raw material Bi2O3、Nb2O5、MnCO3, MgO by chemical formula weigh ingredient, through ball milling, drying, calcined at 750 DEG C after sieving, synthesize principal crystalline phase；The polyvinyl alcohol that additional mass percent is 0.75% again, then after ball milling, drying, sieving, compression moulding is green body；Green body is sintered in 950~1000 DEG C, and high dielectric constant temperature-stable ceramic capacitor dielectric material is made.The present invention has lower sintering temperature (950~1000 DEG C), high dielectric constant (175~190), nearly zero temperature coefficient of capacitance (- 29 × 10‑6/ DEG C~-18 × 10‑6/ DEG C), it is used for the preparation of multiple-layer sheet ceramic capacitor (MLCC), reduces the cost of multilayer device.
Description
Technical field
The ceramic composition that the invention belongs to a kind of characterized by ingredient, in particular to a kind of high dielectric constant temperature are stablized
Type ceramic capacitor dielectric material and preparation method.
Background technique
As the continuous development of modern communication technology, especially mobile communication and satellite communication are towards highly reliable and small size
Direction is developed, and to microwave dielectric material, more stringent requirements are proposed.Microwave dielectric material refers to applied to microwave frequency (mainly
300MHz~300GHz frequency range) as dielectric material and the dielectric materials of one or more functions is completed in circuit.This requires
Microwave dielectric material has high permittivity εr, low dielectric loss tan δ, temperature coefficient of capacitance τεClose to zero or adjustable
Section.
Bi-based pyrochlor system is a kind of emerging low-temperature sintered ceramics material, can be used as the microwave-medium material of high dielectric constant
Material, has the characteristics that high-performance has concurrently with low-temperature sintering, such as dielectric constant height (εr>=80), dielectric loss is small, and sintering temperature is low,
Temperature coefficient adjustable and the advantage for being free of Pb, quite by the concern of domestic and international investigation of materials person since appearance.And it is not and in Ag
Electrode slurry reacts, and the silver-colored palladium slurry of low palladium content can be used as interior electrode, be applied to multiple-layer sheet ceramic capacitor
(MLCC) preparation, and substantially reduce the cost of multilayer device.However, very low (the TCC ≈-of the temperature coefficient of capacitance of material
400×10-6/ DEG C), it is unfavorable for practical application.Therefore, it under conditions of keeping high dielectric constant, reduces dielectric loss, obtain closely
Zero temperature coefficient of capacitance and reduction sintering temperature etc. become researcher's critical issue urgently to be solved.
Summary of the invention
The purpose of the present invention is to solve very low (≈ -400 × 10 TCC of temperature coefficient of capacitance-6/ DEG C) ceramic material
Material, is unfavorable for the problem of practical application.One kind is provided under conditions of keeping high dielectric constant, dielectric loss is reduced, obtains closely
Zero temperature coefficient of capacitance and the temperature-stable ceramic capacitor dielectric with high dielectric constant for reducing sintering temperature
Material and preparation method thereof.
The present invention is achieved by following technical solution.
A kind of high dielectric constant temperature-stable ceramic capacitor dielectric material, chemical formula Bi2Mg1/3Mn1/3Nb4/3O7。
The preparation method of above-mentioned ceramic capacitor dielectric material has following steps：
(1) by raw material Bi2O3、Nb2O5、MnCO3, MgO press Bi2Mg1/3Mn1/3Nb4/3O7Chemical formula weighs ingredient；
(2) powder that step (1) is prepared is put into ball grinder, addition zirconia ball and deionized water, ball milling 4 hours；
Raw material after ball milling is placed in infrared drying oven and is dried, 40 meshes are crossed after drying, obtain evengranular powder；
(3) by step (2), treated that powder is calcined 4 hours at 750 DEG C, synthesizes principal crystalline phase；
(4) polyvinyl alcohol that additional mass percent is 0.75% in the powder after step (3) synthesize principal crystalline phase, is put into
In ball grinder, be added zirconia ball and deionized water, ball milling 12 hours, cross 80 meshes after drying, then with powder compressing machine with
The pressure compression moulding of 4MPa is green body；
(5) step (4) green body after molding is sintered in 950~1000 DEG C, keeps the temperature 4 hours, high dielectric constant temperature is made
Spend stabilization type ceramic capacitor dielectric material.
The drying temperature of the step (2) and step (4) is 100 DEG C.
The mass ratio of the ceramic powder of the step (2) and step (4) and zirconia ball, deionized water is 1: 1: 2.
The green body of the step (4) is the disk of Φ 10mm × 1mm.
The blank forming pressure of the step (4) is 4MPa.
The sintering temperature of the step (5) is 975 DEG C, soaking time 4h.
