CN105565799A - Low-loss temperature-stable high-frequency dielectric ceramic - Google Patents
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Abstract
The invention discloses a low-loss temperature-stable high-frequency dielectric ceramic. A chemical formula of the low-loss temperature-stable high-frequency dielectric ceramic is Bi2(Zn1-xNix)2/3Nb4/3O7. An x in the chemical formula is 0.33-0.37. A method for preparing the low-loss temperature-stable high-frequency dielectric ceramic includes proportioning raw materials Bi2O3, ZnO, Nb2O5 and NiO according to the chemical formula, carrying out ball-milling on the raw materials, drying and sieving the raw materials to obtain powder with uniform particles, calcining the powder at the temperatures of 750 DEG C for 6 hours and synthesizing main crystal phases; adding polyvinyl alcohol into the preliminarily calcined powder, arranging the polyvinyl alcohol and the powder in a ball-milling tank to obtain mixtures, drying and sieving the mixtures and the pressing the mixtures to obtain blanks; sintering the blanks at the temperatures of 925-975 DEG C to obtain the low-loss temperature-stable high-frequency dielectric ceramic. The dielectric constant epsilon<r> of the low-loss temperature-stable high-frequency dielectric ceramic is 95-103, the dielectric loss tan delta of the low-loss temperature-stable high-frequency dielectric ceramic is smaller than or equal to 5*10<-4>, and the capacitance-temperature coefficient of the low-loss temperature-stable high-frequency dielectric ceramic ranges from -7*10<-6>/DEG C to 7*10<-6>/DEG C. The low-loss temperature-stable high-frequency dielectric ceramic has the advantages that the low-loss temperature-stable high-frequency dielectric ceramic can be used for manufacturing multilayer chip ceramic capacitors and is low in sintering temperature, and the production cost can be greatly reduced.
Description
Technical field
The invention belongs to a kind of take composition as the ceramic composition of feature, particularly a kind of low-loss temperature-stabilized high-frequency dielectric ceramic.
Background technology
Nowadays, electronic devices and components have entered novel high speed developing period.Along with the development of modern communication technology, the growth requirement of mobile communication, impels signal equipment to develop rapidly to mobility, portability, miniaturization and microminiaturized aspect, proposes renewal, higher requirement to components and parts.In laminated ceramic capacitor (MLCC) electronic market, (capacitance of 25 DEG C is benchmark to NP0, within the scope of temperature from-55 DEG C to+125 DEG C, temperature coefficient of capacitance (TCC)≤± 30ppm/ DEG C) electrical condenser is the multi-layer ceramic capacitance with temperature compensation characteristic, its specific inductivity and dielectric loss more stable.The NP0 characteristic stupalith of employing MLCC technology has the plurality of advantages such as volume is little, specific volume large, humidity, long lifetime, chip type, parasitic inductance is low, high frequency characteristics is good, the requirement of circuit integration, microminiaturization, high reliability and low cost can be met, become and can adapt to one of element of electronic technology develop rapidly.
Bi
2o
3-ZnO-Nb
2o
5ternary system ceramics medium, it has the advantages such as sintering temperature is low, specific inductivity is high, dielectric loss is little, temperature coefficient of capacitance is adjustable, and it does not react with Ag electrode size, by adopting the silver-colored palladium slurry of low palladium content as interior electrode, can be applicable to the preparation of LTCC (LTCC), and greatly reduce the cost of multilayer device.According to the difference of stoichiometric equation, there is the primary structure that two have different dielectric properties in BZN system pottery: (Bi
1.5zn
0.5) (Zn
0.5nb
1.5) O
7(α-BZN) cubic pyrochlore (ε
r≈ 150, tan δ≤4 × 10
-4, TCC ≈-400 × 10
-6/ DEG C) and Bi
2zn
2/3nb
4/3o
7(β-BZN) monocline titanium zirconium thorium structure (ε
r≈ 80, tan δ≤2 × 10
-4, TCC ≈ 170 × 10
-6/ DEG C).The BZN stupalith of two kinds of structures has the contrary temperature coefficient of capacitance of symbol.For meeting practical application, the temperature coefficient of capacitance of regulation system, adapts to severe applied environment, becomes the direction that investigator makes great efforts.
