CN110590335A - Ba2SmNbO6Preparation method of microwave dielectric material - Google Patents

Ba2SmNbO6Preparation method of microwave dielectric material Download PDF

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CN110590335A
CN110590335A CN201910820399.0A CN201910820399A CN110590335A CN 110590335 A CN110590335 A CN 110590335A CN 201910820399 A CN201910820399 A CN 201910820399A CN 110590335 A CN110590335 A CN 110590335A
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powder
hours
smnbo
materials
absolute ethyl
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周焕福
周贤杰
陈秀丽
张海林
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Guilin University of Technology
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Guilin University of Technology
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/6261—Milling
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B35/64—Burning or sintering processes
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3251—Niobium oxides, niobates, tantalum oxides, tantalates, or oxide-forming salts thereof
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    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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    • C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/661—Multi-step sintering

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Abstract

The invention discloses a Ba2SmNbO6A method for preparing microwave dielectric material. BaCO with purity more than or equal to 99 percent3、Sm2O3And Nb2O5As the main raw material, according to Ba2SmNbO6Proportioning, then carrying out wet ball milling and mixing on the materials for 4 hours, drying the materials by taking absolute ethyl alcohol as a ball milling medium, and presintering the materials for 4 hours at 1200 ℃ in an air atmosphere; carrying out secondary ball milling on the pre-sintered powder, adding 5 wt% of polyvinyl alcohol for granulation, and carrying out compression molding after granulation to obtain Ba2SmNbO6The sintering temperature of the microwave dielectric ceramic prepared by the invention is 1425 ~ 1525 ℃, the dielectric constant is moderate (29.3 ~ 34.9.9),Q×fhigh value (19286 ~ 34882 GHz), temperature coefficient of resonance frequency (τ f ) The size of the composite material is small,the method can be used for manufacturing microwave devices such as resonators, antennas, filters and the like.