Beneficial effects of the present invention are as follows：
A kind of high dielectric constant temperature-stable ceramic capacitor dielectric material and preparation method thereof is provided, it is obtained
Bi2Mg1/3Mn1/3Nb4/3O7Material has lower sintering temperature (950~1000 DEG C), high dielectric constant (175~190),
Nearly zero temperature coefficient of capacitance (- 29 × 10-6/ DEG C~-18 × 10-6/ DEG C), it can be used for multiple-layer sheet ceramic capacitor
(MLCC) preparation substantially reduces the cost of multilayer device.
Specific embodiment
Below by specific embodiment, the invention will be further described, and raw materials used in example is the commercially available pure examination of analysis
Agent, specific embodiment are as follows.
Embodiment 1
(1) by raw material Bi2O3、Nb2O5、MnCO3, MgO press Bi2Mg1/3Mn1/3Nb4/3O7Chemical formula weighs ingredient；
(2) powder by above-mentioned preparation is put into ball grinder, addition zirconia ball and deionized water, and ball milling 4 hours, powder
Mass ratio with zirconia ball, deionized water is 1: 1: 2；Raw material after ball milling is placed in infrared drying oven at 100 DEG C and is dried
It is dry, 40 meshes are crossed after drying, obtain evengranular powder；
(3) above-mentioned uniformly mixed powder is calcined 4 hours at 750 DEG C, synthesizes principal crystalline phase；
(4) polyvinyl alcohol that additional mass percent is 0.75% in powder after firing, is put into ball grinder, is added
Zirconia ball and deionized water, powder and zirconia ball, deionized water mass ratio be 1: 1: 2, ball milling 12 hours, mistake after drying
80 meshes, then the green body for being Φ 10mm × 1mm with the pressure compression moulding of 4MPa with powder compressing machine；
(5) above-mentioned green body after molding is sintered in 950 DEG C, keeps the temperature 4 hours, the low-temperature sintering temperature of high dielectric constant is made
Spend stabilization type ceramic capacitor dielectric material；
(6) its dielectric properties is tested using Agilent 4278A impedance analyzer, under 1MHz, εr=176, TCC=-26
×10-6/℃。
Embodiment 2
(1) by raw material Bi2O3、Nb2O5、MnCO3, ZnO press (Bi1.5Mn0.5)(Zn0.5Nb1.5)O7Chemical formula weighs ingredient；
(2) powder by above-mentioned preparation is put into ball grinder, addition zirconia ball and deionized water, and ball milling 4 hours, powder
Mass ratio with zirconia ball, deionized water is 1: 1: 2；Raw material after ball milling is placed in infrared drying oven at 100 DEG C and is dried
It is dry, 40 meshes are crossed after drying, obtain evengranular powder；
(3) above-mentioned uniformly mixed powder is calcined 4 hours at 750 DEG C, synthesizes principal crystalline phase；
(4) polyvinyl alcohol that additional mass percent is 0.75% in powder after firing, is put into ball grinder, is added
Zirconia ball and deionized water, powder and zirconia ball, deionized water mass ratio be 1: 1: 2, ball milling 12 hours, mistake after drying
80 meshes, then the green body for being Φ 10mm × 1mm with the pressure compression moulding of 4MPa with powder compressing machine；
(5) above-mentioned green body after molding is sintered in 975 DEG C, keeps the temperature 4 hours, the low-temperature sintering temperature of high dielectric constant is made
Spend stabilization type ceramic capacitor dielectric material；
(6) its dielectric properties is tested using Agilent 4278A impedance analyzer, under 1MHz, εr=180, TCC=-18
×10-6/℃。
Embodiment 3
(1) by raw material Bi2O3、Nb2O5、MnCO3, MgO press Bi2Mg1/3Mn1/3Nb4/3O7Chemical formula weighs ingredient；
(2) powder by above-mentioned preparation is put into ball grinder, addition zirconia ball and deionized water, and ball milling 4 hours, powder
Mass ratio with zirconia ball, deionized water is 1: 1: 2；Raw material after ball milling is placed in infrared drying oven at 100 DEG C and is dried
It is dry, 40 meshes are crossed after drying, obtain evengranular powder；
(3) above-mentioned uniformly mixed powder is calcined 4 hours at 750 DEG C, synthesizes principal crystalline phase；
(4) polyvinyl alcohol that additional mass percent is 0.75% in powder after firing, is put into ball grinder, is added
Zirconia ball and deionized water, powder and zirconia ball, deionized water mass ratio be 1: 1: 2, ball milling 12 hours, mistake after drying
80 meshes, then the green body for being Φ 10mm × 1mm with the pressure compression moulding of 4MPa with powder compressing machine；
(5) above-mentioned green body after molding is sintered in 1000 DEG C, keeps the temperature 4 hours, the low-temperature sintering of high dielectric constant is made
Temperature-stable ceramic capacitor dielectric material；
(6) its dielectric properties is tested using Agilent 4278A impedance analyzer, under 1MHz, εr=178, TCC=-24
×10-6/℃。
The present invention is not limited to the above embodiment, and the variation of some details is possible, but therefore this does not violate this hair
Bright scope and spirit.
