CN107500753A - A kind of low-loss titanium barium stannate dielectric material - Google Patents

A kind of low-loss titanium barium stannate dielectric material Download PDF

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Publication number
CN107500753A
CN107500753A CN201710794193.6A CN201710794193A CN107500753A CN 107500753 A CN107500753 A CN 107500753A CN 201710794193 A CN201710794193 A CN 201710794193A CN 107500753 A CN107500753 A CN 107500753A
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dielectric material
low
loss
barium stannate
powder
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李玲霞
孙正
于仕辉
杜明昆
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Tianjin University
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Tianjin University
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B35/46—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 based on titanium oxides or titanates
    • C04B35/462—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 based on titanium oxides or titanates based on titanates
    • C04B35/465—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 based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
    • C04B35/468—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 based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B35/62615—High energy or reactive ball milling
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/442—Carbonates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Abstract

The invention discloses a kind of low-loss titanium barium stannate dielectric material, its chemical formula is：Ba(SnxTi1‑x)O3(0.01≤x≤0.3)；First by BaCO3、TiO2、SnO2Stoichiometrically formula carries out dispensing, is mixed through ball milling, drying, sieving after 1050~1200 DEG C of pre-burnings, then additional 0.5wt%PVA, compressing after ball milling, drying, sieving is base substrate；Base substrate is made with low-loss titanium barium stannate dielectric material in 1275 DEG C~1400 DEG C sintering.The permittivity ε of the present inventionrFor 5000~11560, dielectric loss is 0.003~0.008.

Description

A kind of low-loss titanium barium stannate dielectric material
Technical field
The invention belongs to electronic information material and component field, more particularly to a kind of low-loss titanium barium stannate dielectric material Preparation method
Background technology
As electronics are gradually to miniaturization, information-based and high-intelligentization direction development, electronic component is also carried The requirement of lightness, slimming and subminaturization is gone out.Phased-array radar is a kind of very important electronic equipment, wherein, iron Electric phase shifter is wherein to apply more a kind of component, as phased-array radar progressively develops to miniaturization, low-loss direction, The room temperature dielectric constant of ferroelectric phase shifter dielectric material is improved, reducing dielectric loss and temperature coefficient turns into numerous researchers' Research direction.
BaTiO3Ceramics are a kind of typical ferroelectric materials, and its dielectric constant at room temperature is about 1600, to Curie's temperature 10000 are up to when spending (120 DEG C).But BaTiO3As ferroelectric phase shifter dielectric material, its dielectric loss and temperature coefficient are all It is larger, limit it and further apply.In order to reduce BaTiO3Temperature coefficient, it can be carried out using rare earth element composite mixed Modified method, its Curie peak is set to move to left and broadening, but this kind of method can reduce the dielectric constant of material, and rare earth element Cost is also higher.And use Sn4+The BaTiO of doping3Ba (the Sn formedxTi1-x)O3Solid-solution material, it on the one hand can make its residence In peak be moved to the left (room temperature direction), while improve its dielectric constant, while improve its temperature coefficient stability and reduce damage Consumption；On the other hand BaTiO can also be strengthened3Nonlinear characteristic, be so just easy to its dielectric constant by external electric field Size, so that it has one in dielectric amplifier, frequency multiplier, pulse oscillator, phase shifter and other automatic controls and telecontrol engineering Fixed application prospect.In addition, the BaTiO for mixing Sn3Material, grain-boundary layer capacitor material is also used as after doped semiconducting.
The content of the invention
The purpose of the present invention, it is to overcome in the prior art using the higher rare earth ion of different kinds of ions doping and cost Adulterate BaTiO3Shortcoming and defect caused by dielectric material, there is provided a kind of low-loss titanium barium stannate dielectric material and its preparation side Method, it is increasingly miniaturized with adapting to ferroelectric phase shifter, the needs that low-loss direction is developed, mainly with BaCO3、TiO2、SnO2For original Material, a kind of low-loss titanium barium stannate dielectric material is prepared by solid phase method.
The present invention is achieved by following technical solution.
A kind of low-loss titanium barium stannate dielectric material, its chemical formula are：Ba(SnxTi1-x)O3, wherein 0.01≤x≤0.3；
The preparation method of the low-loss titanium barium stannate dielectric material, specific implementation step are as follows：
(1) by BaCO3、TiO2、SnO2Stoichiometrically formula Ba (SnxTi1-x)O3, wherein 0.01≤x≤0.3 carries out dispensing, After adding deionized water and zirconium ball, ball milling 2-8 hours；
(2) powder after step (1) ball milling is placed in drying box, in 100~120 DEG C of drying, then crosses 40 mesh sieves；
(3) will dry, the powder after sieving is put into moderate oven, in 1050~1200 DEG C of pre-burnings, be incubated 2~6 hours；
(4) additional 0.5wt%PVA in the powder after step (3) pre-burning is mixed, be put into ball grinder, add oxygen Change zirconium ball and deionized water, ball milling 10~15 hours, sieved after drying, then base substrate is pressed into powder compressing machine；
(5) base substrate of step (4) is incubated 2~8 hours, be made with low-loss in 1275 DEG C~1400 DEG C sintering Titanium barium stannate dielectric material.
Step (1) stoichiometric equation Ba (SnxTi1-x)O3X values be 0.15.
Step (1) powder carries out ball milling using planetary ball mill, and drum's speed of rotation is 400 revs/min.
The blank diameter of the step (4) is 10mm, thickness 1mm.
The pressure of step (4) powder compressing machine is 2~6MPa.
The sintering temperature of the step (5) is 1350 DEG C.
The present invention is prepared for a kind of low-loss Ba (Sn by solid phase methodxTi1-x)O3(0.01≤x≤0.3) dielectric material, its Permittivity εrFor 5000~11560, dielectric loss is 0.003~0.008.
Embodiment
The present invention is with BaCO3(analysis is pure), TiO2(analysis is pure), SnO2(analysis is pure) is initial feed, passes through simple solid phase Method prepares ceramic capacitor dielectric material.Specific embodiment is as follows：
Embodiment 1
1. by BaCO3、TiO2、SnO2Stoichiometrically formula Ba (Sn0.15Ti0.85)O3Dispensing is carried out, matches and is：8.172g BaCO3、2.8122g TiO2、0.9287gSnO2, 10g mixed powder is put into nylon tank, adds 200ml deionized waters, 150g zirconium balls, ball milling 6 hours on planetary ball mill are added, rotating speed is 400 revs/min.
2. the powder after ball milling is placed in drying box, in 100 DEG C of drying, 40 mesh sieves are crossed afterwards；
3. the powder moderate oven after sieving will be dried, in 1100 DEG C of pre-burnings, 4 hours are incubated.
4. the powder after step 3 pre-burning is mixed with 0.5wt%PVA, be put into ball grinder, add zirconia ball and Deionized water, ball milling 12 hours, sieves after drying, then is pressed into base substrate with powder compressing machine with 4MPa pressure；
5. base substrate is incubated 4 hours, low-loss Ba (Sn are made in 1350 DEG C of sintering0.15Ti0.85)O3Dielectric material.
Embodiment 2~10
For embodiment 2~10 in addition to x values, calcined temperature, sintering temperature, other preparation technologies are entirely identical to embodiment 1.
The specific embodiment of the invention tests institute at 1 khz by HEWLETT PACKARD 4278A (Agilent 4278A) Obtain the dielectric properties of product.
The related process parameters and its dielectric properties of specific embodiment are as shown in table 1.
Table 1

