CN101851091A - Temperature change resistance composite high-dielectric electronic material and preparation method thereof - Google Patents
Temperature change resistance composite high-dielectric electronic material and preparation method thereof Download PDFInfo
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- CN101851091A CN101851091A CN 201010147770 CN201010147770A CN101851091A CN 101851091 A CN101851091 A CN 101851091A CN 201010147770 CN201010147770 CN 201010147770 CN 201010147770 A CN201010147770 A CN 201010147770A CN 101851091 A CN101851091 A CN 101851091A
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Abstract
The invention relates to a temperature change resistance composite high-dielectric electronic material and a preparation method thereof. The electronic material comprises the components by weight percent: 42-45% of BaTiO3, 19-26% of (Na 0.5, Bi 0.5) TiO3, 28-38% of Pb (Sn0.6, Ti0.4) O3, 0.6-1% of MgO and 0.2-2% of Sm2O3, wherein the Pb (Sn0.6, Ti0.4) O3 is prepared by PbO, SnO2 and TiO2, and the molar ratio of the PbO, the SnO2 and the TiO2 is 5: 3: 2; and the (Na 0.5, Bi 0.5) TiO3 is prepared by NaCO3, Bi2O3 and TiO2, and the molar ratio of the NaCO3, the Bi2O3 and the TiO2 is 2: 1: 4. The preparation method comprises: prefabricating the Pb (Sn0.6, Ti0.4) O3, prefabricating the (Na, Bi) TiO3, forming blank and sintering. The invention has low manufacturing cost, and is applicable to electron devices such as a capacitor, a filter and the like.
Description
Technical field
The present invention relates to a kind of is the composite high-dielectric electronic material of feature with the composition, specifically, but is composite high-dielectric electronic dielectric material of a kind of temperature resistance change and preparation method thereof.
Background technology
Dielectric substance should have higher dielectric constant, and has the wide operation temperature area of trying one's best under the prerequisite that guarantees less specific inductivity rate of temperature change.Although worldwide research institution has carried out a large amount of research to dielectric substance since half a century; make its performance perameter aspect a lot of, obtain bigger lifting; but the operating temperature range of current material is still narrower; when envrionment temperature rises to more than 150 ℃; its specific inductivity can be undergone mutation usually; device and even circuitry were lost efficacy, therefore can not satisfy radar, aircraft and the more and more high requirement of other special equipments.
Summary of the invention
Goal of the invention of the present invention is the defective at prior art, one provides a kind of high reliability request that can satisfy electron device, satisfy the dielectric substance that is suitable for work under rugged surrounding temperature (55～+ 200 ℃) of the more and more high requirement of radar, aircraft and other special equipments, two provide a kind of BaTiO
3-(Na
0.5, Bi
0.5) TiO
3-Pb (Sn
0.6, Ti
0.4) O
3System material medium and preparation method thereof.
Realize that the foregoing invention purpose adopts following technical scheme:
A kind of temperature change resistance composite high-dielectric electronic material, its component and raw material weight per-cent thereof are as follows: BaTiO
3Be 42～45%, (Na
0.5, Bi
0.5) TiO
3Be 19～26%, Pb (Sn
0.6, Ti
0.4) O
3Be 28～38%, MgO is 0.6～1%, Sm
2O
3Be 0.2～2%; Pb (Sn wherein
0.6, Ti
0.4) O
3Use PbO, SnO
2With TiO
2Preparation, PbO, SnO
2With TiO
2Mol ratio be 5: 3: 2; (Na
0.5, Bi
0.5) TiO
3Use NaCO
3, Bi
2O
3With TiO
2Preparation, NaCO
3, Bi
2O
3With TiO
2Mol ratio be 2: 1: 4.
