CN101659546A - Barium strontium titanate ceramic capacitor material and preparation method thereof - Google Patents
Barium strontium titanate ceramic capacitor material and preparation method thereof Download PDFInfo
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- CN101659546A CN101659546A CN200810118990A CN200810118990A CN101659546A CN 101659546 A CN101659546 A CN 101659546A CN 200810118990 A CN200810118990 A CN 200810118990A CN 200810118990 A CN200810118990 A CN 200810118990A CN 101659546 A CN101659546 A CN 101659546A
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Abstract
The invention relates to a barium strontium titanate ceramic capacitor material and a preparation method thereof. The material is characterized by comprising the following components: 80 to 98 volumepercent of BaxSr1-xTiO3 and 2 to 20 volume percent of BaO-SiO2-B2O3 glass, wherein the range of x is between 0.2 and 0.5; and the molar contents of the compositions in BaO-SiO2-B2O3 glass are: 48 to 49 percent of BaO, 20 to 21 percent of SiO2, 26 to 27 percent of B2O3, 1 to 2 percent of SrO, 1 to 2 percent of ZrO2, 0.5 to 1 percent of Al2O3, 0.1 to 0.4 percent of MgO and 0.1 to 0.3 percent of Bi2O3. The barium strontium titanate ceramic capacitor material and the preparation method thereof provided by the invention can reduce the sintering temperature of barium strontium titanate by 250 to 400DEG C and the holding time to 1 hour, refine crystal grains to 1 to 3 micrometre, maintain dielectric loss at 1*10<-3> and increase pulse breakdown field strength to 40kV/mm, thereby meeting the requirements of a ceramic capacitor.
Description
Technical field
The present invention relates to a kind of ceramic capacitor material and preparation method thereof, especially a kind of is the ceramic capacitor material and preparation method thereof of base with the strontium-barium titanate, belongs to the function ceramics field.
Background technology
Ba
xSr
1-xTiO
3(BST) pottery is because of having good ferroelectric, piezoelectricity and insulating property, being widely used in the little and capacious miniature capacitor of volume, thermistor, ultra-large dynamic RAM, tuning microwave device etc., is one of most widely used material of electronic ceramic fields.Can adjust Curie temperature and the specific inductivity of BST by changing Ba/Sr ratio, to satisfy corresponding service requirements.The BST of high Ba content becomes the research focus of vast researcher owing to have voltage-controlled, the temperature control adjustability of high-k and specific inductivity; And for the research of the dielectric properties of low Ba content BST seldom.The BST of low Ba content is a paraelectric phase in room temperature, has low dielectric loss and higher dielectric constant, and at microwave device, changeover condenser, particularly energy storage aspect has broad application prospects.And when adopting solid-phase sintering process to prepare the BST stupalith, often exigent sintering temperature (1350 ℃～1400 ℃).This not only to the equipment requirements height, be unfavorable for reducing production costs, and easily cause crystal grain thick, influence the reduction of the dielectric properties, particularly disruptive strength of material.
Therefore, providing a kind of can either have low-dielectric loss stupalith of high compressive strength and preparation method thereof again at the lesser temps densified sintering product, just becomes this technical field to be badly in need of the technical barrier that will solve.
Summary of the invention
One of purpose of the present invention provides a kind ofly can either have the low-dielectric loss stupalith of high compressive strength again at the lesser temps densified sintering product.
For achieving the above object, the present invention takes following technical scheme to be achieved:
A kind of barium strontium titanate ceramic capacitor material is characterized in that: it is formed and proportioning is: the Ba of 80vol%～98vol%
xSr
1-xTiO
3, the BaO-SiO of 2vol%～20vol%
2-B
2O
3Be glass; Described Ba
xSr
1-xTiO
3In the x span be 0.2～0.5; Described BaO-SiO
2-B
2O
3The molar content that is each composition in the glass is BaO 48%～49%, SiO
220%～21%, B
2O
326%～27%, SrO 1%～2%, ZrO
21%～2%, Al
2O
30.5%～1%, MgO 0.1%～0.4%, Bi
2O
30.1%～0.3%.
