CN101747036A - Low-frequency dielectric ceramic with low-temperature sintering and ultralow temperature change ratio and preparation method thereof - Google Patents

Low-frequency dielectric ceramic with low-temperature sintering and ultralow temperature change ratio and preparation method thereof Download PDF

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CN101747036A
CN101747036A CN200910254380A CN200910254380A CN101747036A CN 101747036 A CN101747036 A CN 101747036A CN 200910254380 A CN200910254380 A CN 200910254380A CN 200910254380 A CN200910254380 A CN 200910254380A CN 101747036 A CN101747036 A CN 101747036A
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CN101747036B (en
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苏皓
方芳
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Hebei University of Science and Technology
Hebei Polytechnic University
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Abstract

The invention discloses low-frequency dielectric ceramic with low-temperature sintering and ultralow temperature change ratio and a preparation method thereof. The low-frequency dielectric ceramic comprises the following components and raw materials in percentage by weight: 57 to 72 percent of BaTiO3, 6 to 12 percent of PbTiO3 fusion block, 9 to 16 percent of (Na, Bi) TiO3 fusion block, 4 to 8 percent of Nb2O5, 0.7 to 1.5 percent of MgO, 0.1 to 3 percent of Sm2O3, 1.2 to 5 percent of SnO2 and 0.2 to 3 percent of ZnO; wherein the PbTiO3 fusion block is prepared from PbO and TiO2 according to the weight ratio of 1 to 1.2; the (Na, Bi) TiO3 fusion block is prepared from NaCO3, Bi2O3 and TiO2 according to the weight ratio of a: b: c, wherein a is from 70 to 73, b is from 115 to 118, and c is from 154 to 164. The preparation method comprises the following steps of: (1) prefabricating the PbTiO3 fusion block; (2) prefabricating the (Na, Bi) TiO3 fusion block; and (3) forming a blank and sintering. The dielectric ceramic is suitable for electronic components of capacitors, filters, and the like, and low in manufacturing cost.

Description

Ultralow rate of temperature change frequency dielectric ceramic with low of low-temperature sintering and preparation method thereof
Technical field
The present invention relates to a kind of is the ceramic composition of feature with the composition, specifically, but is ultralow rate of temperature change frequency dielectric ceramic with low of a kind of low-temperature sintering and preparation method thereof.
Background technology
Current, frequency dielectric ceramic with low has two important developing direction: low temperature co-fired and high-temperature stability.
LTCC Technology (Low Temperature Cofired Ceramic, LTCC) be that the low-temperature sintered ceramics powder is made the accurate and fine and close green band of thickness, on the green band, utilize technologies such as laser boring, micropore slip casting, accurate conductor paste printing to make the circuitry needed figure, and a plurality of passive devices (as electrical condenser, wave filter, coupling mechanism etc.) are imbedded in the multilayer ceramic substrate, overlap together then, then at sintering below 900 ℃.Because sintering temperature is lower, internal and external electrode can use metals such as silver, copper, gold respectively, and needn't use expensive palladium-silver mixed electrods.The employed medium ceramic material of LTCC technical requirements can densification under the sintering temperature below 900 ℃, have dielectric properties preferably, and the densification temperature of generic media pottery is usually more than 1100 ℃, if low-temperature sintering then can make the quality factor of material sharply descend.
In addition, dielectric ceramics should have the wide operation temperature area of trying one's best, and has the specific inductivity rate of temperature change of trying one's best little in operation temperature area.If the specific inductivity rate of temperature change is bigger, the device that then makes can change electrical specification with variation of temperature in the middle of work, the parameter value of device is drifted about, and causes the circuit cisco unity malfunction, even causes complete machine to break down.Although worldwide research institution has carried out a large amount of research to dielectric ceramic material since half a century, make its performance perameter aspect a lot of, obtain bigger lifting, the specific inductivity rate of temperature change of current material is still bigger.In the standard that EIA formulates, the frequency dielectric ceramic with low material of X7R, X8R, three kinds of different operating warm areas of X9R is the specific inductivity rate of temperature change upper limit with 15% all, but 15% velocity of variation can influence circuit working in the middle of practical application, must expend extra circuit resource and remedy just and can make the circuit works better.If use the frequency dielectric ceramic with low of ultralow rate of temperature change, then can circuit layout with and make in significantly save cost, obtain higher stability, to satisfy the more and more high requirement of electronic system.