Summary of the invention
Object of the present invention, being for meeting practical application, adapting to severe applied environment, provides a kind of low loss capacitance amount temperature coefficient nearly zero type media ceramic electric capacity.
The present invention is achieved by following technical solution.
A kind of low-loss temperature-stabilized high-frequency dielectric ceramic, chemical formula is Bi
2(Zn
1-xni
x)
2/3nb
4/3o
7, x=0.32 ~ 0.35;
The preparation method of this low-loss temperature-stabilized high-frequency dielectric ceramic, has following steps:
(1) by raw material Bi
2o
3, ZnO, Nb
2o
5, NiO presses Bi
2(Zn
1-xni
x)
2/3nb
4/3o
7, x=0.32 ~ 0.35 chemical formula weigh batching;
(2) powder that step (1) is prepared is put into ball grinder, add zirconia ball and deionized water, ball milling 6 hours; Raw material after ball milling is placed in infrared drying oven and dries, and crosses 40 mesh sieves, obtains evengranular powder;
(3) step (2) evengranular powder is calcined 6 hours at 750 DEG C, synthesis principal crystalline phase;
(4) in the powder after step (3) pre-burning, additional mass percent is the polyvinyl alcohol of 0.75%, put into ball grinder, add zirconia ball and deionized water, ball milling 12 hours, cross 80 mesh sieves after drying, then be pressed into base substrate with powder compressing machine with the pressure of 4MPa;
(5) by the base substrate after shaping for step (4) in 925 ~ 975 DEG C of sintering, be incubated 5 hours, make low-loss temperature-stabilized high-frequency dielectric ceramic.
Described step (2) is 100 DEG C with the bake out temperature in step (4).
The mass ratio of the ceramic powder in described step (2) and step (4) and zirconia ball, deionized water is 1: 1: 2.
Base substrate in described step (4) is the disk of Φ 10mm × 1mm.
Sintering temperature in described step (5) is 950 DEG C, is incubated 5 hours.
The invention provides the high-frequency dielectric ceramic material of a kind of low-temperature sintering, low-loss, nearly zero type of temperature factor, obtained Bi
2(Zn
1-xni
x)
2/3nb
4/3o
7, x=0.32 ~ 0.35 dielectric material, its sintering temperature is 925 ~ 975 DEG C, DIELECTRIC CONSTANT ε
rbetween 95 ~ 103, dielectric loss tan δ≤5 × 10
-4, temperature coefficient of capacitance TCC is-7 × 10
-6/ DEG C ~ 7 × 10
-6/ DEG C within the scope of.High-frequency dielectric ceramic material of the present invention, can be used for the preparation of multiple-layer sheet ceramic capacitor (MLCC), and in addition, this material also has lower sintering temperature, greatly can reduce the cost producing laminated ceramic capacitor.
Embodiment
Below by specific embodiment, the invention will be further described, raw materials usedly in example is commercially available analytical reagent, and specific embodiment is as follows.
