CN1699276A - Low-temperature sintered zinc titanate high-frequency dielectric ceramic and preparation method thereof - Google Patents
Low-temperature sintered zinc titanate high-frequency dielectric ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a low-temperature sintered zinc titanate high-frequency dielectric ceramic and preparation method, wherein the ceramic comprises zinc oxide produced by decomposing one portion of basic zinc carbonate, one portion of anatase nano-TiO2 and 0.75-1.00 wt% of vanadium pentoxide and diboron trioxide additive, wherein the basic zinc carbonate is used for producing zinc oxide, the preparation comprises ball grinding, drying, grinding, forming, pre-calcination, sintering and silvering.
Description
(1) technical field
The present invention relates to the high-frequency dielectric ceramic field of material subject, but be a kind of low temperature agglomerating zinc titanate high-frequency dielectric ceramic and preparation method thereof.
(2) background technology
In recent years, along with the fast development of mobile communication and satellite communication, as the material of high-frequency integrated circuit or dielectric resonator---high-frequency dielectric ceramic has very big demand.
In addition, the progress of portable information communication equipment has caused various because the various types of wiring boards that multicore sheet high-frequency element or LTCC (LTCC) produce and the development of multi-chip module, this just requires device miniaturization, chip type, lightweight, impel media ceramic to realize that lamination burns altogether, wherein require to have the metal or alloy of good electrical conductivity as interior electrode with other dielectric materialss or inductive material.Up to the present the representative high-frequency dielectric composition of well-known as: zirconia titanate tin system, barium oxide-TiO 2 series and as tantalum zincic acid barium, BMT, the niobium zincic acid barium of barium-uhligite family, many under 1300-1500 ℃ high temperature sintering, therefore, carrying out to adopt the high palladium of price, platinum or palladium/silver alloys when lamination burns altogether as inner electrode.
Silver and copper are cheap, have little high-frequency loss and favorable conductive rate, are the best alternative materials of electrode in the slice component.But the fusing point of silver and copper is very low, is respectively 961 ℃ and 1085 ℃, be lower than the sintering temperature of general stupalith, therefore, realizing dielectric materials and Ferrite Material, and during the co-sintered sintering between dielectric materials and the dielectric materials, electrode materials is melted at low temperatures, ineffective.In recent years, research can with silver, copper or the common low sintering media ceramic of silver/copper alloy, become one of the focus of electronic material research field and difficult point.At present, the technology of reduction sintering temperature commonly used mainly contains three kinds: chemical synthesis, as sol-gel method etc.; The special sintering method, such as hot pressed sintering, HIP sintering, microwave sintering etc.; Doping low melting point sintering aid.But, this several method has the defective that himself is difficult to overcome, chemical synthesis and special sintering method often need special equipment, and expensive raw material, and complex process, be unfavorable for realizing the suitability for industrialized production requirement, and the low melting point sintering aid that mixes merely can reduce the dielectric properties of material, also be difficult to further popularization in the long term.
(3) summary of the invention
Make for overcoming special equipment of the needs that exist in the prior art and expensive raw material that preparation cost increases, the low deficiency of dielectric properties of complicated process of preparation and material, but the present invention proposes a kind of low temperature agglomerating zinc titanate high-frequency dielectric ceramic and preparation method thereof, and its sintering temperature is from 850～950 ℃.
Raw material of the present invention comprises zinc subcarbonate, nano-anatase mine-titanium oxide and additive, and wherein, zinc subcarbonate is with generating zinc oxide, and additive is Vanadium Pentoxide in FLAKES and boron trioxide.Proportioning raw materials is: 1 part of zinc subcarbonate decomposes the zinc oxide that generates, the additive of 1 part of nano-anatase mine-titanium oxide and 0.75～1.00 weight %.