Summary of the invention
The objective of the invention is defective at prior art, one provides a kind of ultralow rate of temperature change frequency dielectric ceramic with low that can satisfy LTCC (LTCC) technology, and two provide the preparation method of the ultralow rate of temperature change frequency dielectric ceramic with low of this low-temperature sintering.
Realize that the foregoing invention purpose adopts following technical scheme:
The ultralow rate of temperature change frequency dielectric ceramic with low of a kind of low-temperature sintering, its component and raw material weight per-cent thereof are as follows: BaTiO 3Be 57～72%, PbTiO 3Frit is 6～12%, (Na, Bi) TiO 3Frit is 9～16%, Nb 2O 5Be 4～8%, MgO is 0.7～1.5%, Sm 2O 3Be 0.1～3%, SnO 2Be 1.2～5%, ZnO is 0.2～3%; PbTiO wherein 3Frit uses PbO and TiO 2Preparation, PbO and TiO 2Weight ratio be 1～1.2; (Na, Bi) TiO 3Frit uses NaCO 3, Bi 2O 3With TiO 2Weight ratio be a: b: c, wherein a value is 70～73, the b value is 115～118, the c value is 154～164.
The preparation method of the ultralow rate of temperature change frequency dielectric ceramic with low of a kind of low-temperature sintering comprises the steps:
(1) prefabricated PbTiO 3Frit: press PbO and TiO 2Weight ratio be 1～1.2 the batching, batching is inserted ball mill, add 1～3 times of volumes of deionized water ball milling 1～12 hour, under 105 ℃ of environment, dry or carry out spraying drying and obtain powder, powder is passed through 200 purpose screen clothes, the minus sieve material is heated to 930 ℃～960 ℃ insulations 2～3 hours, and the room temperature cooling makes PbTiO 3Frit;
(2) prefabricated (Na, Bi) TiO 3Frit: press NaCO 3, Bi 2O 3With TiO 2Weight ratio be a: b: c batching, wherein a value is 70～73, the b value is 115～118, the c value is 154～164; Batching is inserted ball mill, add 1～3 times of volumes of deionized water ball milling 1～12 hour, under 105 ℃ of environment, dry or carry out spraying drying and obtain powder, powder is passed through 200 purpose screen clothes, the minus sieve material is heated to 900 ℃～920 ℃ insulations 1.5～2.5 hours, the room temperature cooling makes (Na, Bi) TiO 3Frit;
(3) according to weight BaTiO 3Be 57～72%, PbTiO 3Frit is 6～12%, (Na, Bi) TiO 3Frit is 9～16%, Nb 2O 5Be 4～8%, MgO is 0.7～1.5%, Sm 2O 3Be 0.1～3%, SnO 2Be 1.2～5%, ZnO is 0.2～3% 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; Under 105 ℃ of environment, dry or carry out spraying drying then and obtain powder, powder is passed through 500 purpose screen clothes, the organic binder bond or the paraffin that in the minus sieve material, add 5%～6% weight ratio, add 90～120Mpa pressure and make green compact, be heated to 840 ℃～875 ℃ insulations 2～3 hours afterwards, the room temperature cooling makes ceramic dielectic.
The invention has the beneficial effects as follows, a kind of low temperature sintering perovskite structure microwave-medium ceramics and preparation method are provided, can satisfy the requirement of LTCC Technology, has lower sintering temperature, have ultralow specific inductivity rate of temperature change simultaneously, saved great amount of cost in can and making in circuit layout, obtained higher stability.The raw materials for production that the present invention adopts all have cheap characteristics, have reduced raw materials cost.Satisfy technology such as working as third-generation mobile communication, satellite communications, broadcast television, radar, electronic countermeasure, guidance to highly reliable stabilization of electronics and requirement cheaply.
Description of drawings
The test result figure of the media ceramic of the excellent property that Fig. 1 can realize for the present invention.