The preparation method of above-mentioned barium strontium titanate ceramic capacitor material comprises the steps:
(1) adopts the synthetic Ba of traditional solid reaction process
xSr
1-xTiO
3Powder, x span are 0.2～0.5;
(2) by mole content, with B component aCO
348%～49%, SiO
220%～21%, B
2O
326%～27%, SrCO
31%～2%, ZrO
21%～2%, Al
2O
30.5%～1%, MgO 0.1%～0.4%, Bi
2O
30.1%～0.3% thorough mixing, 1100 ℃ of fusion 1h pour glass metal in the cold water into fast and quench, and make glass fragment, then with glass fragment ball milling 4h, cross 400 mesh sieves, make glass powder;
(3) glass powder is added to the Ba of step (1) preparation of 80vol%～98vol% in 2vol%～20vol% ratio
xSr
1-xTiO
3In the powder, as dispersion agent, adopt the agate abrading-ball with ethanol, ball milling 24h is dried in 90 ℃ of baking ovens, gets powder;
(4) with step (3) gained powder process isostatic cool pressing, pressing pressure is 200Mpa, and being pressed into diameter is 20mm, the sample of thickness 2mm, and in the air atmosphere, 1000～1150 ℃ of sintering 1h make ceramics sample.
A kind of optimal technical scheme is characterized in that: described step (1) is for choosing analytically pure chemical reagent BaCO
3, SrCO
3And TiO
2, press Ba
xSr
1-xTiO
3Batching, ball milling 24h, oven dry at 1150 ℃ of calcining 4h, forms Ba
xSr
1-xTiO
3Powder.
Beneficial effect
Advantage of the present invention is to add a certain amount of BaO-SiO in strontium-barium titanate
2-B
2O
3Be glass, make sintering temperature reduce by 250 ℃～400 ℃, soaking time was reduced to 1 hour, grain refining to 1～3 micron, and dielectric loss remains on 1 * 10
-3About, the pulse breakdown field intensity is brought up to～40kV/mm.Be fit to very much make high pressure resistant low-loss laminated ceramic capacitor.
The present invention will be further described below by the drawings and specific embodiments, but and do not mean that limiting the scope of the invention.
Description of drawings
Fig. 1 is the stereoscan photograph of Comparative Examples 1 gained sample.
Fig. 2 is the stereoscan photograph of embodiment 1 gained sample.
Fig. 3 is the stereoscan photograph of embodiment 2 gained samples.
Fig. 4 is the stereoscan photograph of embodiment 3 gained samples.
Fig. 5 is the stereoscan photograph of embodiment 4 gained samples.
Embodiment
Comparative Examples 1
(1) at first chooses analytically pure chemical reagent BaCO
3, SrCO
3And TiO
2, press Ba
0.4Sr
0.6TiO
3Batching, ball milling 24h, oven dry at 1150 ℃ of calcining 4h, forms Ba
0.4Sr
0.6TiO
3Powder.
(2) with Ba
0.4Sr
0.6TiO
3Powder is through isostatic cool pressing, and pressing pressure is 200Mpa, and being pressed into diameter is 20mm, the sample of thickness 2mm, and in the air atmosphere, 1400 ℃ of sintering 4h make ceramics sample.
The ceramics sample upper and lower surface through polish etch, by scanning electron microscope (Hitachi S4800, magnification is 2k times), is observed its microscopic appearance, as shown in Figure 1, pure Ba
0.4Sr
0.6TiO
3Crystal grain is thick, and mean sizes is tens microns, and grain-size is inhomogeneous, has some big holes at intragranular and crystal boundary place.
The ceramics sample that burns till is carried out the disruptive strength test through cutting and polish the sample of making thickness 0.3mm, and the sample upper and lower surface through polishing is fired silver electrode by silver, tests its dielectric properties, and is as shown in table 1.
The dielectric properties of table 1 Comparative Examples 1 described component
| Compositing formula | Specific inductivity (room temperature, 1kHz) | Dielectric loss (room temperature, 1kHz) | Breaking down field strength (kV/mm) |
| ??Ba 0.4Sr 0.6TiO 3 | ??1088 | ??0.0009 | ??19.1 |
Embodiment 1
(1) at first chooses analytically pure chemical reagent BaCO
3, SrCO
3And TiO
2, press Ba
0.4Sr
0.6TiO
3Batching, ball milling 24h, oven dry at 1150 ℃ of calcining 4h, forms Ba
0.4Sr
0.6TiO
3Powder.