The present invention utilizes zinc subcarbonate to obtain the starting raw material zinc oxide of preparation ceramic composition, and resulting zinc oxide is nano level, has very high activity, can promote ceramic post sintering.Detailed process is:
(1) make it be decomposed into zinc oxide analytically pure zinc subcarbonate heating, Heating temperature is 350 ℃, and soaking time is 3 hours, and temperature rise rate is 5 ℃/minute.
(2) 1: 1 in molar ratio proportioning of zinc oxide and nano-anatase mine-titanium oxide is mixed the back ball milling, and oven dry, grinding, pre-burning.Wherein calcined temperature is 700 ℃, and the time is 2 hours, and bake out temperature is 80～100 ℃, and the time is 3～6 hours.
(3) add Vanadium Pentoxide in FLAKES and boron trioxide additive.The mol ratio of Vanadium Pentoxide in FLAKES and boron trioxide is: 1～3: 3～1, and addition is 0.75～1.00 weight %.
(4) ball milling, oven dry once more adds the polyvinyl alcohol adhesive aqueous solution and ground 2 hours, produces the particle of about 200 microns sizes, and pressure forming.
(5) the sample thermal treatment after the moulding, burn out binder, and with biscuit sintering between 850 ℃ to 950 ℃ temperature, its temperature rise rate is 10 ℃/minute.
(6) sample behind the sintering is ground through polishing, and behind the even coated with conductive silver slurry of its surface, thermal treatment between 550～620 ℃ of temperature, its heating-up time is 3.5～5 hours.
(7) sample behind the silver ink firing is polished.
The present invention is not when changing preparation technology, according to different needs, only need to change the proportioning of additive Vanadium Pentoxide in FLAKES and boron trioxide, just can obtain the specific inductivity and the dielectric loss value of a series of variations, and guarantee that still ceramic sintering temperature maintains below 900 ℃.
The invention has the advantages that and to use equipment commonly used, as resistance furnace, baking oven, ball mill etc., the cheap raw material that employing is easy to obtain, use simple operational path realize the zinc titanate media ceramic at sintering below 900 ℃, be applicable to that making is with the slice component of base metals such as silver, copper or silver/copper alloy as interior electrode, as lamination sheet type wave filter, lamination sheet type electrical condenser/inducer multiple device and low-temperature sintering substrate, resonator and wave filter or ceramic antenna etc., thereby reduced the cost of manufacture of slice component significantly.
(4) embodiment
Embodiment one:
Present embodiment has adopted chemical process to obtain the starting raw material zinc oxide of preparation ceramic composition.The proportioning raw materials of present embodiment is: 1 part of zinc subcarbonate decomposes the zinc oxide that generates, and 1 part of nano-anatase mine-titanium oxide adds the additive of 1.00 weight %, and additive is 100 in the base-material gross weight.
Preparation process is:
(1) analytically pure zinc subcarbonate is heated to 350 ℃ and makes it be decomposed into zinc oxide, soaking time is 3 hours, and temperature rise rate is 5 ℃/minute.The particle diameter of gained zinc oxide is 50～80 nanometers.
(2) with zinc oxide and 1: 1 in molar ratio proportioning of nano-anatase mine-titanium oxide, with planetary mills mixing and ball milling 24 hours in the polyethylene jar, with dehydrated alcohol, the zirconium ball is a medium, and wherein the titanium dioxide particle diameter is 30～50 nanometers.Wet feed behind the ball milling with 85 ℃ of oven dry 3.5 hours, uses agate mortar levigate dry powder in baking oven then, places corundum crucible, 700 ℃ of pre-burnings 2 hours.
(3) the pre-burning powder adds additive after agate mortar is levigate, and additive is Vanadium Pentoxide in FLAKES and boron trioxide, and addition is 0.80 weight %, and wherein the mole proportioning of Vanadium Pentoxide in FLAKES and the compound additive of boron trioxide is 3: 1, is designated as 3VB.
(4) ball milling 12 hours once more, oven dry is to the polyvinyl alcohol adhesive aqueous solution that wherein adds 2.00 weight %, ground 2 hours with agate mortar, produce the particle of about 200 microns sizes, with the forming under the pressure of this particle in 120 MPas, the size of moulding sample is decided according to mould.