A kind of preparation method of temperature change resistance composite high-dielectric electronic material comprises the steps:
(1) prefabricated Pb (Sn
0.6, Ti
0.4) O
3: press PbO, SnO
2With TiO
2Mol ratio be 5: 3: 2 the batching, batching is inserted ball mill, add 1～3 times of volumes of deionized water ball milling 1～12 hour, oven dry obtains powder under 105 ℃ of environment, powder is passed through 200 purpose screen clothes, powder after sieving is heated to 980 ℃～990 ℃ insulations 3～5 hours, and the room temperature cooling makes Pb (Sn
0.6, Ti
0.4) O
3
(2) prefabricated (Na
0.5, Bi
0.5) TiO
3: press NaCO
3, Bi
2O
3With TiO
2Mol ratio be 2: 1: 4 the batching, batching is inserted ball mill, add 1～3 times of volumes of deionized water ball milling 1～12 hour, oven dry obtains powder under 105 ℃ of environment, powder is passed through 200 purpose screen clothes, powder after sieving is heated to 900 ℃～920 ℃ insulations 1.5～2.5 hours, and the room temperature cooling makes (Na
0.5, Bi
0.5) TiO
3
(3) according to weight BaTiO
3Be 42～45%, (Na
0.5, Bi
0.5) TiO
3Frit is 19～26%, Pb (Sn
0.6, Ti
0.4) O
3Frit is 28～38%, and MgO is 0.6～1%, Sm
2O
3Be 0.2～2% preparation raw material, with joining raw material insert ball mill, add the deionized water ball milling 1～12 hour of 1～3 times of volume; Oven dry obtains powder under 105 ℃ of environment then, powder is passed through 500 purpose screen clothes, the organic binder bond or the paraffin that add 5%～6% weight ratio in the powder after sieving, add 90～120Mpa pressure and make green compact, be heated to 1180 ℃～1200 ℃ insulations 4～9 hours afterwards, the room temperature cooling makes temperature change resistance composite high-dielectric electronic material.
The invention has the beneficial effects as follows, a kind of temperature change resistance composite high-dielectric electronic material of working under-55～+ 200 ℃ of rugged surrounding temperatures of being suitable for is provided, can satisfy the high reliability request of electron device.Although worldwide research institution has carried out a large amount of research to dielectric substance since half a century; make its performance perameter aspect a lot of, obtain bigger lifting; but the operating temperature range of current material is still narrower; when envrionment temperature rises to more than 150 ℃; its specific inductivity can be undergone mutation usually; device and even circuitry were lost efficacy, therefore can not satisfy radar, aircraft and the more and more high requirement of other special equipments.Dielectric substance provided by the invention exactly can satisfy this harsh requirement.In addition, the specific inductivity of the dielectric substance that the present invention proposes is higher, and the room temperature dielectric constant that is higher than existing similar heat stable material is not higher than 2800 level.
Description of drawings
Fig. 1 is the test result of the dielectric material of the present invention's excellent property that can realize.
Embodiment
Present embodiment is a kind of temperature change resistance composite high-dielectric electronic material and preparation method thereof, adopts raw material to be: chemical pure BaTiO
3, chemical pure PbO, chemical pure TiO
2, analytical pure SnO
2, chemical pure NaCO
3, chemical pure Bi
2O
3, chemical pure TiO
2, chemical pure MgO, analytical pure Sm
2O
3
Its component and raw material weight per-cent thereof are as follows: BaTiO
3Be 42～45%, (Na
0.5, Bi
0.5) TiO
3Frit is 19～26%, Pb (Sn
0.6, Ti
0.4) O
3Frit is 28～38%, and MgO is for O.6～1%, Sm
2O
3Be 0.2～2%; Pb (Sn wherein
0.6, Ti
0.4) O
3Use PbO, SnO
2With TiO
2Preparation, PbO, SnO
2With TiO
2Mol ratio be 5: 3: 2; (Na
0.5, Bi
0.5) TiO
3Use NaCO
3, Bi
2O
3With TiO
2Preparation, NaCO
3, Bi
2O
3With TiO
2Mol ratio be 2: 1: 4.
