CN105565799B - A kind of low-loss temperature-stabilized high-frequency dielectric ceramic - Google Patents
A kind of low-loss temperature-stabilized high-frequency dielectric ceramic Download PDFInfo
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Abstract
The invention discloses a kind of low-loss temperature-stabilized high-frequency dielectric ceramic, chemical formula Bi2(Zn1‑xNix)2/3Nb4/3O7, x=0.33~0.37.First by raw material Bi2O3、ZnO、Nb2O5, NiO press chemical formula dispensing, then through ball milling, dry, sieving, obtain evengranular powder, calcine 6 hours at 750 DEG C, synthesis principal crystalline phase；Powder China and foreign countries Polyvinyl alcohol after pre-burning, grinding jar, drying, after sieving, it is pressed into base substrate；Low-loss temperature-stabilized high-frequency dielectric ceramic is made in 925~975 DEG C of sintering in base substrate.The permittivity ε of the present inventionrFor 95~103, dielectric loss tan δ≤5 × 10‑4, temperature coefficient of capacitance is 7 × 10‑6/ DEG C~7 × 10‑6/℃.The present invention is used for the preparation of multiple-layer sheet ceramic capacitor, has relatively low sintering temperature, greatly reduces production cost.
Description
Technical field
The invention belongs to a kind of ceramic composition characterized by composition, more particularly to a kind of low-loss temperature-stabilized is high
Frequency media ceramic.
Background technology
Nowadays, electronic component comes into novel high speed developing period.With the continuous development of modern communication technology,
The growth requirement of mobile communication, communication equipment is promoted to be developed rapidly in terms of mobility, portability, miniaturization and miniaturization,
Renewal, higher requirement are proposed to component.In multilayer ceramic capacitor (MLCC) electronic market, NP0 (25 DEG C of electric capacity
On the basis of value, within the scope of temperature is from -55 DEG C to+125 DEG C, temperature coefficient of capacitance (TCC)≤± 30ppm/ DEG C) electric capacity
Device is the multi-layer ceramic capacitance for having temperature compensation characteristic, and its dielectric constant and dielectric loss are more stable.Using MLCC technologies
NP0 characteristic ceramic materials have small volume, specific volume big, humidity, the long-life, chip type, stray inductance is low, high frequency characteristics is good etc.
Plurality of advantages, can meet the requirement of circuit integration, miniaturization, high reliability and low cost, it has also become most adapt to electronics skill
One of element of art rapid development.
Bi2O3-ZnO-Nb2O5Ternary system ceramics medium, it has, and sintering temperature is low, dielectric constant is high, dielectric loss is small,
The advantages that temperature coefficient of capacitance is adjustable, and it does not react with Ag electrode sizes, by using the silver-colored palladium of low palladium content
Slurry can be applied to LTCC (LTCC) preparation, and substantially reduce the cost of multilayer device as interior electrode.According to
Two primary structures with different dielectric properties be present in the difference of stoichiometric equation, BZN systems ceramics：(Bi1.5Zn0.5)
(Zn0.5Nb1.5)O7(α-BZN) cubic pyrochlore (εr≈150,tanδ≤4×10-4,TCC≈-400×10-6/ DEG C) and
Bi2Zn2/3Nb4/3O7(β-BZN) monocline titanium zirconium thorium structure (εr≈80,tanδ≤2×10-4,TCC≈170×10-6/℃).Two kinds
The BZN ceramic materials of structure have the opposite temperature coefficient of capacitance of symbol.To meet practical application, the capacitance of regulation system
Temperature coefficient, severe application environment is adapted to, turn into the direction of researcher's effort.
The content of the invention
The purpose of the present invention, it is to meet practical application, adapts to severe application environment, there is provided a kind of low loss capacitance amount temperature
Spend the nearly zero type media ceramic electric capacity of coefficient.
The present invention is achieved by following technical solution.