Embodiment 1
(1) by raw material Bi
2o
3, ZnO, Nb
2o
5, NiO presses Bi
2(Zn
1-xni
x)
2/3nb
4/3o
7, the chemical formula weigh batching of x=0.35;
(2) powder of above-mentioned preparation is put into ball grinder, add zirconia ball and deionized water, ball milling 6 hours, the mass ratio of powder and zirconia ball, deionized water is 1: 1: 2; Raw material after ball milling is placed in infrared drying oven in 100 DEG C of oven dry, crosses 40 mesh sieves, obtain evengranular powder after drying;
(3) the above-mentioned powder mixed is calcined 6 hours at 750 DEG C, synthesis principal crystalline phase;
(4) in powder after firing, additional mass percent is the polyvinyl alcohol of 0.75%, put into ball grinder, add zirconia ball and deionized water, the mass ratio of powder and zirconia ball, deionized water is 1: 1: 2, ball milling 12 hours, cross 80 mesh sieves after drying, then be pressed into the base substrate of Φ 10mm × 1mm with powder compressing machine with the pressure of 4MPa;
(5) by above-mentioned shaping after base substrate in 950 DEG C sintering 5 hours, make low-loss temperature-stabilized high-frequency dielectric ceramic material;
(6) Agilent4278A electric impedance analyzer is adopted to test its dielectric properties, under 1MHz, ε
r=102, tan δ=4.3 × 10
-4, TCC=-5 × 10
-6/ DEG C.
Embodiment 2-4
Main technologic parameters and the dielectric properties of embodiment 2-4 refer to table 1, 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 do not run counter to scope and spirit of the present invention.
Claims (5)
1. a low-loss temperature-stabilized high-frequency dielectric ceramic, chemical formula is Bi
2(Zn
1-xni
x)
2/3nb
4/3o
7, x=0.32 ~ 0.35.
The preparation method of this low-loss temperature-stabilized high-frequency dielectric ceramic, has following steps:
(1) by raw material Bi
2o
3, ZnO, Nb
2o
5, NiO presses Bi
2(Zn
1-xni
x)
2/3nb
4/3o
7, x=0.32 ~ 0.35 chemical formula weigh batching;
(2) powder that step (1) is prepared is put into ball grinder, add zirconia ball and deionized water, ball milling 6 hours; Raw material after ball milling is placed in infrared drying oven and dries, and crosses 40 mesh sieves, obtains evengranular powder;
(3) step (2) evengranular powder is calcined 6 hours at 750 DEG C, synthesis principal crystalline phase;
(4) in the powder after step (3) pre-burning, additional mass percent is the polyvinyl alcohol of 0.75%, put into ball grinder, add zirconia ball and deionized water, ball milling 12 hours, cross 80 mesh sieves after drying, then be pressed into base substrate with powder compressing machine with the pressure of 4MPa;
(5) by the base substrate after shaping for step (4) in 925 ~ 975 DEG C of sintering, be incubated 5 hours, make low-loss temperature-stabilized high-frequency dielectric ceramic.
2. a kind of low-loss temperature-stabilized high-frequency dielectric ceramic according to claim 1, is characterized in that, described step (2) is 100 DEG C with the bake out temperature in step (4).
3. a kind of low-loss temperature-stabilized high-frequency dielectric ceramic according to claim 1, is characterized in that, the mass ratio of the ceramic powder in described step (2) and step (4) and zirconia ball, deionized water is 1: 1: 2.
4. a kind of low-loss temperature-stabilized high-frequency dielectric ceramic according to claim 1, is characterized in that, the base substrate in described step (4) is the disk of Φ 10mm × 1mm.
5. a kind of low-loss temperature-stabilized high-frequency dielectric ceramic according to claim 1, is characterized in that, the sintering temperature in described step (5) is 950 DEG C, is incubated 5 hours.
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| CN105565799B CN105565799B (en) | 2017-12-19 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| 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 |
| CN110156455A (en) * | 2019-07-04 | 2019-08-23 | 贵州振华电子信息产业技术研究有限公司 | A kind of bismuth oxide-niobium oxide base ltcc substrate material and preparation method thereof |
Citations (3)
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|---|---|---|---|---|
| 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 |
|---|
| LINGXIA LI等: "Structures, phase transformations, and dielectric properties of Bi2(Zn1-xMgx)2/3Nb4/3O7 pyrochlore ceramics as temperature stable LTCC material", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110156455A (en) * | 2019-07-04 | 2019-08-23 | 贵州振华电子信息产业技术研究有限公司 | A kind of bismuth oxide-niobium oxide base ltcc substrate material 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 |
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