CN103979963A - High-dielectric-constant NP0 type dielectric ceramic and preparing method of high-dielectric-constant NP0 type dielectric ceramic - Google Patents
High-dielectric-constant NP0 type dielectric ceramic and preparing method of high-dielectric-constant NP0 type dielectric ceramic Download PDFInfo
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- CN103979963A CN103979963A CN201410175154.4A CN201410175154A CN103979963A CN 103979963 A CN103979963 A CN 103979963A CN 201410175154 A CN201410175154 A CN 201410175154A CN 103979963 A CN103979963 A CN 103979963A
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Abstract
The invention discloses high-dielectric-constant NP0 type dielectric ceramic and a preparing method of the high-dielectric-constant NP0 type dielectric ceramic. The chemical formula of the high-dielectric-constant NP0 type dielectric ceramic is (Bi<1.8>Zn<0.2>)(Zn<0.5>Nb<1.5-x>Sn<x>)O<7.15-x/2>(0<=x<=0.1). According to the preparing method, Bi2O3, Nb2O5, SnO2 and ZnO are adopted as raw materials, calcining is carried out at 750 DEG C, and sintering is carried out at 950 to 1025 DEG C; the proportion of Bi to Zn in a position A in a pyrochlore structure is changed, and then, Sn<4+> with high ionic polarizability is adopted for replacing Nb<5+> with similar radii in a position B, so the dielectric constant of a system is increased. The high-dielectric-constant NP0 type dielectric ceramic and the preparing method have the advantages that the dielectric constant is between 120 and 170, the temperature coefficient of capacitance (TCC) is in a range of -29*10<-6>/DEG C to 22*10<-6>/DEG C, the high-dielectric-constant NP0 type dielectric ceramic and the method can be used for preparing multilayer ceramic capacitors (MLCC), the sintering is carried out at a lower temperature, and the cost of multilayer devices is greatly reduced.
Description
Technical field
The invention belongs to a kind of the take ceramic composition that composition is feature, particularly high-frequency dielectric ceramic of a kind of novel high-k, temperature-stable and preparation method thereof.
Background technology
In recent years, along with the develop rapidly of electronics and information industry, for the electronic component of the equipment such as mobile communication, constantly pursuing miniaturization, high frequency and high reliability.The advantages such as use that multiple-layer sheet ceramic capacitor (MLCC) relies on its small volume, large specific volume, humidity, long lifetime, high reliability, chip type and adapts to the unicircuit from low frequency to uhf-range, have obtained development rapidly.
NP0 electrical condenser is a kind of the most frequently used I class ceramic condenser with temperature compensation characteristic, and its electrical capacity is highly stable, is widely used in the tank capacitance of vibrator, resonator and the coupling capacity in high frequency circuit.According to the international EIA of Electronic Industries Association USA (Electronic Industries Association) standard, NP0 temperature-stable electrical condenser refers to that take the capacitance of 25 ℃ is benchmark, in temperature within the scope of-55 ℃ to+125 ℃, temperature coefficient of capacitance (TCC)≤± 30ppm/ ℃.Adopt the NP0 characteristic stupalith of MLCC technology to there is 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, can adapt to the use of the unicircuit from low frequency to uhf-range, and greatly improve circuit packing density, dwindle machine volume, become and can adapt to one of element of electronic technology develop rapidly.
Bi
2o
3-ZnO-Nb
2o
5three component system media ceramic has pyrochlore structure, and its molecular formula can be written as A
2b
2o
6o ', with change of component, there are two primary structures with different dielectric properties in this 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/ ℃) 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/ ℃).This system has the advantages such as sintering temperature is low, specific inductivity is high, dielectric loss is little, and it does not react with Ag electrode size, can adopt the silver-colored palladium slurry of low palladium content as interior electrode, can be applicable to the preparation of multiple-layer sheet ceramic capacitor (MLCC), and greatly reduce the cost of multilayer device.Yet the temperature factor of system is larger, for meeting practical application, reconcile the temperature factor of system, further improve the specific inductivity of system, become the direction that investigator makes great efforts.