Specific embodiment is as follows:
Embodiment one:
(1) prefabricated Pb (Sn
0.6, Ti
0.4) O
3: press PbO, SnO
2With TiO
2Mol ratio be 5: 3: 2 the batching, batching is inserted ball mill, add 3 times of volumes of deionized water ball millings 12 hours, oven dry obtains powder under 105 ℃ of environment, powder by 200 purpose screen clothes, is heated to 990 ℃ of insulations 5 hours with the powder after sieving, and the room temperature cooling makes Pb (Sn
0.6, Ti
0.4) O
3
(2) prefabricated (Na
0.5, Bi
0.5) TiO
3: press NaCO
3, Bi
2O
3With TiO
2Mol ratio be 2: 1: 4 the batching, batching is inserted ball mill, add 3 times of volumes of deionized water ball millings 12 hours, oven dry obtains powder under 105 ℃ of environment, powder by 200 purpose screen clothes, is heated to 900 ℃ of ℃ of insulations 2.5 hours with the powder after sieving, and the room temperature cooling makes (Na
0.5, Bi
0.5) TiO
3
(3) according to weight BaTiO
3Be 42%, (Na
0.5, Bi
0.5) TiO
3Frit is 19%, Pb (Sn
0.6, Ti
0.4) O
3Frit is 38%, and MgO is for O.6%, Sm
2O
3Be 0.4% preparation raw material, with joining raw material insert ball mill, add the deionized water ball milling 9 hours of 3 times of volumes; Oven dry obtains powder under 105 ℃ of environment then, powder is passed through 500 purpose screen clothes, the organic binder bond or the paraffin that add 5% weight ratio in the powder after sieving, add 120Mpa pressure and make green compact, be heated to 1200 ℃ of insulations 7 hours afterwards, the room temperature cooling makes temperature change resistance composite high-dielectric electronic material.
Embodiment two:
(1) prefabricated Pb (Sn
0.6, Ti
0.4) O
3: press PbO, SnO
2With TiO
2Mol ratio be 5: 3: 2 the batching, batching is inserted ball mill, add 3 times of volumes of deionized water ball millings 8 hours, oven dry obtains powder under 105 ℃ of environment, powder by 200 purpose screen clothes, is heated to 990 ℃ of insulations 5 hours with the powder after sieving, and the room temperature cooling makes Pb (Sn
0.6, Ti
0.4) O
3
(2) prefabricated (Na
0.5, Bi
0.5) TiO
3: press NaCO
3, Bi
2O
3With TiO
2Mol ratio be 2: 1: 4 the batching, batching is inserted ball mill, add 3 times of volumes of deionized water ball millings 8 hours, oven dry obtains powder under 105 ℃ of environment, powder by 200 purpose screen clothes, is heated to 920 ℃ of insulations 2 hours with the powder after sieving, and the room temperature cooling makes (Na
0.5, Bi
0.5) TiO
3
(3) according to weight BaTiO
3Be 43%, (Na
0.5, Bi
0.5) TiO
3Frit is 21%, Pb (Sn
0.6, Ti
0.4) O
3Frit is 34%, and MgO is 0.8%, Sm
2O
3Be 1.2% preparation raw material, with joining raw material insert ball mill, add the deionized water ball milling 12 hours of 3 times of volumes; Oven dry obtains powder under 105 ℃ of environment then, powder is passed through 500 purpose screen clothes, the organic binder bond or the paraffin that add 6% weight ratio in the powder after sieving, add 120Mpa pressure and make green compact, be heated to 1190 ℃ of insulations 8 hours afterwards, the room temperature cooling makes temperature change resistance composite high-dielectric electronic material.