(2) press the component of table 2, through thorough mixing, 1100 ℃ of fusion 1h pour glass metal in the cold water into fast and quench, and make glass fragment, then with glass fragment ball milling 4h, cross 400 mesh sieves, make glass powder A.
The composition of table 2 glass powder A
(3) according to 98vol%Ba
0.4Sr
0.6TiO
3The glass powder A proportioning of+2vol% as dispersion agent, adopts the agate abrading-ball with ethanol, and ball milling 24h is dried in 90 ℃ of baking ovens, gets powder.
(4) with step (3) prepared powder process isostatic cool pressing, pressing pressure is 200Mpa, and being pressed into diameter is 20mm, the sample of thickness 2mm, and in the air atmosphere, 1150 ℃ of sintering 1h make ceramics sample.
The ceramics sample upper and lower surface through polish etch, by scanning electron microscope (Hitachi S4800, magnification is 5k times), is observed its microscopic appearance.As shown in Figure 2, add the glass powder A of 2vol%, the sample grain-size obviously reduces, and average grain size is 3 μ m.
The ceramics sample that burns till is carried out the disruptive strength test through cutting and polish the sample of making thickness 0.3mm, and the sample upper and lower surface through polishing is fired silver electrode by silver, tests its dielectric properties, and is as shown in table 3.
The dielectric properties of table 3 embodiment 1 described component
| Compositing formula | Specific inductivity (room temperature, 1kHz) | Dielectric loss (room temperature, 1kHz) | Breaking down field strength (kV/mm) |
| ??98vol％Ba 0.4Sr 0.6TiO 3+ 2vol% glass powder A | ??852 | ??0.00281 | ??40.0 |
Embodiment 2
According to 95vol%Ba
0.4Sr
0.6TiO
3+ 5vol% glass powder A proportioning, concrete operational path is identical with embodiment 2.The microscopic appearance of the described component of present embodiment adds 5vol% glass powder A as shown in Figure 3, and the sample grain-size obtains further refinement, and average grain size is 2 μ m.Dielectric properties are as shown in table 4.
The dielectric properties of table 4 embodiment 2 described components
| Compositing formula | Specific inductivity (room temperature, 1kHz) | Dielectric loss (room temperature, 1kHz) | Breaking down field strength (kV/mm) |
| ??95vol％Ba 0.4Sr 0.6TiO 3+ 5vol% glass powder A | ??814 | ??0.00101 | ??41.0 |
Embodiment 3
According to 90vol%Ba
0.4Sr
0.6TiO
3+ 10vol% glass powder A proportioning, concrete operational path is identical with embodiment 2.The microscopic appearance of the described component of present embodiment adds 10vol% glass powder A as shown in Figure 4, and the sample average grain-size is 1.5 μ m.Dielectric properties are as shown in table 5.
The dielectric properties of table 5 embodiment 3 described components
| Compositing formula | Specific inductivity (room temperature, 1kHz) | Dielectric loss (room temperature, 1kHz) | Breaking down field strength (kV/mm) |
| ??90vol％Ba 0.4Sr 0.6TiO 3+ 10vol% glass powder A | ??706 | ??0.00115 | ??41.5 |
Embodiment 4
According to 80vol%Ba
0.4Sr
0.6TiO
3+ 20vol% glass powder A proportioning, concrete operational path is identical with embodiment 2.The microscopic appearance of the described component of present embodiment adds 20vol% glass powder A as shown in Figure 5, and the sample average grain-size is less than 1 μ m.Dielectric properties are as shown in table 6.
The dielectric properties of table 6 embodiment 4 described components
| Compositing formula | Specific inductivity (room temperature, 1kHz) | Dielectric loss (room temperature, 1kHz) | Breaking down field strength (kV/mm) |
| ??80vol％Ba 0.4Sr 0.6TiO 3+ 20vol% glass powder A | ??468 | ??0.00125 | ??46.2 |
Embodiment 5
(1) at first chooses the pure chemical reagent BaCO of AG
3, SrCO
3And TiO
2, press Ba
0.2Sr
0.8TiO
3Batching, ball milling 24h, oven dry at 1150 ℃ of calcining 4h, forms Ba
0.2Sr
0.8TiO
3Powder.
(2) press the component of table 7, through thorough mixing, 1100 ℃ of fusion 1h pour glass metal in the cold water into fast and quench, and make glass fragment, then with glass fragment ball milling 4h, cross 400 mesh sieves, make glass powder B.