A kind of low-loss temperature-stabilized high-frequency dielectric ceramic, chemical formula Bi2(Zn1-xNix)2/3Nb4/3O7, x=0.32
~0.35；
The preparation method of the low-loss temperature-stabilized high-frequency dielectric ceramic, there are following steps：
(1) by raw material Bi2O3、ZnO、Nb2O5, NiO press Bi2(Zn1-xNix)2/3Nb4/3O7, the chemical formula of x=0.32~0.35
Weigh dispensing；
(2) powder that step (1) is prepared is put into ball grinder, adds zirconia ball and deionized water, ball milling 6 hours；
Raw material after ball milling, which is placed in infrared drying oven, dries, and crosses 40 mesh sieves, obtains evengranular powder；
(3) step (2) evengranular powder is calcined 6 hours at 750 DEG C, synthesizes principal crystalline phase；
(4) additional mass percent is 0.75% polyvinyl alcohol in the powder after step (3) pre-burning, is put into ball grinder
In, zirconia ball and deionized water are added, ball milling 12 hours, 80 mesh sieves are crossed after drying, then with powder compressing machine with 4MPa pressure
Force and base substrate is made；
(5) base substrate after step (4) is molded is incubated 5 hours, it is stable that low-loss temperature is made in 925~975 DEG C of sintering
Type high-frequency dielectric ceramic.
The step (2) is 100 DEG C with the drying temperature in step (4).
The step (2) and the mass ratio of the ceramic powder in step (4) and zirconia ball, deionized water are 1: 1: 2.
The disk that base substrate in the step (4) is Φ 10mm × 1mm.
Sintering temperature in the step (5) is 950 DEG C, is incubated 5 hours.
The invention provides a kind of low-temperature sintering, low-loss, nearly zero type of temperature coefficient high-frequency dielectric ceramic material, be made
Bi2(Zn1-xNix)2/3Nb4/3O7, the dielectric material of x=0.32~0.35, its sintering temperature is 925~975 DEG C, permittivity εr
Between 95~103, dielectric loss tan δ≤5 × 10-4, temperature coefficient of capacitance TCC is -7 × 10-6/ DEG C~7 × 10-6/℃
In the range of.The high-frequency dielectric ceramic material of the present invention, available for multiple-layer sheet ceramic capacitor (MLCC) preparation, in addition, should
Material also has relatively low sintering temperature, can substantially reduce the cost of production multilayer ceramic capacitor.
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、ZnO、Nb2O5, NiO press Bi2(Zn1-xNix)2/3Nb4/3O7, x=0.35 chemical formula weighing
Dispensing；
(2) powder by above-mentioned preparation is put into ball grinder, adds zirconia ball and deionized water, ball milling 6 hours, powder
Mass ratio with zirconia ball, deionized water is 1: 1: 2；Raw material after ball milling is placed in infrared drying oven in 100 DEG C of drying, is dried
40 mesh sieves are crossed after dry, obtain evengranular powder；
(3) above-mentioned well mixed powder is calcined 6 hours at 750 DEG C, synthesizes principal crystalline phase；
(4) additional mass percent is 0.75% polyvinyl alcohol in powder after firing, is put into ball grinder, is added
The mass ratio of zirconia ball and deionized water, powder and zirconia ball, deionized water is 1: 1: 2, ball milling 12 hours, mistake after drying
80 mesh sieves, then Φ 10mm × 1mm base substrate is pressed into powder compressing machine with 4MPa pressure；
(5) base substrate after above-mentioned shaping is sintered 5 hours in 950 DEG C, low-loss temperature-stabilized high-frequency dielectric pottery is made
Ceramic material；
(6) its dielectric properties is tested using Agilent 4278A electric impedance analyzers, under 1MHz, εr=102, tan δ=4.3
×10-4, TCC=-5 × 10-6/℃。
Embodiment 2-4
Embodiment 2-4 main technologic parameters refer to table 1 with dielectric properties, and preparation process is identical with embodiment 1.
Table 1
The present invention is not limited to above-described embodiment, and the change of some details is possible, but therefore this does not run counter to this hair
Bright scope and spirit.
