CN104311010B - A kind of low-loss temperature-stabilized radio ceramics condenser dielectric and preparation method thereof - Google Patents
A kind of low-loss temperature-stabilized radio ceramics condenser dielectric and preparation method thereof Download PDFInfo
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- CN104311010B CN104311010B CN201410527486.4A CN201410527486A CN104311010B CN 104311010 B CN104311010 B CN 104311010B CN 201410527486 A CN201410527486 A CN 201410527486A CN 104311010 B CN104311010 B CN 104311010B
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Abstract
The invention discloses a kind of low-loss temperature-stabilized radio ceramics condenser dielectric, chemical formula is (Bi
1.8zn
0.2) (Zn
0.6nb
1.4-2xsn
xw
x) O
7, x=0.02 ~ 0.05.First by raw material Bi
2o
3, ZnO, Nb
2o
5, SnO
2, WO
3by above-mentioned chemical formula weigh batching, through ball milling, dry, sieve, calcine after synthesize principal crystalline phase; Additional mass percent is the polyvinyl alcohol of 0.75% again, ball milling, dries, sieves, is pressed into base substrate; Base substrate, in 925 ~ 975 DEG C of sintering, makes low-loss temperature-stabilized high-frequency dielectric ceramic material.Sintering temperature of the present invention is 925 ~ 975 DEG C, DIELECTRIC CONSTANT ε
rbetween 93 ~ 101, dielectric loss tan δ≤5 × 10
-4, temperature coefficient of capacitance is-28 × 10
-6/ DEG C ~ 23 × 10
-6/ DEG C within the scope of, can be used for the preparation of multiple-layer sheet ceramic capacitor (MLCC), reduce the cost of device.
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 radio ceramics condenser dielectric and preparation method thereof.
Background technology
In recent years, along with the development of modern communication technology, especially mobile communication and satellite communication are towards highly reliable and small size future development, have higher requirement to microwave dielectric material.(capacitance of 25 DEG C is benchmark to the NP0 characteristic of employing MLCC technology, within the scope of temperature from-55 DEG C to+125 DEG C, temperature coefficient of capacitance (TCC)≤± 30ppm/ DEG C) stupalith have that volume is little, the plurality of advantages such as specific volume is large, humidity, life-span length, chip type, parasitic inductance is low, high frequency characteristics is good, the use of the unicircuit from low frequency to uhf-range can be adapted to, and greatly improve Circuit assembly density, reduce machine volume, 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, the silver-colored palladium slurry of low palladium content can be adopted as interior electrode, can be applicable to the preparation of LTCC (LTCC), and greatly reduce the cost of multilayer device.With change of component, Bi
2o
3-ZnO-Nb
2o
5there is the primary structure that two have different dielectric properties in 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, reconciling the temperature factor of system, becoming the direction that investigator makes great efforts.
Summary of the invention
Object of the present invention, being the shortcoming for overcoming media ceramic temperature stability difference prepared by prior art, providing a kind of low-loss temperature-stabilized high-frequency dielectric ceramic and preparation method thereof.
The present invention is achieved by following technical solution.
A kind of low-loss temperature-stabilized radio ceramics condenser dielectric, chemical formula is (Bi
1.8zn
0.2) (Zn
0.6nb
1.4-2xsn
xw
x) O
7, x=0.02 ~ 0.05;
The preparation method of this low-loss temperature-stabilized radio ceramics condenser dielectric, has following steps:
(1) by raw material Bi
2o
3, ZnO, Nb
2o
5, SnO
2, WO
3by (Bi
1.8zn
0.2) (Zn
0.6nb
1.4-2xsn
xw
x) O
7, the wherein chemical formula weigh batching of x=0.02 ~ 0.05;
(2) raw material that step (1) is prepared is put into ball grinder, add zirconia ball and deionized water, ball milling 4 hours; Raw material after ball milling is placed in infrared drying oven dry, crosses 40 mesh sieves after drying, obtain evengranular powder;
(3) powder after step (2) being processed is calcined 4 hours at 750 DEG C, synthesis principal crystalline phase;
(4) in the powder of step (3) synthesis principal crystalline phase, 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 2MPa;
(5) by the base substrate after shaping for step (4) in 925 ~ 975 DEG C of sintering, be incubated 4 hours, make low-loss temperature-stabilized high-frequency dielectric ceramic material;
(6) the high-frequency dielectric performance of test article.
The bake out temperature of described step (2) or step (4) is 100 DEG C.
The mass ratio of the ceramic powder of described step (2) or 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 950 DEG C.
Beneficial effect of the present invention: provide a kind of low-temperature sintering low-loss temperature-stable radio ceramics capacitor dielectric material (Bi
1.8zn
0.2) (Zn
0.6nb
1.4-2xsn
xw
x) O
7(x=0.02 ~ 0.05), its sintering temperature is 925 ~ 975 DEG C, DIELECTRIC CONSTANT ε
rbetween 93 ~ 101, dielectric loss tan δ≤5 × 10
-4, temperature coefficient of capacitance TCC is-28 × 10
-6/ DEG C ~ 23 × 10
-6/ DEG C within the scope of, high-frequency dielectric ceramic material of the present invention, has lower sintering temperature, can be used for the preparation of multiple-layer sheet ceramic capacitor (MLCC).
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.