The composition of table 7 glass powder B
(3) glass powder B is added in the BST powder in the 10vol% ratio, as dispersion agent, adopt the agate abrading-ball with ethanol, ball milling 24h is dried in 90 ℃ of baking ovens.
(4) with prepared powder process isostatic cool pressing, pressing pressure is 200Mpa, and being pressed into diameter is 20mm, the sample of thickness 2mm, and in the air atmosphere, 1000 ℃ of sintering 1h make ceramics sample.
The ceramic disks of burning till is carried out the disruptive strength test through cutting and polish the sample of making thickness 0.3mm, and the sample upper and lower surface through polishing is fired silver electrode by silver, tests its dielectric properties, and is as shown in table 8.
The dielectric properties of table 8 embodiment 5 described components
| Compositing formula | Specific inductivity (room temperature, 1kHz) | Dielectric loss (room temperature, 1kHz) | Breaking down field strength (kV/mm) |
| ??90vol％Ba 0.2Sr 0.8TiO 3 | ??373 | ??0.0005 | ??49.6 |
| + 10vol% glass powder B |
Embodiment 6
(1) at first chooses the pure chemical reagent BaCO of AG
3, SrCO
3And TiO
2, press Ba
0.3Sr
0.7TiO
3Batching, ball milling 24h, oven dry at 1150 ℃ of calcining 4h, forms Ba
0.3Sr
0.7TiO
3Powder.
(2) press the component of table 9, through thorough mixing, 1100 ℃ of fusion 1h pour glass metal in the cold water into fast and quench, and make glass fragment, then with glass fragment ball milling 4h, cross 400 mesh sieves, make glass powder C.
The composition of table 9 glass powder C
(3) glass powder C is added in the BST powder in the 10vol% ratio, as dispersion agent, adopt the agate abrading-ball with ethanol, ball milling 24h is dried in 90 ℃ of baking ovens.
(4) with prepared powder process isostatic cool pressing, pressing pressure is 200Mpa, and being pressed into diameter is 20mm, the sample of thickness 2mm, and in the air atmosphere, 1050 ℃ of sintering 1h make ceramics sample.
The ceramic disks of burning till is carried out the disruptive strength test through cutting and polish the sample of making thickness 0.3mm, and the sample upper and lower surface through polishing is fired silver electrode by silver, tests its dielectric properties, and is as shown in table 10.
The dielectric properties of table 10 embodiment 6 described components
| Compositing formula | Specific inductivity (room temperature, 1kHz) | Dielectric loss (room temperature, 1kHz) | Breaking down field strength (kV/mm) |
| ?90vol％Ba 0.3Sr 0.7TiO 3+ 10vol% glass powder C | ??523 | ??0.00072 | ??46.3 |
Embodiment 7
(1) at first chooses the pure chemical reagent BaCO of AG
3, SrCO
3And TiO
2, press Ba
0.5Sr
0.5TiO
3Batching, ball milling 24h, oven dry at 1150 ℃ of calcining 4h, forms Ba
0.5Sr
0.5TiO
3Phase.
(2) press the component of table 11, through thorough mixing, 1100 ℃ of fusion 1h pour glass metal in the cold water into fast and quench, and make glass fragment, then with glass fragment ball milling 4h, cross 400 mesh sieves, make glass powder D.
The composition of table 11 glass powder D
(3) glass powder D is added in the BST powder in the 10vol% ratio, as dispersion agent, adopt the agate abrading-ball with ethanol, ball milling 24h is dried in 90 ℃ of baking ovens.
(4) with prepared powder process isostatic cool pressing, pressing pressure is 200Mpa, and being pressed into diameter is 20mm, the sample of thickness 2mm, and in the air atmosphere, 1150 ℃ of sintering 1h make ceramics sample.
The ceramic disks of burning till is carried out the disruptive strength test through cutting and polish the sample of making thickness 0.3mm, and the sample upper and lower surface through polishing is fired silver electrode by silver, tests its dielectric properties, and is as shown in table 12.