Claims (5)
1. a kind of low-loss temperature-stabilized high-frequency dielectric ceramic, chemical formula Bi2(Zn1-xNix)2/3Nb4/3O7, x=0.32~
0.35；
The preparation method of the low-loss temperature-stabilized high-frequency dielectric ceramic, there are following steps：
(1) by raw material Bi2O3、ZnO、Nb2O5, NiO press Bi2(Zn1-xNix)2/3Nb4/3O7, the chemical formula of x=0.32~0.35, which weighs, matches somebody with somebody
Material；
(2) powder that step (1) is prepared is put into ball grinder, adds zirconia ball and deionized water, ball milling 6 hours；Ball milling
Raw material afterwards, which is placed in infrared drying oven, dries, and crosses 40 mesh sieves, obtains evengranular powder；
(3) step (2) evengranular powder is calcined 6 hours at 750 DEG C, synthesizes principal crystalline phase；
(4) additional mass percent is 0.75% polyvinyl alcohol in the powder after step (3) pre-burning, is put into ball grinder,
Zirconia ball and deionized water are added, ball milling 12 hours, 80 mesh sieves are crossed after drying, then with powder compressing machine with 4MPa pressure pressure
Base substrate is made；
(5) base substrate after step (4) is molded is incubated 5 hours, low-loss temperature-stabilized height is made in 925~975 DEG C of sintering
Frequency media ceramic.
A kind of 2. low-loss temperature-stabilized high-frequency dielectric ceramic according to claim 1, it is characterised in that the step
(2) it is 100 DEG C with the drying temperature in step (4).
A kind of 3. low-loss temperature-stabilized high-frequency dielectric ceramic according to claim 1, it is characterised in that the step
(2) mass ratio with the powder in step (4) and zirconia ball, deionized water is 1: 1: 2.
A kind of 4. low-loss temperature-stabilized high-frequency dielectric ceramic according to claim 1, it is characterised in that the step
(4) disk that the base substrate in is Φ 10mm × 1mm.
A kind of 5. low-loss temperature-stabilized high-frequency dielectric ceramic according to claim 1, it is characterised in that the step
(5) sintering temperature in is 950 DEG C, is incubated 5 hours.
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| 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 |
| CN106830922A (en) * | 2017-03-14 | 2017-06-13 | 湖南云平环保科技有限公司 | Low temperature sintering high-dielectric constant ceramic material and its manufacture method |
| CN106966721A (en) * | 2017-04-26 | 2017-07-21 | 天津大学 | A kind of barium zirconium titanate ceramic with high-k and preparation method thereof |
| CN107459351A (en) * | 2017-08-31 | 2017-12-12 | 天津大学 | A kind of temperature-stable Dielectric Materials at Radio Frequencies |
| CN108484166A (en) * | 2018-01-19 | 2018-09-04 | 天津大学 | A kind of niobates LTCC microwave-medium ceramics and preparation method thereof |
| CN110156455B (en) * | 2019-07-04 | 2021-10-26 | 贵州振华电子信息产业技术研究有限公司 | Bismuth oxide-niobium oxide based LTCC substrate material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5449652A (en) * | 1993-06-04 | 1995-09-12 | Battelle Memorial Institute | Ceramic compositions for BZN dielectric resonators |
| 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 |
| CN103864427A (en) * | 2014-02-27 | 2014-06-18 | 天津大学 | Low-temperature sintering temperature-stabilizing type high-frequency dielectric ceramic and preparation method thereof |
-
2015
- 2015-12-18 CN CN201510974136.7A patent/CN105565799B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5449652A (en) * | 1993-06-04 | 1995-09-12 | Battelle Memorial Institute | Ceramic compositions for BZN dielectric resonators |
| 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 |
| CN103864427A (en) * | 2014-02-27 | 2014-06-18 | 天津大学 | Low-temperature sintering temperature-stabilizing type high-frequency dielectric ceramic and preparation method thereof |
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等;《Journal of Alloys and Compounds》;20140326;第604卷;说明书实验步骤部分，图1 * |
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