(5) the sample after the moulding in resistance furnace through 520 ℃ of thermal treatments, burn out binder, wherein, the heating-up time is 7 hours, soaking time is 1.5 hours.Then, with the biscuit of the burn out binder temperature at 900 ℃, sintering is 4 hours under the air atmosphere, and temperature rise rate is 10 ℃/minute.
(6) sample behind the sintering is ground with the carborundum polishing sand paper,, require the silver slurry to cover specimen surface evenly, fully at its surperficial homogeneous conductive silver slurry.Then, will apply the silver-colored sample of starching 560 ℃ of thermal treatments 5 hours, the heating-up time is 3.5 hours.
(7) sample behind the silver ink firing is carefully polished off the silver of seamed edge with sand paper, do not form short circuit to guarantee its upper and lower surface.
Use HP-4294A type electric impedance analyzer to test dielectric properties at ambient temperature, test frequency is 1 megahertz and 10 megahertzes.Under the test frequency of 10 megahertzes, the relative permittivity ε of gained pottery is 22.4, and dielectric loss is 2.39 * 10 for tg δ
-3
Embodiment two:
Present embodiment has adopted chemical process to obtain the starting raw material zinc oxide of preparation ceramic composition.The proportioning raw materials of present embodiment is: 1 part of zinc subcarbonate decomposes the zinc oxide that generates, and 1 part of nano-anatase mine-titanium oxide adds the additive of 1.00 weight %, and additive is 100 in the base-material gross weight.
Preparation process is:
(1) analytically pure zinc subcarbonate is heated to 350 ℃ and makes it be decomposed into zinc oxide, soaking time is 3 hours, and temperature rise rate is 5 ℃/minute.The particle diameter of gained zinc oxide is 50～80 nanometers.
(2) with zinc oxide and 1: 1 in molar ratio proportioning of nano-anatase mine-titanium oxide, with planetary mills mixing and ball milling 24 hours in the polyethylene jar, with dehydrated alcohol, the zirconium ball is a medium, and wherein the titanium dioxide particle diameter is 30～50 nanometers.Wet feed behind the ball milling with 90 ℃ of oven dry 4.5 hours, uses agate mortar levigate dry powder in baking oven then, places corundum crucible, 700 ℃ of pre-burnings 2 hours.
(3) the pre-burning powder adds additive after agate mortar is levigate, and additive is Vanadium Pentoxide in FLAKES and boron trioxide, and addition is 0.90 weight %, and wherein the mole proportioning of Vanadium Pentoxide in FLAKES and the compound additive of boron trioxide is 1: 3, is designated as VB3.
(4) ball milling 12 hours once more, oven dry is to the polyvinyl alcohol adhesive aqueous solution that wherein adds 2.00 weight %, ground 2 hours with agate mortar, produce the particle of about 200 microns sizes, with the forming under the pressure of this particle in 120 MPas, the size of moulding sample is decided according to mould.
(5) the sample after the moulding in resistance furnace through 550 ℃ of thermal treatments, burn out binder, wherein, the heating-up time is 7 hours, soaking time is 1.5 hours.Then, with the biscuit of the burn out binder temperature at 875 ℃, sintering is 4 hours under the air atmosphere, and temperature rise rate is 10 ℃/minute.
(6) sample behind the sintering is ground with the carborundum polishing sand paper,, require the silver slurry to cover specimen surface evenly, fully at its surperficial homogeneous conductive silver slurry.Then, will apply the silver-colored sample of starching 580 ℃ of thermal treatments 5 hours, the heating-up time is 4 hours.
(7) sample behind the silver ink firing is carefully polished off the silver of seamed edge with sand paper, do not form short circuit to guarantee its upper and lower surface.