Description

Ba2SmNbO6Preparation method of microwave dielectric material
Technical Field
The invention belongs to the field of electronic ceramics and manufacture thereof, and relates to Ba of microwave components such as dielectric substrates, antennas, resonators and the like used at microwave frequency2SmNbO6A method for preparing microwave dielectric material.
Background
The microwave dielectric material is ceramic which is used as a medium in a microwave frequency band (300 MHz ~ 300 GHz) circuit and can perform one or more functions, and is mainly used for preparing resonators, filters, dielectric antennas and dielectric conductorsA wave circuit, and the like. In recent years, with the development of low cost, miniaturization and light weight of microwave components, microwave dielectric materials having excellent microwave dielectric properties (high dielectric properties) are requiredQ×fOf moderate value, dielectric constant, near zeroτ f The value) and the low density, which put higher demands on microwave components and dielectric substrates based on microwave dielectric ceramics, however, at present, serial microwave dielectric ceramics are developed successively, however, the microwave dielectric ceramics with the medium dielectric constant of 25 ~ 35 is less, and microwave components such as resonators and filters have strong demands on the microwave dielectric ceramics with the dielectric constant in the range.
Many excellent dielectric constant microwave dielectric materials are reported, such as: BaZn0.33Ta0.67O3(BZT)，Ba(Y1/2Ta1/2)O3(BYT). However, the disadvantages of expensive raw materials and scarce resources have led to great interest in finding alternative materials. And niobium-based microwave dielectric materials, e.g. BaZn0.33Nb0.67O3, Ba(Zn/Co)0.33Nb0.67O3The performance is excellent, and the dielectric performance is second to BZT and BYT. And because the main component niobium is rich in raw materials and low in price. Therefore, the technical problem to be solved by the invention is to provide a preparation method of a microwave dielectric ceramic material with a medium dielectric constant.
Disclosure of Invention
The purpose of the invention is to provide a Ba2SmNbO6A method for preparing microwave dielectric material.
The method comprises the following specific steps:
BaCO with purity more than or equal to 99 percent3、Sm2O3And Nb2O5As the main raw material, according to Ba2SmNbO6Mixing materials, mixing materials to obtain mixed powder, adding anhydrous ethanol into the mixed powder according to the mass ratio of the anhydrous ethanol to the mixed powder of 1:1, wet-milling for 4 hours, grinding, drying at 120 ~ 130 deg.C, sieving with 80 mesh sieve, pressing into block raw materials,heating the pressed blocky raw material from room temperature to 1200 ℃ at the heating rate of 5 ℃/min, preserving heat for 4 hours at the temperature to prepare a burning block, crushing the burning block into powder, adding absolute ethyl alcohol into the powder according to the mass ratio of the absolute ethyl alcohol to the powder of 1:1, putting the powder into a nylon tank, ball-milling the powder for 4 hours, taking the powder out, putting the powder into a drying furnace, drying the powder at 120 ~ 130 ℃, adding 5 wt% of polyvinyl alcohol into the obtained powder for granulation, pressing the powder into a small cylinder with the diameter of 12mm and the thickness of 6mm, discharging glue at 500 ~ 600 ℃ for 4 hours, cooling the small cylinder with the temperature of 500 ℃ and 600 ℃ to obtain a porcelain, sintering the porcelain at 1425 ~ 1525 ℃ for 4 hours to obtain Ba2SmNbO6Microwave dielectric material.
The method is simple to operate, and the prepared microwave dielectric material has excellent microwave performance: dielectric constant of (ε r ) The temperature of the mixture is moderate,Q×fvalue high and τ f The product has small value, and can be used for manufacturing microwave devices such as resonators, antennas, filters, etc.
Detailed Description
Example 1:
BaCO with purity =99%3、Sm2O3And Nb2O5As the main raw material, according to Ba2SmNbO6Preparing materials, and then mixing the materials to obtain mixed powder; adding absolute ethyl alcohol into mixed powder according to the mass ratio of the absolute ethyl alcohol to the mixed powder of 1:1, mixing for 4 hours by a wet grinding method, drying at 125 ℃ after grinding, sieving by a 80-mesh sieve, pressing into a block raw material, heating the pressed block raw material from room temperature to 1200 ℃ at the temperature at the heating rate of 5 ℃/min, preserving the heat for 4 hours to prepare a fired block, crushing the fired block into powder, adding the absolute ethyl alcohol into the powder according to the mass ratio of the absolute ethyl alcohol to the powder of 1:1, placing the powder into a nylon tank, ball-milling for 4 hours, taking out, placing the powder into a drying furnace, drying at 125 ℃, adding 5 wt% of polyvinyl alcohol into the obtained powder for granulation, pressing into small ceramic columns with the diameter of 12mm and the thickness of 6mm after granulation, discharging glue for 4 hours at 550 ℃, obtaining a material after furnace cooling, sintering the ceramic material for 4 hours at 1425 ℃, thus obtaining Ba2SmNbO6Microwave dielectric material.
Example 2:
the final sintering temperature was changed to 1450 ℃ and the other steps were the same as in example 1.
Example 3:
the final sintering temperature was changed to 1475 ℃ and the other steps were the same as in example 1.
Example 4:
the final sintering temperature was changed to 1500 ℃, and the other steps were the same as in example 1.
Example 5:
the final sintering temperature was changed to 1525 ℃ and the other steps were the same as in example 1.
Table 1 lists Ba obtained in example 1 ~ 52SmNbO6The microwave dielectric property of the microwave dielectric material. The dielectric properties of the microwaves were evaluated by the cylindrical dielectric resonator method.
The ceramic can be widely used for manufacturing microwave electronic components such as various dielectric substrates, antennas, filters and the like, and meets the technical requirements of modern mobile communication systems.
TABLE 1 Ba2SmNbO6Microwave dielectric property of microwave dielectric material
。

Claims (1)

