CN1331803C - (Balx-ySrxYy) TiO3 based dielectrical ceramic material and preparation process thereof - Google Patents
(Balx-ySrxYy) TiO3 based dielectrical ceramic material and preparation process thereof Download PDFInfo
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- CN1331803C CN1331803C CNB2005101360077A CN200510136007A CN1331803C CN 1331803 C CN1331803 C CN 1331803C CN B2005101360077 A CNB2005101360077 A CN B2005101360077A CN 200510136007 A CN200510136007 A CN 200510136007A CN 1331803 C CN1331803 C CN 1331803C
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Abstract
The present invention discloses (Ba<1-x-y>Sr<x>Y<y>) TiO3 based dielectric ceramic material and a preparation method thereof, which belongs to dielectric ceramic technology. The (Ba<1-x-y>Sr<x>Y<y>) TiO3 based dielectric ceramic material is composed of (Ba<1-x-y>Sr<x>Y<y>) TiO3, MnO2 and MgO, wherein the mass content of the (Ba<1-x-y>Sr<x>Y<y>) TiO3 is 96%, x is equal to 0.29 to 0.58, y is equal to 0.003 to 0.016, the mass content of the MnO2 is from one percent to three percent, and the mass content of the MgO is from one percent to three percent. The process of the method comprises that BaCO3, TiO2, Y2O3 and SrCO3 are mixed into a mixture according to the mol ratio of (Ba<1-x-y>Sr<x>Y<y>) TiO3, then the mixture, a milling ball and deionized water are mixed according to the mass ratio to carry out ball milling work, the milled material slurry is dried to pre-synthesize the (Ba<1-x-y>Sr<x>Y<y>) TiO3, the MnO2 and the MgO are added to the pre-synthesized material according to the mass percent, and the mixture, the milling ball and the deionized water are mixed by mass, milled and dried; then polyvinyl alcohol water solution is added to the mixture and evenly mixed, and sieving granulation, compression molding work and sintering work are carried out to prepare the (Ba<1-x-y>Sr<x>Y<y>) TiO3 based dielectric ceramic material. The present invention has the advantages that (Ba<1-x-y>Sr<x>Y<y>) TiO3 based dielectric ceramic has fine crystal particle, high dielectric constant, low dielectric loss, high breakdown electric field strength and good material repeatability.
Description
Technical field
The present invention relates to a kind of (Ba
1-x-ySr
xY
y) TiO
3Based dielectric stupalith and preparation method thereof belongs to the dielectric ceramics technology.
Background technology
The research of centering high voltage ceramic capacitor both at home and abroad is very active, and main by changing material prescription, some other ion that mixes reaches material modification and unleaded purpose.The research that has B
2O
3-Li
2CO
3To Mn doping (Ba, Sr) TiO
3The influence of ceramic performance, because the Curie temperature of research system is all more than room temperature, thereby this system has shown higher dielectric loss, general all at (Tao Hu more than 1%, Tim J.Price, et al, the effect of Mn on microstructure andproperties of BaSrTiO
3With B
2O
3-LiCO
3, Journal of the European Ceramic Society, 25 (2005) 2531～2535); The research that has adopts sol-gel processing to make (Ba, Sr) TiO earlier
3Powder, sintering has made (Ba, Sr) TiO at a lower temperature again
3Ferroelectric ceramic(s), the result shows, the material dielectric constant of acquisition is on the low side (Wang Jiang beautiful jade etc. strontium-barium titanate (Ba
xSr
1-xTiO
3) research of pottery preparation and dielectric properties thereof, functional materials, 2004,2 (35) 212～213.).O.PThakur, people such as Chandra Prakash have studied microwave sintering to Ba
0.95S
0.05TiO
3The ferroelectric ceramic(s) Effect on Performance, but the dielectric loss of the material that obtains is up to (O.P.Thakur, Chandra Prakash, et al, dielectricbehavior of Ba more than 2.17%
0.95S
0.05TiO
3Ceramics sintered by microwave, Materials Science and Engineering, B96 (2002) 221～225.).
Summary of the invention
The object of the present invention is to provide a kind of (Ba
1-x-ySr
xY
y) TiO
3Based dielectric stupalith and preparation method thereof makes dielectric ceramics with this method, has unleaded and the low-loss characteristics of high-k.