Summary of the invention
Object of the present invention is that a kind of high-k NP0 type media ceramic and preparation method thereof is provided on the basis of existing technology.
The present invention is achieved by following technical solution.
A high-k NP0 type media ceramic, chemical formula is (Bi
1.8zn
0.2) (Zn
0.5nb
1.5-xsn
x) O
7.15-x/2(0≤x≤0.1);
The preparation method of this high-k NP0 type media ceramic, has following steps:
(1) by raw material Bi
2o
3, Nb
2o
5, SnO
2, ZnO is by (Bi
1.8zn
0.2) (Zn
0.5nb
1.5-xsn
x) O
7.15-x/2the stoichiometric ratio weigh batching of (0≤x≤0.1);
(2) powder of step (1) preparation is put into ball grinder, add zirconia ball and deionized water, ball milling 4 hours; Raw material after ball milling is placed in to infrared drying oven and dries, after drying, cross 40 mesh sieves, obtain evengranular powder;
(3) powder after step (2) processing is calcined at 750 ℃, be incubated 4 hours, synthetic principal crystalline phase;
(4) polyvinyl alcohol that in the powder after step (3) is processed, additional mass percent is 0.75%, put into ball grinder, add zirconia ball and deionized water, ball milling 12 hours, after drying, cross 80 mesh sieves, then with the pressure of 2MPa, be pressed into base substrate with powder compressing machine;
(5) by the base substrate after step (4) moulding in 950～1025 ℃ of sintering, be incubated 4 hours, make high-k NP0 type media ceramic;
(6) the high-frequency dielectric performance of test article.
The bake out temperature of described step (2) and step (4) is 100 ℃.
The mass ratio of the ceramic powder of described step (2) and step (4) and zirconia ball, deionized water is 1: 1: 2.
The base substrate of described step (4) is the disk of Φ 10mm * 1mm.
The sintering temperature of described step (5) is 1000 ℃.
Beneficial effect of the present invention: be to provide a kind of high-k temperature-stable ceramic capacitor dielectric material, (the Bi making
1.8zn
0.2) (Zn
0.5nb
1.5-xsn
x) O
7.15-x/2(0≤x≤0.1) dielectric material, its sintering temperature is 950～1025 ℃, DIELECTRIC CONSTANT ε
rbetween 120～170, temperature coefficient of capacitance TCC is-29 * 10
-6/ ℃～22 * 10
-6/ ℃ within the scope of, the high-frequency dielectric ceramic material that this method makes, has higher specific inductivity, meets the standard of NP0 type dielectric material, and can be used for the preparation of multiple-layer sheet ceramic capacitor (MLCC).
Embodiment
The present invention is raw materials used is commercially available analytical reagent, and below by specific embodiment, the invention will be further described, and specific embodiment is as follows.
Embodiment 1
(1) by raw material Bi
2o
3, Nb
2o
5, SnO
2, ZnO is by (Bi
1.8zn
0.2) (Zn
0.5nb
1.4sn
0.1) O
7.1stoichiometric ratio weigh batching;
(2) powder of step (1) preparation is put into ball grinder, add zirconia ball and deionized water, ball milling 4 hours, the mass ratio of powder and zirconia ball, deionized water is 1: 1: 2; Raw material after ball milling is placed in to infrared drying oven and at 100 ℃, dries, after drying, cross 40 mesh sieves, obtain evengranular powder;
(3) powder step (2) being mixed is calcined at 750 ℃, is incubated 4 hours, synthetic principal crystalline phase;
(4) polyvinyl alcohol that in the powder after step (3) calcining, additional mass percent is 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, in 100 ℃ of rear mistake 80 mesh sieves of oven dry, then with powder compressing machine, with the pressure of 2MPa, be pressed into the base substrate of Φ 10mm * 1mm;
(5) by the base substrate after step (4) moulding in 1000 ℃ of sintering, be incubated 4 hours, make the low-temperature sintering NP0 type ceramic capacitor dielectric material of high-k;
(6) adopt Agilent4278A electric impedance analyzer to test its dielectric properties, under 1MHz, ε
r=170, tan δ=0.0045, TCC=0.37 * 10
-6/ ℃.