Embodiment
Present embodiment is ultralow rate of temperature change frequency dielectric ceramic with low of a kind of low-temperature sintering and preparation method thereof, adopts raw material to be: chemical pure BaTiO 3, chemical pure PbO, chemical pure TiO 2, chemical pure NaCO 3, chemical pure Bi 2O 3, chemical pure TiO 2, chemical pure Nb 2O 5, chemical pure MgO, analytical pure Sm 2O 3, analytical pure SnO 2, analytical pure ZnO.
Its component and raw material weight per-cent thereof are as follows: BaTiO 3Be 57～72%, PbTiO 3Frit is 6～12%, (Na, Bi) TiO 3Frit is 9～16%, Nb 2O 5Be 4～8%, MgO is 0.7～1.5%, Sm 2O 3Be 0.1～3%, SnO 2Be 1.2～5%, ZnO is 0.2～3%; PbTiO wherein 3Frit uses PbO and TiO 2Preparation, PbO and TiO 2Weight ratio be 1～1.2; (Na, Bi) TiO 3Frit uses NaCO 3, Bi 2O 3With TiO 2Weight ratio be a: b: c, wherein a value is 70～73, the b value is 115～118, the c value is 154～164.
Specific embodiment is as follows:
Embodiment 1:
(1) prefabricated PbTiO 3Frit: press PbO and TiO 2Weight ratio be 1.02 the batching, batching is inserted ball mill, add 3 times of volumes of deionized water ball millings 7 hours, under 105 ℃ of environment, dry or carry out spraying drying and obtain powder, powder by 200 purpose screen clothes, is heated to 930 ℃ of insulations 3 hours with the minus sieve material, and the room temperature cooling makes PbTiO 3Frit;
(2) prefabricated (Na, Bi) TiO 3Frit: press NaCO 3, Bi 2O 3With TiO 2Weight ratio be 71: 117: 160 the batching, batching is inserted ball mill, add 3 times of volumes of deionized water ball millings 5 hours, under 105 ℃ of environment, dry or carry out spraying drying and obtain powder, powder is passed through 200 purpose screen clothes, the minus sieve material is heated to 920 ℃ of insulations 2.5 hours, and the room temperature cooling makes (Na, Bi) TiO 3Frit;
(3) according to weight BaTiO 3Be 66%, PbTiO 3Frit is 7%, (Na, Bi) TiO 3Frit is 11%, Nb 2O 5Be 6%, MgO is 0.9%, Sm 2O 3Be 2.1%, SnO 2Be 3.8%, ZnO is 2.2% preparation raw material, with joining raw material insert ball mill, add the deionized water ball milling 10 hours of 3 times of volumes; Under 105 ℃ of environment, dry or carry out spraying drying then and obtain powder, powder by 500 purpose screen clothes, is added the organic binder bond or the paraffin of 5% weight ratio in the minus sieve material, add 120Mpa pressure and make green compact, be heated to 875 ℃ of insulations 3 hours afterwards, the room temperature cooling makes ceramic dielectic.
Embodiment 2:
(1) prefabricated PbTiO 3Frit: press PbO and TiO 2Weight ratio be 1.07 the batching, batching is inserted ball mill, add 3 times of volumes of deionized water ball millings 7 hours, under 105 ℃ of environment, dry or carry out spraying drying and obtain powder, powder by 200 purpose screen clothes, is heated to 930 ℃ of insulations 3 hours with the minus sieve material, and the room temperature cooling makes PbTiO 3Frit;
(2) prefabricated (Na, Bi) TiO 3Frit: press NaCO 3, Bi 2O 3With TiO 2Weight ratio be 70: 115: 164 the batching, batching is inserted ball mill, add 3 times of volumes of deionized water ball millings 5 hours, under 105 ℃ of environment, dry or carry out spraying drying and obtain powder, powder is passed through 200 purpose screen clothes, the minus sieve material is heated to 950 ℃ of insulations 2.5 hours, and the room temperature cooling makes (Na, Bi) TiO 3Frit;
(3) according to weight BaTiO 3Be 63%, PbTiO 3Frit is 9%, (Na, Bi) TiO 3Frit is 13%, Nb 2O 5Be 5%, MgO is 0.9%, Sm 2O 3Be 1.9%, SnO 2Be 4.2%, ZnO is 3% preparation raw material, with joining raw material insert ball mill, add the deionized water ball milling 10 hours of 3 times of volumes; Under 105 ℃ of environment, dry or carry out spraying drying then and obtain powder, powder by 500 purpose screen clothes, is added the organic binder bond or the paraffin of 5% weight ratio in the minus sieve material, add 120Mpa pressure and make green compact, be heated to 860 ℃ of insulations 3 hours afterwards, the room temperature cooling makes ceramic dielectic.