The present invention is realized by following technical proposals, a kind of (Ba
1-x-ySr
xY
y) TiO
3The based dielectric stupalith is characterized in that being made up of following ingredients and mass content thereof:
(Ba
1-x-ySr
xY
y) TiO
3: 96%, wherein, x=0.29～0.58, y=0.003～0.016;
MnO
2：(1～3)％；
MgO：(1～3)％。
Above-mentioned (Ba
1-x-ySr
xY
y) TiO
3Based dielectric ceramic material method is characterized in that comprising following process: with BaCO
3, TiO
2, Y
2O
3And SrCO
3By (Ba
1-x-ySr
xY
y) TiO
3Mol ratio is prepared burden, wherein, x=0.29～0.58, y=0.003～0.016 then should batching be mixed by mass ratio with abrading-ball and deionized water and was carried out ball milling 4～6 hours at 1: 1: 2, places baking oven through 110～130 ℃ of oven dry the slip behind the ball milling.To dry material pre-Synthetic 2 h～6h under 1040 ℃～1150 ℃ then, furnace cooling makes (Ba after room temperature afterwards
1-x-ySr
xY
y) TiO
3Synthetic material; (Ba with mass percent 96%
1-x-ySr
xY
y) TiO
3Synthetic material, mass percent are the MnO of (1～3) %
2Prepare burden for the MgO of (1～3) % with mass percent, should batching mix at 1: 1: 1.5 by mass ratio and carried out ball milling 6～12 hours with abrading-ball and deionized water, with the slip behind the ball milling place enamel tray at baking oven through 110～130 ℃ of oven dry.To dry material then, to add 5～8% mass percent be that 5% polyvinyl alcohol water solution mixes, and crosses 40 mesh sieve granulations then.The granulation material adopts 100～400MPa pressure dry-pressing formed.Moulded blank placed put into the resistance kiln roasting on the aluminum oxide backing plate, on the backing plate, prevent adhesion with the zirconium dioxide bedding and padding between sheet and the sheet.Sample respectively is incubated 20 minutes at 120～150 ℃ and 200～350 ℃ in the temperature-rise period, controls heat-up rate then, guarantees per hour to heat up at 300～400 ℃, and sample is at 1220 ℃～1350 ℃ sintering 2h～6h, and the furnace cooling that cuts off the power supply then is to room temperature.After the removing of the zirconium dioxide bedding and padding on the ceramics after burning till, pass through ultrasonic cleaning, drying, the even silver coating electrode slurry in two sides, be incubated 10 minutes burning infiltration silver electrodes through 530～850 ℃.
Outstanding advantage of the present invention is (Ba
1-x-ySr
xY
y) TiO
3The based dielectric pottery has that crystal grain is thin, specific inductivity is high, dielectric loss is low, disruptive field intensity is high, material repeated fine.
Embodiment
Embodiment:
With BaCO
3, TiO
2, Y
2O
3And SrCO
3By (Ba
0.611Sr
0.38Y
0.009) TiO
3Mol ratio is prepared burden, then should batching be to mix at 1: 1: 2 to carry out ball milling 4～6 hours with abrading-ball and deionized water by mass ratio, place baking oven through 120 ℃ of oven dry the slip behind the ball milling.To dry material pre-Synthetic 2 h under 1100 ℃ then, furnace cooling is to room temperature afterwards.According to above-mentioned prescription with (Ba
0.611Sr
0.38Y
0.009) TiO
3Batching 50g is that example is calculated prescription and batching: 23.313gBaCO
3+ 15.444g TiO
2+ 10.847g SrCO
3+ 0.0019g Y
2O
3Pressed mass ratio 1: 1: 2, mixing and ball milling 4h with batching and abrading-ball and deionized water.The ball milling material is dry after 1080 ℃, be incubated 2 hours and synthesizes in advance.Take by weighing again in the synthetic material and allocate 1.0140g MnO into
2, 1.0151g MgO, pressed mass ratio 1: 1: 1.5 by batching and abrading-ball and deionized water again, the adding deionized water carries out secondary ball milling 6h; 5% polyvinyl alcohol water solution 3.5m1 of adding 7% carries out granulation after the ball milling material drying, and the granulation material is crossed 40 mesh sieves, then compacting Φ 10mm * 2mm disk sample under 350MPa pressure; Sample carried out sintering 2 hours at 1300 ℃, and the ceramic sample after burning till is behind ultrasonic cleaning 20min, and with the ceramics preheating, the even silver coating electrode slurry in two sides is through 10 minutes burning infiltration silver electrodes of 530 ℃ of insulations.After tested, the performance of sample is ε
r=4745; Tg δ=0.16%; The disruptive field intensity of test sample is 6.40kv/mm under room temperature alternating electric field condition.