Embodiment three:
(1) prefabricated Pb (Sn
0.6, Ti
0.4) O
3: press PbO, SnO
2With TiO
2Mol ratio be 5: 3: 2 the batching, batching is inserted ball mill, add 3 times of volumes of deionized water ball millings 12 hours, oven dry obtains powder under 105 ℃ of environment, powder by 200 purpose screen clothes, is heated to 990 ℃ of insulations 5 hours with the powder after sieving, and the room temperature cooling makes Pb (Sn
0.6, Ti
0.4) O
3
(2) prefabricated (Na
0.5, Bi
0.5) TiO
3: press NaCO
3, Bi
2O
3With TiO
2Mol ratio be 2: 1: 4 the batching, batching is inserted ball mill, add 3 times of volumes of deionized water ball millings 12 hours, oven dry obtains powder under 105 ℃ of environment, powder by 200 purpose screen clothes, is heated to 920 ℃ of insulations 1.5 hours with the powder after sieving, and the room temperature cooling makes (Na
0.5, Bi
0.5) TiO
3
(3) according to weight BaTiO
3Be 45%, (Na
0.5, Bi
0.5) TiO
3Frit is 23%, Pb (Sn
0.6, Ti
0.4) O
3Frit is 29%, and MgO is 1%, Sm
2O
3Be 2% preparation raw material, with joining raw material insert ball mill, add the deionized water ball milling 12 hours of 3 times of volumes; Oven dry obtains powder under 105 ℃ of environment then, powder is passed through 500 purpose screen clothes, the organic binder bond or the paraffin that add 6% weight ratio in the powder after sieving, add 120Mpa pressure and make green compact, be heated to 1200 ℃ of insulations 9 hours afterwards, the room temperature cooling makes temperature change resistance composite high-dielectric electronic material.
The foregoing description provides three kinds of different ingredients respectively, is met the composite high-dielectric electronic material of different sintering temperatures, differing dielectric constant.With obtain the coated metal electrode of electronic material, under the LCF of 1KHz frequency, in the different isoperibol, measure electrical capacity and also calculate relative permittivity ε.
The test result of the dielectric material of the excellent property that can realize for the present invention in the accompanying drawing 1, as Fig. 1, room temperature dielectric constant is 2950, remains in 15% at the absolute value of-55～+ 200 ℃ of following change in dielectric constant rates, can satisfy radar, aircraft and the more and more high requirement of other special equipments.
Dielectric substance of the present invention is applicable to electron devices commonly used such as wave filter, electrical condenser, is particularly useful for requiring to guarantee under-55～+ 200 ℃ of mal-conditions the electronic system of high reliability.
More than disclosed only be specific embodiments of the invention; though the present invention discloses as above with preferred embodiment; but the present invention is not limited thereto; any those skilled in the art can think variation; in not breaking away from design philosophy of the present invention and scope; the present invention is carried out various changes and retouching, all should drop within protection scope of the present invention.
Claims (3)
1. a temperature change resistance composite high-dielectric electronic material is characterized in that, the weight percent of its component and raw material thereof is as follows: BaTiO
3Be 42～45%, (Na
0.5, Bi
0.5) TiO
3Be 19～26%, Pb (Sn
0.6, Ti
0.4) O
3Be 28～38%, MgO is 0.6～1%, Sm
2O
3Be 0.2～2%.
2. a temperature change resistance composite high-dielectric electronic material as claimed in claim 1 is characterized in that, the Pb (Sn in described component and the raw material thereof
0.6, Ti
0.4) O
3Use PbO, SnO
2With TiO
2Preparation, PbO, SnO
2With TiO
2Mol ratio be 5: 3: 2; (Na in described component and the raw material thereof
0.5, Bi
0.5) TiO
3Use NaCO
3, Bi
2O
3With TiO
2Preparation, NaCO
3, Bi
2O
3With TiO
2Mol ratio be 2: 1: 4.