(1) by raw material Bi
2o
3, ZnO, Nb
2o
5, SnO
2, WO
3by (Bi
1.8zn
0.2) (Zn
0.6nb
1.4-2xsn
xw
x) O
7, the wherein chemical formula weigh batching of x=0.02 ~ 0.05;
(2) raw material of above-mentioned preparation is put into ball grinder, add zirconia ball and deionized water, ball milling 4 hours, the mass ratio of raw material and zirconia ball, deionized water is 1: 1: 2; Raw material after ball milling is placed in infrared drying oven to dry at 100 DEG C, crosses 40 mesh sieves after drying, obtain evengranular powder;
(3) the above-mentioned powder mixed is calcined 4 hours at 750 DEG C, synthesis principal crystalline phase;
(4) synthesizing additional mass percent in the powder of principal crystalline phase is after firing 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 2MPa;
(5) by above-mentioned shaping after base substrate in 925 ~ 975 DEG C of sintering, be incubated 4 hours, make low-loss temperature-stabilized radio ceramics capacitor dielectric material;
(6) adopt Agilent4278A electric impedance analyzer to test its dielectric properties, test frequency is 1MHz.
Related process parameters and the dielectric properties of embodiment 1-4 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 scope and spirit of the present invention.
Claims (5)
1. a low-loss temperature-stabilized radio ceramics condenser dielectric, chemical formula is (Bi
1.8zn
0.2) (Zn
0.6nb
1.4-2xsn
xw
x) O
7, x=0.02 ~ 0.05;
The preparation method of this low-loss temperature-stabilized radio ceramics condenser dielectric, has following steps:
(1) by raw material Bi
2o
3, ZnO, Nb
2o
5, SnO
2, WO
3by (Bi
1.8zn
0.2) (Zn
0.6nb
1.4-2xsn
xw
x) O
7, the wherein chemical formula weigh batching of x=0.02 ~ 0.05;
(2) raw material that step (1) is prepared is put into ball grinder, add zirconia ball and deionized water, ball milling 4 hours; Raw material after ball milling is placed in infrared drying oven dry, crosses 40 mesh sieves after drying, obtain evengranular powder;
(3) powder after step (2) being processed is calcined 4 hours at 750 DEG C, synthesis principal crystalline phase;
(4) in the powder of step (3) synthesis principal crystalline phase, 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 2MPa;
(5) by the base substrate after shaping for step (4) in 925 ~ 975 DEG C of sintering, be incubated 4 hours, make low-loss temperature-stabilized high-frequency dielectric ceramic material;
(6) the high-frequency dielectric performance of test article.
2. a kind of low-loss temperature-stabilized radio ceramics condenser dielectric according to claim 1, is characterized in that, the bake out temperature of described step (2) or step (4) is 100 DEG C.
3. a kind of low-loss temperature-stabilized radio ceramics condenser dielectric according to claim 1, is characterized in that, the mass ratio of the ceramic powder of described step (2) or step (4) and zirconia ball, deionized water is 1: 1: 2.
4. a kind of low-loss temperature-stabilized radio ceramics condenser dielectric according to claim 1, is characterized in that, the base substrate of described step (4) is the disk of Φ 10mm × 1mm.
5. a kind of low-loss temperature-stabilized radio ceramics condenser dielectric according to claim 1, is characterized in that, the sintering temperature of described step (5) is 950 DEG C.
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| CN104311010B true CN104311010B (en) | 2016-04-20 |
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| CN110171965B (en) * | 2019-04-26 | 2021-07-06 | 武汉理工大学 | NPO capacitor dielectric material and preparation method thereof |
| CN110526711A (en) * | 2019-09-10 | 2019-12-03 | 天津大学 | Magnesium zirconium niobium tin tungsten series microwave dielectric ceramic and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1876600A (en) * | 2006-06-22 | 2006-12-13 | 西安交通大学 | Bismuth zinc niobate / barium strontium titanate composite dielectric adjustable thick film preparation method |
| CN101693988A (en) * | 2009-10-20 | 2010-04-14 | 西安交通大学 | Method for preparing BZN thin film for embedded type capacitor |
| CN102249307A (en) * | 2011-05-06 | 2011-11-23 | 天津大学 | Preparation method of Bi1.5MgNb1.5O7 (BMN) dielectric film |
-
2014
- 2014-10-09 CN CN201410527486.4A patent/CN104311010B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1876600A (en) * | 2006-06-22 | 2006-12-13 | 西安交通大学 | Bismuth zinc niobate / barium strontium titanate composite dielectric adjustable thick film preparation method |
| CN101693988A (en) * | 2009-10-20 | 2010-04-14 | 西安交通大学 | Method for preparing BZN thin film for embedded type capacitor |
| CN102249307A (en) * | 2011-05-06 | 2011-11-23 | 天津大学 | Preparation method of Bi1.5MgNb1.5O7 (BMN) dielectric film |
Non-Patent Citations (2)
| Title |
|---|
| BiV04掺杂对(Bi0.5Zn0.5)(Zn0.5Nb1.5)07陶瓷介电性能的影响;周焕福 等;《硅酸盐学报》;20051231;第33卷(第12期);1454-1456 * |
| Structure, IR spectra and dielectric properties of Bi2O3–ZnO–SnO2–Nb2O5 quarternary pyrochlore;Huiling Du 等;《Ceramics International》;20021231;第28卷;231-234 * |
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