Embodiment 3:
(1) prefabricated PbTiO 3Frit: press PbO and TiO 2Weight ratio be 1.13 the batching, batching is inserted ball mill, add 3 times of volumes of deionized water ball millings 7 hours, under 105 ℃ of environment, dry or carry out spraying drying and obtain powder, powder by 200 purpose screen clothes, is heated to 940 ℃ of insulations 3 hours with the minus sieve material, and the room temperature cooling makes PbTiO 3Frit;
(2) prefabricated (Na, Bi) TiO 3Frit: press NaCO 3, Bi 2O 3With TiO 2Weight ratio be 73: 118: 158 the batching, batching is inserted ball mill, add 3 times of volumes of deionized water ball millings 5 hours, under 105 ℃ of environment, dry or carry out spraying drying and obtain powder, powder is passed through 200 purpose screen clothes, the minus sieve material is heated to 900 ℃ of insulations 2.5 hours, and the room temperature cooling makes (Na, Bi) TiO 3Frit;
(3) according to weight BaTiO 3Be 69.3%, PbTiO 3Frit is 6.6%, (Na, Bi) TiO 3Frit is 9.1%, Nb 2O 5Be 8%, MgO is 1.3%, Sm 2O 3Be 3%, SnO 2Be 1.2%, ZnO is 1.5% preparation raw material, with joining raw material insert ball mill, add the deionized water ball milling 9 hours of 3 times of volumes; Under 105 ℃ of environment, dry or carry out spraying drying then and obtain powder, powder by 500 purpose screen clothes, is added the organic binder bond or the paraffin of 5% weight ratio in the minus sieve material, add 120Mpa pressure and make green compact, be heated to 840 ℃ of insulations 3 hours afterwards, the room temperature cooling makes ceramic dielectic.
The foregoing description provides three kinds of different ingredients respectively, is met the ceramic dielectic of different sintering temperatures, differing dielectric constant.With obtain the coated metal electrode of ceramic dielectic, under the LCF of 1KHz frequency, in the different isoperibol, measure electrical capacity and also calculate relative permittivity ε.
The test result of the media ceramic of the excellent property that can realize for the present invention in the accompanying drawing 1,25 ℃ of specific inductivity of room temperature are 1930, the absolute value of change in dielectric constant rate remains in 2% in-55～+ 150 ℃ of (X8R) operation temperature areas.
Dielectric ceramics of the present invention is applicable to wave filter, electron device commonly used such as electrical condenser can satisfy the requirement of LTCC Technology to sintering temperature, particularly has ultralow specific inductivity rate of temperature change, can guarantee high reliability, raw materials for production are cheap simultaneously.
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. the ultralow rate of temperature change frequency dielectric ceramic with low of low-temperature sintering is characterized in that its component and raw material weight per-cent thereof are as follows: BaTiO 3Be 57～72%, PbTiO 3Frit is 6～12%, (Na, Bi) TiO 3Frit is 9～16%, Nb 2O 5Be 4～8%, MgO is 0.7～1.5%, Sm 2O 3Be 0.1～3%, SnO 2Be 1.2～5%, ZnO is 0.2～3%.
2. the ultralow rate of temperature change frequency dielectric ceramic with low of low-temperature sintering as claimed in claim 1 is characterized in that the PbTiO in described component and the raw material thereof 3Frit uses PbO and TiO 2Preparation, PbO and TiO 2Weight ratio be 1～1.2; (Na, Bi) TiO 3Frit uses NaCO 3, Bi 2O 3With TiO 2Weight ratio be a: b: c, wherein a value is 70～73, the b value is 115～118, the c value is 154～164.