Embodiment 2-4
Embodiment 2-4 and the preparation technology's of embodiment 1 difference are the different of x and sintering temperature in chemical formula, and its corresponding dielectric properties refer to table 1.
Table 1
The present invention is not limited to above-described embodiment, and the variation of some details is possible, but therefore this do not run counter to scope and spirit of the present invention.
Claims (5)
1. a high-k NP0 type media ceramic, chemical formula is (Bi
1.8zn
0.2) (Zn
0.5nb
1.5-xsn
x) O
7.15-x/2(0≤x≤0.1);
The preparation method of this high-k NP0 type media ceramic, has following steps:
(1) by raw material Bi
2o
3, Nb
2o
5, SnO
2, ZnO is by (Bi
1.8zn
0.2) (Zn
0.5nb
1.5-xsn
x) O
7.15-x/2the stoichiometric ratio weigh batching of (0≤x≤0.1);
(2) powder of step (1) preparation is put into ball grinder, add zirconia ball and deionized water, ball milling 4 hours; Raw material after ball milling is placed in to infrared drying oven and dries, after drying, cross 40 mesh sieves, obtain evengranular powder;
(3) powder after step (2) processing is calcined at 750 ℃, be incubated 4 hours, synthetic principal crystalline phase;
(4) polyvinyl alcohol that in the powder after step (3) is processed, additional mass percent is 0.75%, put into ball grinder, add zirconia ball and deionized water, ball milling 12 hours, after drying, cross 80 mesh sieves, then with the pressure of 2MPa, be pressed into base substrate with powder compressing machine;
(5) by the base substrate after step (4) moulding in 950～1025 ℃ of sintering, be incubated 4 hours, make high-k NP0 type media ceramic;
(6) the high-frequency dielectric performance of test article.
2. high-k NP0 type media ceramic according to claim 1, is characterized in that, the bake out temperature of described step (2) and step (4) is 100 ℃.
3. high-k NP0 type media ceramic according to claim 1, is characterized in that, the mass ratio of the ceramic powder of described step (2) and step (4) and zirconia ball, deionized water is 1: 1: 2.
4. high-k NP0 type media ceramic according to claim 1, is characterized in that, the base substrate of described step (4) is the disk of Φ 10mm * 1mm.
5. high-k NP0 type media ceramic according to claim 1, is characterized in that, the sintering temperature of described step (5) is 1000 ℃.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104311011A (en) * | 2014-10-09 | 2015-01-28 | 天津大学 | Low-temperature sintering stable-temperature dielectric ceramic material |
| CN105777106A (en) * | 2016-03-04 | 2016-07-20 | 天津大学 | Low-temperature-sintered low-loss ceramic capacitor dielectric material |
| CN105801103A (en) * | 2016-02-23 | 2016-07-27 | 天津大学 | High-frequency dielectric ceramic material with high dielectric constant and low loss and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1431166A (en) * | 2003-01-17 | 2003-07-23 | 西安交通大学 | High frequency dielectric ceramic material sintered under low temp and its preparation |
-
2014
- 2014-04-28 CN CN201410175154.4A patent/CN103979963A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1431166A (en) * | 2003-01-17 | 2003-07-23 | 西安交通大学 | High frequency dielectric ceramic material sintered under low temp and its preparation |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104311011A (en) * | 2014-10-09 | 2015-01-28 | 天津大学 | Low-temperature sintering stable-temperature dielectric ceramic material |
| CN105801103A (en) * | 2016-02-23 | 2016-07-27 | 天津大学 | High-frequency dielectric ceramic material with high dielectric constant and low loss and preparation method thereof |
| CN105777106A (en) * | 2016-03-04 | 2016-07-20 | 天津大学 | Low-temperature-sintered low-loss ceramic capacitor dielectric material |
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Application publication date: 20140813 |