3. the preparation method of a temperature change resistance composite high-dielectric electronic material as claimed in claim 1 is characterized in that, comprises the steps:
(1) prefabricated Pb (Sn
0.6, Ti
0.4) O
3: press PbO, SnO
2With TiO
2Mol ratio be 5: 3: 2 the batching, batching is inserted ball mill, add 1～3 times of volumes of deionized water ball milling 1～12 hour, oven dry obtains powder under 105 ℃ of environment, powder is passed through 200 purpose screen clothes, powder after sieving is heated to 980 ℃～990 ℃ insulations 3～5 hours, and the room temperature cooling makes Pb (Sn
0.6, Ti
0.4) O
3
(2) prefabricated (Na
0.5, Bi
0.5) TiO
3: press NaCO
3, Bi
2O
3With TiO
2Mol ratio be 2: 1: 4 the batching, batching is inserted ball mill, add 1～3 times of volumes of deionized water ball milling 1～12 hour, oven dry obtains powder under 105 ℃ of environment, powder is passed through 200 purpose screen clothes, powder after sieving is heated to 900 ℃～920 ℃ insulations 1.5～2.5 hours, and the room temperature cooling makes (Na
0.5, Bi
0.5) TiO
3
(3) according to weight BaTiO
3Be 42～45%, (Na
0.5, Bi
0.5) TiO
3Frit is 19～26%, Pb (Sn
0.6, Ti
0.4) O
3Frit is 28～38%, and MgO is 0.6～1%, Sm
2O
3Be 0.2～2% preparation raw material, with joining raw material insert ball mill, add the deionized water ball milling 1～12 hour of 1～3 times of volume; Oven dry obtains powder under 105 ℃ of environment then, powder is passed through 500 purpose screen clothes, the organic binder bond or the paraffin that add 5%～6% weight ratio in the powder after sieving, add 90～120Mpa pressure and make green compact, be heated to 1180 ℃～1200 ℃ insulations 4～9 hours afterwards, the room temperature cooling makes temperature change resistance composite high-dielectric electronic material.
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|---|---|---|---|
| CN2010101477700A CN101851091B (en) | 2010-04-14 | 2010-04-14 | Temperature change resistance composite high-dielectric electronic material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101477700A CN101851091B (en) | 2010-04-14 | 2010-04-14 | Temperature change resistance composite high-dielectric electronic material and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN101851091A true CN101851091A (en) | 2010-10-06 |
| CN101851091B CN101851091B (en) | 2012-09-12 |
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|---|---|---|---|
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05290627A (en) * | 1992-04-08 | 1993-11-05 | Nikko Co | Manufacture of high frequency dielectric bzn sintered body |
| US5449652A (en) * | 1993-06-04 | 1995-09-12 | Battelle Memorial Institute | Ceramic compositions for BZN dielectric resonators |
| JP2000044341A (en) * | 1998-07-22 | 2000-02-15 | Amecs Corp Ltd | Dielectric ceramic composition |
| CN1382841A (en) * | 2002-03-12 | 2002-12-04 | 中国科学院上海硅酸盐研究所 | Melt method for growing sosoloid monocrystal of lead lead-titanate niobium-zincate |
| CN1636930A (en) * | 2004-12-07 | 2005-07-13 | 天津大学 | Composite and prepn process of electronic ceramic material with superhigh temperature stability |
-
2010
- 2010-04-14 CN CN2010101477700A patent/CN101851091B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05290627A (en) * | 1992-04-08 | 1993-11-05 | Nikko Co | Manufacture of high frequency dielectric bzn sintered body |
| US5449652A (en) * | 1993-06-04 | 1995-09-12 | Battelle Memorial Institute | Ceramic compositions for BZN dielectric resonators |
| JP2000044341A (en) * | 1998-07-22 | 2000-02-15 | Amecs Corp Ltd | Dielectric ceramic composition |
| CN1382841A (en) * | 2002-03-12 | 2002-12-04 | 中国科学院上海硅酸盐研究所 | Melt method for growing sosoloid monocrystal of lead lead-titanate niobium-zincate |
| CN1636930A (en) * | 2004-12-07 | 2005-07-13 | 天津大学 | Composite and prepn process of electronic ceramic material with superhigh temperature stability |
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| Publication number | Publication date |
|---|---|
| CN101851091B (en) | 2012-09-12 |
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