3. the preparation method of the ultralow rate of temperature change frequency dielectric ceramic with low of low-temperature sintering as claimed in claim 1 is characterized in that, comprises the steps:
(1) prefabricated PbTiO 3Frit: press PbO and TiO 2Weight ratio be 1～1.2 the batching, batching is inserted ball mill, add 1～3 times of volumes of deionized water ball milling 1～12 hour, under 105 ℃ of environment, dry or carry out spraying drying and obtain powder, powder is passed through 200 purpose screen clothes, the minus sieve material is heated to 930 ℃～960 ℃ insulations 2～3 hours, and the room temperature cooling makes PbTiO 3Frit;
(2) prefabricated (Na, Bi) TiO 3Frit: press NaCO 3, Bi 2O 3With TiO 2Weight ratio be a: b: c batching, wherein a value is 70～73, the b value is 115～118, the c value is 154～164; Batching is inserted ball mill, add 1～3 times of volumes of deionized water ball milling 1～12 hour, under 105 ℃ of environment, dry or carry out spraying drying and obtain powder, powder is passed through 200 purpose screen clothes, the minus sieve material is heated to 900 ℃～920 ℃ insulations 1.5～2.5 hours, the room temperature cooling makes (Na, Bi) TiO 3Frit;
(3) according to weight BaTiO 3Be 57～72%, PbTiO 3Frit is 6～12%, (Na, Bi) TiO 3Frit is 9～16%, Nb 2O 5Be 4～8%, MgO is 0.7～1.5%, Sm 2O 3Be 0.1～3%, SnO 2Be 1.2～5%, ZnO is 0.2～3% 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; Under 105 ℃ of environment, dry or carry out spraying drying then and obtain powder, powder is passed through 500 purpose screen clothes, the organic binder bond or the paraffin that in the minus sieve material, add 5%～6% weight ratio, add 90～120Mpa pressure and make green compact, be heated to 840 ℃～875 ℃ insulations 2～3 hours afterwards, the room temperature cooling makes ceramic dielectic.
CN2009102543800A 2009-12-22 2009-12-22 Low-frequency dielectric ceramic with low-temperature sintering and ultralow temperature change ratio and preparation method thereof Expired - Fee Related CN101747036B (en)

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CN103864418A (en) * 2014-02-27 2014-06-18 天津大学 Preparation method of ceramic capacitor dielectric with high dielectric constant and ultra-wide working temperature
CN103936411A (en) * 2014-04-03 2014-07-23 天津大学 Method for preparing ultra-wide temperature stable barium titanate dielectric material by adopting annealing method
CN103936410A (en) * 2014-04-03 2014-07-23 天津大学 Manganese carbonate-doped high-temperature stable barium titanate-based dielectric material
CN111410526A (en) * 2020-03-27 2020-07-14 广东风华高新科技股份有限公司 Perovskite-doped barium stannate material and preparation method and application thereof
CN114315350A (en) * 2022-01-24 2022-04-12 武汉理工大学 Sodium bismuth titanate-barium zirconate titanate lead-free wide-temperature energy storage ceramic and preparation method thereof

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CN1187483C (en) * 2002-03-12 2005-02-02 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
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CN103864418A (en) * 2014-02-27 2014-06-18 天津大学 Preparation method of ceramic capacitor dielectric with high dielectric constant and ultra-wide working temperature
CN103864418B (en) * 2014-02-27 2015-10-07 天津大学 The preparation method of the ceramic capacitor dielectric of high-k ultra-wide working temperature
CN103936411A (en) * 2014-04-03 2014-07-23 天津大学 Method for preparing ultra-wide temperature stable barium titanate dielectric material by adopting annealing method
CN103936410A (en) * 2014-04-03 2014-07-23 天津大学 Manganese carbonate-doped high-temperature stable barium titanate-based dielectric material
CN111410526A (en) * 2020-03-27 2020-07-14 广东风华高新科技股份有限公司 Perovskite-doped barium stannate material and preparation method and application thereof
CN111410526B (en) * 2020-03-27 2020-12-29 广东风华高新科技股份有限公司 Perovskite-doped barium stannate material and preparation method and application thereof
CN114315350A (en) * 2022-01-24 2022-04-12 武汉理工大学 Sodium bismuth titanate-barium zirconate titanate lead-free wide-temperature energy storage ceramic and preparation method thereof
CN114315350B (en) * 2022-01-24 2023-05-23 武汉理工大学 Bismuth sodium titanate-barium zirconate titanate leadless wide-temperature energy storage ceramic and preparation method thereof

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