The dielectric properties of table 12 embodiment 7 described components
| Compositing formula | Specific inductivity (room temperature, 1kHz) | Dielectric loss (room temperature, 1kHz) | Breaking down field strength (kV/mm) |
| ??90vol％Ba 0.5Sr 0.5TiO 3+ 10vol% glass powder D | ?1184 | ?0.0023 | ??34.1 |
Claims (3)
1, a kind of barium strontium titanate ceramic capacitor material is characterized in that: it is formed and proportioning is: the Ba of 80vol%～98vol%
xSr
1-xTiO
3, the BaO-SiO of 2vol%～20vol%
2-B
2O
3Be glass; Described Ba
xSr
1-xTiO
3In the x span be 0.2～0.5; Described BaO-SiO
2-B
2O
3The molar content that is each composition in the glass is BaO48%～49%, SiO
220%～21%, B
2O
326%～27%, SrO 1%～2%, ZrO
21%～2%, Al
2O
30.5%～1%, MgO 0.1%～0.4%, Bi
2O
30.1%～0.3%.
2, the preparation method of barium strontium titanate ceramic capacitor material according to claim 1 comprises the steps:
(1) adopts the synthetic Ba of traditional solid reaction process
xSr
1-xTiO
3Powder, x span are 0.2～0.5;
(2) by mole content, with B component aCO
348%～49%, SiO
220%～21%, B
2O
326%～27%, SrCO
31%～2%, ZrO
21%～2%, Al
2O
30.5%～1%, MgO 0.1%～0.4%, Bi
2O
30.1%～0.3% thorough mixing, 1100 ℃ of fusion 1h pour glass metal in the cold water into fast and quench, and make glass fragment, then with glass fragment ball milling 4h, cross 400 mesh sieves, make glass powder;
(3) glass powder is added to the Ba of step (1) preparation of 80vol%～98vol% in 2vol%～20vol% ratio
xSr
1-xTiO
3In the powder, as dispersion agent, adopt the agate abrading-ball with ethanol, ball milling 24h is dried in 90 ℃ of baking ovens, gets powder;
(4) with step (3) gained powder process isostatic cool pressing, pressing pressure is 200Mpa, and being pressed into diameter is 20mm, the sample of thickness 2mm, and in the air atmosphere, 1000～1150 ℃ of sintering 1h make ceramics sample.
3, the preparation method of barium strontium titanate ceramic capacitor material according to claim 2 is characterized in that: in the described step (1), choose analytically pure chemical reagent BaCO
3, SrCO
3And TiO
2, press Ba
xSr
1-xTiO
3Batching, ball milling 24h, oven dry is at 1150 ℃ of calcining 4h, synthetic Ba
xSr
1-xTiO
3Powder.
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|---|---|---|---|
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|---|---|---|---|
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ID=41787830
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| CN102030526B (en) * | 2010-11-11 | 2013-02-13 | 厦门松元电子有限公司 | Anti-reduction ceramic dielectric material and preparation method thereof |
| CN103288446A (en) * | 2012-02-29 | 2013-09-11 | 深圳光启创新技术有限公司 | Ceramic composite material and super material prepared from same |
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| CN104003716B (en) * | 2014-05-08 | 2015-08-26 | 华南理工大学 | A kind of anti-reduction low temperature sintered high frequency heat stable dielectric ceramic and preparation method thereof |
| CN104725036A (en) * | 2015-02-10 | 2015-06-24 | 景德镇陶瓷学院 | High-temperature low-loss barium strontium titanate-based energy-storage ceramic and preparation method thereof |
| CN106229097A (en) * | 2016-08-09 | 2016-12-14 | 安徽省宁国天成电工有限公司 | Thermal resistor that a kind of linearity is good and application thereof |
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| CN107098695A (en) * | 2017-05-27 | 2017-08-29 | 武汉理工大学 | A kind of X7R capacitor ceramic materials of high breakdown strength and preparation method thereof |
| CN107098695B (en) * | 2017-05-27 | 2020-10-16 | 武汉理工大学 | X7R capacitor ceramic material with high breakdown strength and preparation method thereof |
| CN109704763A (en) * | 2018-12-28 | 2019-05-03 | 有研工程技术研究院有限公司 | A kind of preparation method of low-temperature sintering ceramic dielectric material |
| CN109704763B (en) * | 2018-12-28 | 2021-06-15 | 有研工程技术研究院有限公司 | Preparation method of low-temperature sintered ceramic dielectric material |
| CN112408975A (en) * | 2019-08-23 | 2021-02-26 | 兴勤电子工业股份有限公司 | Ceramic composition, ceramic sintered body, multilayer ceramic electronic component and method for producing the same |
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