Claims (5)
1. a kind of high dielectric constant temperature-stable ceramic capacitor dielectric material, chemical formula Bi2Mg1/3Mn1/3Nb4/3O7；
The preparation method of above-mentioned ceramic capacitor dielectric material has following steps：
(1) by raw material Bi2O3、Nb2O5、MnCO3, MgO press Bi2Mg1/3Mn1/3Nb4/3O7Chemical formula weighs ingredient；
(2) powder that step (1) is prepared is put into ball grinder, addition zirconia ball and deionized water, ball milling 4 hours；By ball
Raw material after mill, which is placed in infrared drying oven, dries, and 40 meshes are crossed after drying, obtain evengranular powder；
(3) by step (2), treated that powder is calcined 4 hours at 750 DEG C, synthesizes principal crystalline phase；
(4) polyvinyl alcohol that additional mass percent is 0.75% in the powder after step (3) synthesize principal crystalline phase, is put into ball milling
In tank, zirconia ball and deionized water is added, ball milling 12 hours, 80 meshes are crossed after drying, then with powder compressing machine with 4MPa's
Pressure compression moulding is green body；
(5) step (4) green body after molding is sintered in 950~1000 DEG C, keeps the temperature 4 hours, it is steady that high dielectric constant temperature is made
Sizing ceramic capacitor dielectric material.
2. a kind of high dielectric constant temperature-stable ceramic capacitor dielectric material according to claim 1, feature exist
In the drying temperature of the step (2) and step (4) is 100 DEG C.
3. a kind of high dielectric constant temperature-stable ceramic capacitor dielectric material according to claim 1, feature exist
In the powder and zirconia ball of the step (2) and step (4), the mass ratio of deionized water are 1: 1: 2.
4. a kind of high dielectric constant temperature-stable ceramic capacitor dielectric material according to claim 1, feature exist
In the green body of the step (4) is the disk of Φ 10mm × 1mm.
5. a kind of high dielectric constant temperature-stable ceramic capacitor dielectric material according to claim 1, feature exist
In the sintering temperature of the step (5) is 975 DEG C, soaking time 4h.
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| CN106631015A (en) * | 2016-11-18 | 2017-05-10 | 郑州丽福爱生物技术有限公司 | Molybdenum-containing bismuth-based pyrochlore high dielectric constant microwave dielectric material as well as preparation and application thereof |
| CN106927810A (en) * | 2017-03-08 | 2017-07-07 | 湖南云平环保科技有限公司 | Low temperature sintering high-dielectric constant dielectric material and its manufacture method |
| CN106892655A (en) * | 2017-03-31 | 2017-06-27 | 天津大学 | A kind of high-k temperature-stable ceramic capacitor dielectric material |
| CN107399967A (en) * | 2017-08-11 | 2017-11-28 | 天津大学 | A kind of ultra-low loss huge dielectric constant temperature-stable capacitor dielectric material |
| CN107459351A (en) * | 2017-08-31 | 2017-12-12 | 天津大学 | A kind of temperature-stable Dielectric Materials at Radio Frequencies |
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| FR2845685A1 (en) * | 2002-10-15 | 2004-04-16 | Thales Sa | Ceramic material with elevated permittivity for Low Temperature Co-firing Ceramics technology for production of high capacity condensers in very thin multi-layer structures |
| CN105000877A (en) * | 2015-07-21 | 2015-10-28 | 天津大学 | High-quality-factor temperature-stabilization type microwave dielectric material and preparation method thereof |
| CN105060892A (en) * | 2015-09-11 | 2015-11-18 | 天津大学 | Composite tantalate microwave dielectric ceramic with near-zero frequency temperature coefficient |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2845685A1 (en) * | 2002-10-15 | 2004-04-16 | Thales Sa | Ceramic material with elevated permittivity for Low Temperature Co-firing Ceramics technology for production of high capacity condensers in very thin multi-layer structures |
| CN105000877A (en) * | 2015-07-21 | 2015-10-28 | 天津大学 | High-quality-factor temperature-stabilization type microwave dielectric material and preparation method thereof |
| CN105060892A (en) * | 2015-09-11 | 2015-11-18 | 天津大学 | Composite tantalate microwave dielectric ceramic with near-zero frequency temperature coefficient |
Non-Patent Citations (1)
| Title |
|---|
| Structures, phase transformations, and dielectric properties of Bi2(Zn1-xMgx)2/3Nb4/3O7 pyrochlore ceramics as temperature stable LTCC material;Lingxia Li et al.;《Journal of Alloys and Compounds》;20140326;第604卷;说明书实验步骤部分，图1 * |
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