Use HP-4294A type electric impedance analyzer to test dielectric properties at ambient temperature, test frequency is 1 megahertz and 10 megahertzes.Under the test frequency of 10 megahertzes, the relative permittivity ε of gained pottery is 27.3, and dielectric loss tg δ is 1.92 * 10
-3Concrete dielectric properties are as shown in table 1.
Embodiment three:
Present embodiment has adopted chemical process to obtain the starting raw material zinc oxide of preparation ceramic composition.The proportioning raw materials of present embodiment is: 1 part of zinc subcarbonate decomposes the zinc oxide that generates, and 1 part of nano-anatase mine-titanium oxide adds the additive of 1.00 weight %, and additive is 100 in the base-material gross weight.
Preparation process is:
(1) analytically pure zinc subcarbonate is heated to 350 ℃ and makes it be decomposed into zinc oxide, soaking time is 3 hours, and temperature rise rate is 5 ℃/minute.The particle diameter of gained zinc oxide is 50～80 nanometers.
(2) with zinc oxide and 1: 1 in molar ratio proportioning of nano-anatase mine-titanium oxide, with planetary mills mixing and ball milling 24 hours in the polyethylene jar, with dehydrated alcohol, the zirconium ball is a medium, and wherein the titanium dioxide particle diameter is 30～50 nanometers.Wet feed behind the ball milling with 100 ℃ of oven dry 5.5 hours, uses agate mortar levigate dry powder in baking oven then, places corundum crucible, 700 ℃ of pre-burnings 2 hours.
(3) the pre-burning powder adds additive after agate mortar is levigate, and additive is Vanadium Pentoxide in FLAKES and boron trioxide, and addition is 1.00 weight %, and wherein the mole proportioning of Vanadium Pentoxide in FLAKES and the compound additive of boron trioxide is 1: 1, is designated as VB.
(4) ball milling 12 hours once more, oven dry is to the polyvinyl alcohol adhesive aqueous solution that wherein adds 2.00 weight %, ground 2 hours with agate mortar, produce the particle of about 200 microns sizes, with the forming under the pressure of this particle in 120 MPas, the size of moulding sample is decided according to mould.
(5) the sample after the moulding in resistance furnace through 580 ℃ of thermal treatments, burn out binder, wherein, the heating-up time is 7 hours, soaking time is 1.5 hours.Then, with the biscuit of the burn out binder temperature at 930 ℃, sintering is 4 hours under the air atmosphere, and temperature rise rate is 10 ℃/minute.
(6) sample behind the sintering is ground with the carborundum polishing sand paper,, require the silver slurry to cover specimen surface evenly, fully at its surperficial homogeneous conductive silver slurry.Then, will apply the silver-colored sample of starching 600 ℃ of thermal treatments 5 hours, the heating-up time is 5 hours.
(7) sample behind the silver ink firing is carefully polished off the silver of seamed edge with sand paper, do not form short circuit to guarantee its upper and lower surface.
Use HP-4294A type electric impedance analyzer to test dielectric properties at ambient temperature, test frequency is 1 megahertz and 10 megahertzes.Under the test frequency of 10 megahertzes, the relative permittivity ε of gained pottery is 18.4, and dielectric loss is 3.83 * 10 for tg δ
-3
Claims (2)
1. but low temperature agglomerating zinc titanate high-frequency dielectric ceramic is characterized in that:
A. as starting raw material, wherein, zinc subcarbonate is with generating zinc oxide with zinc subcarbonate and nano-anatase mine-titanium oxide for this high-frequency dielectric ceramic composition, and additive is Vanadium Pentoxide in FLAKES and boron trioxide;
B. its proportioning raw materials is: 1 part of zinc subcarbonate decomposes the zinc oxide that generates, 1 part of nano-anatase mine-titanium oxide, and the additive of 0.75～1.00 weight %;