Claims (2)
1. (Ba
1-x-ySr
xY
y) TiO
3The based dielectric stupalith is characterized in that being made up of following ingredients and mass content thereof:
(Ba
1-x-ySr
xY
y) TiO
3: 96%, wherein, x=0.29～0.58, y=0.003～0.016;
MnO
2：(1～3)％；
MgO：(1～3)％。
2. (Ba
1-x-ySr
xY
y) TiO
3The preparation method of based dielectric stupalith is characterized in that comprising following process: with BaCO
3, TiO
2, Y
2O
3And SrCO
3By (Ba
1-x-ySr
xY
y) TiO
3Mol ratio is prepared burden, wherein, x=0.29～0.58, y=0.003～0.016, then should batching mix at 1: 1: 2 by mass ratio and carried out ball milling 4～6 hours with abrading-ball and deionized water, place baking oven through 110～130 ℃ of oven dry the slip behind the ball milling, will dry material pre-Synthetic 2 h～6h under 1040 ℃～1150 ℃ then, furnace cooling makes (Ba after room temperature afterwards
1-x-ySr
xY
y) TiO
3Synthetic material; (Ba with mass percent 96%
1-x-ySr
xY
y) TiO
3Synthetic material, mass percent are the MnO of (1～3) %
2MgO for (1～3) % prepares burden with mass percent, should batching mix at 1: 1: 1.5 by mass ratio and carried out ball milling 6～12 hours with abrading-ball and deionized water, with the slip behind the ball milling place enamel tray at baking oven through 110～130 ℃ of oven dry, to dry material then, to add 5～8% mass percent be that 5% polyvinyl alcohol water solution mixes, cross 40 mesh sieve granulations then, the granulation material adopts 100～400MPa pressure dry-pressing formed, moulded blank placed put into the resistance kiln roasting on the aluminum oxide backing plate, on the backing plate, prevent adhesion with the zirconium dioxide bedding and padding between sheet and the sheet, sample respectively is incubated 20 minutes at 120～150 ℃ and 200～350 ℃ in the temperature-rise period, control heat-up rate then, guarantee per hour to heat up at 300～400 ℃, sample is at 1220 ℃～1350 ℃ sintering 2h～6h, the furnace cooling that cuts off the power supply then is to room temperature, after the removing of the zirconium dioxide bedding and padding on the ceramics after burning till, through ultrasonic cleaning, dry, the even silver coating electrode slurry in two sides, through 10 minutes burning infiltration silver electrodes of 530～850 ℃ of insulations.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101360077A CN1331803C (en) | 2005-12-28 | 2005-12-28 | (Balx-ySrxYy) TiO3 based dielectrical ceramic material and preparation process thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101360077A CN1331803C (en) | 2005-12-28 | 2005-12-28 | (Balx-ySrxYy) TiO3 based dielectrical ceramic material and preparation process thereof |
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|---|---|
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| CN1331803C true CN1331803C (en) | 2007-08-15 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101774803B (en) * | 2009-01-13 | 2013-06-05 | 中山市天键电声有限公司 | A (Ba, sr) TiO3-based ceramic medium and its prepn |
| CN101774802B (en) * | 2010-01-16 | 2012-10-31 | 中山市天键电子工业有限公司 | Ceramic dielectric material and preparation method thereof |
| CN101863154B (en) * | 2010-06-17 | 2012-07-04 | 天津大学 | Multilayer gradient Ba1-xSrxTiO3 (BST) dielectric ceramic material and preparation method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6514895B1 (en) * | 2000-06-15 | 2003-02-04 | Paratek Microwave, Inc. | Electronically tunable ceramic materials including tunable dielectric and metal silicate phases |
| EP1422209A2 (en) * | 2002-11-22 | 2004-05-26 | Paratek Microwave, Inc. | Method for producing low-loss tunable ceramic composites with improved breakdown strengths |
| CN1626475A (en) * | 2002-09-27 | 2005-06-15 | 广东风华高新科技集团有限公司 | Anti reductive powder of media ceramics and preparation method, as well as method in use for preparing ceramic capacitor in multiple layers |
| CN1634798A (en) * | 2003-12-30 | 2005-07-06 | 广东风华高新科技集团有限公司 | Unreduced thermal compensation ceramic medium materials and ceramic capacitor made thereof |
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2005
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6514895B1 (en) * | 2000-06-15 | 2003-02-04 | Paratek Microwave, Inc. | Electronically tunable ceramic materials including tunable dielectric and metal silicate phases |
| CN1626475A (en) * | 2002-09-27 | 2005-06-15 | 广东风华高新科技集团有限公司 | Anti reductive powder of media ceramics and preparation method, as well as method in use for preparing ceramic capacitor in multiple layers |
| EP1422209A2 (en) * | 2002-11-22 | 2004-05-26 | Paratek Microwave, Inc. | Method for producing low-loss tunable ceramic composites with improved breakdown strengths |
| CN1634798A (en) * | 2003-12-30 | 2005-07-06 | 广东风华高新科技集团有限公司 | Unreduced thermal compensation ceramic medium materials and ceramic capacitor made thereof |
Non-Patent Citations (1)
| Title |
|---|
| 掺杂Y2O3对BaSrTiO3介质瓷性能的影响 曲远方等，电子元件与材料，第24卷第11期 2005 * |
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