1. Ba2SmNbO6The preparation method of the microwave dielectric material is characterized by comprising the following specific steps:
BaCO with purity more than or equal to 99 percent3、Sm2O3And Nb2O5As the main raw material, according to Ba2SmNbO6Preparing materials, mixing materials to obtain mixed powder, adding absolute ethyl alcohol into the mixed powder according to the mass ratio of the absolute ethyl alcohol to the mixed powder of 1:1, mixing for 4 hours by a wet grinding method, drying at 120 ~ 130 ℃, sieving by a 80-mesh sieve, pressing into block raw materials after sieving, heating the pressed block raw materials from room temperature to 1200 ℃ at the heating rate of 5 ℃/min, preserving the heat at the temperature for 4 hours to prepare a clinker, crushing the clinker into powder, and mixing according to the mass ratio of the absolute ethyl alcohol to the mixed powder of 1:1Adding absolute ethyl alcohol into powder according to the mass ratio of 1:1, placing the powder into a nylon tank, ball-milling the powder for 4 hours, taking the powder out, placing the powder into a drying furnace, drying the powder at 120 ~ 130 ℃ to 130 ℃, adding 5 wt% of polyvinyl alcohol into the obtained powder, granulating the powder, pressing the powder into a small cylinder with the diameter of 12mm and the thickness of 6mm, discharging glue at 500 ~ 600 ℃ for 4 hours, cooling the powder along with the furnace to obtain porcelain, and sintering the porcelain at 1425 ~ 1525 ℃ for 4 hours to obtain Ba2SmNbO6Microwave dielectric material.
CN201910820399.0A 2019-09-01 2019-09-01 Ba2SmNbO6Preparation method of microwave dielectric material Pending CN110590335A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101182205A (en) * 2007-11-16 2008-05-21 北京交通大学 Yttrium niobate solid-phase reaction synthetic sintering method capable of being used for microwave dielectric ceramic
US20120264615A1 (en) * 2011-04-15 2012-10-18 Amit Goyal Chemical solution seed layer for rabits tapes
US20120264612A1 (en) * 2011-04-15 2012-10-18 Amit Goyal Buffer layers for rebco films for use in superconducting devices
CN108395215A (en) * 2018-03-05 2018-08-14 北京理工大学 A kind of tetragonal phase double-perovskite Ba2-xSrxSmTaO6The preparation method of ceramic material
CN108690612A (en) * 2018-06-29 2018-10-23 陕西科技大学 It is a kind of to adulterate orange red fluorescent powder and preparation method thereof by the europium of matrix of niobates

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101182205A (en) * 2007-11-16 2008-05-21 北京交通大学 Yttrium niobate solid-phase reaction synthetic sintering method capable of being used for microwave dielectric ceramic
US20120264615A1 (en) * 2011-04-15 2012-10-18 Amit Goyal Chemical solution seed layer for rabits tapes
US20120264612A1 (en) * 2011-04-15 2012-10-18 Amit Goyal Buffer layers for rebco films for use in superconducting devices
CN108395215A (en) * 2018-03-05 2018-08-14 北京理工大学 A kind of tetragonal phase double-perovskite Ba2-xSrxSmTaO6The preparation method of ceramic material
CN108690612A (en) * 2018-06-29 2018-10-23 陕西科技大学 It is a kind of to adulterate orange red fluorescent powder and preparation method thereof by the europium of matrix of niobates

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
FU W.T.等: "New insight into the symmetry and the structure of the double perovskites Ba2LnNbO6 (Ln=lanthanides and Y)", 《JOURNAL OF SOLID STATE CHEMISTRY》 *
HENMI, K等: "Crystal structures and magnetic properties of ordered perovskites Ba(2)LnNbO(6) (Ln = lanthanide elements)", 《JOURNAL OF SOLID STATE CHEMISTRY 》 *
PASCHOAL, C. W. A.;: "Computer modeling of Ba2RE3+NbO6 (RE3+ = rare-earth and Y) compounds", 《JOURNAL OF PHYSICS-CONDENSED MATTER》 *
SAINES, PAUL J.等: "Structural phase transitions and crystal chemistry of the series Ba(2)LnB " O-6 (Ln = lanthanide and B " = Nb5+ or Sb5+)", 《JOURNAL OF SOLID STATE CHEMISTRY 》 *

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