C. the mol ratio of Vanadium Pentoxide in FLAKES and boron trioxide is: 1～3: 3～1, and addition is 0.75～1.00 weight %.
2. one kind prepares the method for high-frequency dielectric ceramic according to claim 1, raw material is prepared burden according to a certain ratio, and pass through ball milling, oven dry, grinding, moulding, pre-burning, sintering and be coated with silver, makes pottery, it is characterized in that:
A. make it be decomposed into zinc oxide analytically pure zinc subcarbonate heating, Heating temperature is 350 ℃, and soaking time is 3 hours, and temperature rise rate is 5 ℃/minute;
B. the calcined temperature of powder mix is 700 ℃, and the time is 2 hours;
C. in the pre-burning powder, add Vanadium Pentoxide in FLAKES and boron trioxide additive, and ball milling, oven dry.
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| CN100335442C (en) * | 2005-12-23 | 2007-09-05 | 北京科技大学 | Method for preparing zinc titanite based microwave ceramic under low temperature |
| CN102167580A (en) * | 2010-12-23 | 2011-08-31 | 西安科技大学 | Dielectric ceramic for high-frequency section and preparation method thereof |
| CN101445364B (en) * | 2008-12-30 | 2012-02-15 | 西安广芯电子科技有限公司 | Zn-Ni-Ti microwave media ceramic capable of being sintered at low temperature and having high dielectric constant and preparation method thereof |
| CN103693682A (en) * | 2014-01-07 | 2014-04-02 | 哈尔滨工业大学 | Synthesis method of ZnTiO3 porous nano material |
| CN105016380A (en) * | 2015-08-19 | 2015-11-04 | 徐州工程学院 | Low-temperature solid-phase synthesis method of ZnTiO3 micro crystal |
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| JP3406787B2 (en) * | 1996-09-30 | 2003-05-12 | 京セラ株式会社 | Manufacturing method of dielectric porcelain |
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- 2005-05-25 CN CNB2005100427101A patent/CN1294103C/en not_active Expired - Fee Related
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| CN100335442C (en) * | 2005-12-23 | 2007-09-05 | 北京科技大学 | Method for preparing zinc titanite based microwave ceramic under low temperature |
| CN101445364B (en) * | 2008-12-30 | 2012-02-15 | 西安广芯电子科技有限公司 | Zn-Ni-Ti microwave media ceramic capable of being sintered at low temperature and having high dielectric constant and preparation method thereof |
| CN102167580A (en) * | 2010-12-23 | 2011-08-31 | 西安科技大学 | Dielectric ceramic for high-frequency section and preparation method thereof |
| CN103693682A (en) * | 2014-01-07 | 2014-04-02 | 哈尔滨工业大学 | Synthesis method of ZnTiO3 porous nano material |
| CN105016380A (en) * | 2015-08-19 | 2015-11-04 | 徐州工程学院 | Low-temperature solid-phase synthesis method of ZnTiO3 micro crystal |
| CN109825879A (en) * | 2019-02-27 | 2019-05-31 | 徐超 | A kind of preparation method of metallic fiber dispersed material and its application in pipeline material |
| CN110229002A (en) * | 2019-07-04 | 2019-09-13 | 贵州振华电子信息产业技术研究有限公司 | A kind of low-temperature co-burning ceramic material and preparation method |
| CN110229002B (en) * | 2019-07-04 | 2022-04-22 | 贵州振华电子信息产业技术研究有限公司 | Low-temperature co-fired ceramic material and preparation method thereof |
| CN112034147A (en) * | 2020-08-19 | 2020-12-04 | 江苏国瓷泓源光电科技有限公司 | Method for detecting weldability of silver paste of ceramic filter |
| CN112034147B (en) * | 2020-08-19 | 2022-08-12 | 江苏国瓷泓源光电科技有限公司 | Method for detecting weldability of silver paste of ceramic filter |
| CN113415823A (en) * | 2021-05-25 | 2021-09-21 | 福建省云智新材料科技有限公司 | Preparation method of zinc titanate for thermal control coating of spacecraft |
| CN113415823B (en) * | 2021-05-25 | 2024-03-29 | 福建省云智新材料科技有限公司 | Preparation method of zinc orthotitanate for spacecraft thermal control coating |
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