Claims (6)

1. a kind of low-loss titanium barium stannate dielectric material, its chemical formula are：Ba(SnxTi1-x)O3, wherein 0.01≤x≤0.3.
The preparation method of the low-loss titanium barium stannate dielectric material, specific implementation step are as follows：
(1) by BaCO3、TiO2、SnO2Stoichiometrically formula Ba (SnxTi1-x)O3, wherein 0.01≤x≤0.3 carries out dispensing, add After deionized water and zirconium ball, ball milling 2-8 hours；
(2) powder after step (1) ball milling is placed in drying box, in 100~120 DEG C of drying, then crosses 40 mesh sieves；
(3) will dry, the powder after sieving is put into moderate oven, in 1050~1200 DEG C of pre-burnings, be incubated 2~6 hours；
(4) additional 0.5wt%PVA in the powder after step (3) pre-burning is mixed, be put into ball grinder, add zirconium oxide Ball and deionized water, ball milling 10~15 hours, sieve, then be pressed into base substrate with powder compressing machine after drying；
(5) base substrate of step (4) is incubated 2~8 hours, be made with low-loss titanium tin in 1275 DEG C~1400 DEG C sintering Sour barium dielectric material.
2. a kind of low-loss titanium barium stannate dielectric material according to claim 1, it is characterised in that the step (1) is changed Learn metering-type Ba (SnxTi1-x)O3X values be 0.15.
A kind of 3. low-loss titanium barium stannate dielectric material according to claim 1, it is characterised in that step (1) powder Material carries out ball milling using planetary ball mill, and drum's speed of rotation is 400 revs/min.
4. a kind of low-loss titanium barium stannate dielectric material according to claim 1, it is characterised in that the step (4) Blank diameter is 10mm, thickness 1mm.
A kind of 5. low-loss titanium barium stannate dielectric material according to claim 1, it is characterised in that step (4) powder The pressure of last tablet press machine is 2~6MPa.
6. a kind of low-loss titanium barium stannate dielectric material according to claim 1, it is characterised in that the step (5) Sintering temperature is 1350 DEG C.
CN201710794193.6A 2017-09-06 2017-09-06 A kind of low-loss titanium barium stannate dielectric material Pending CN107500753A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108689703A (en) * 2018-06-26 2018-10-23 桂林电子科技大学 A kind of Lead-free ferroelectric ceramics material and preparation method thereof for adjusting characteristic with huge dielectric constant and electricity
CN109133913A (en) * 2018-07-27 2019-01-04 广东工业大学 A kind of high dielectric constant tin calcium acid barium titanium and its preparation method and application
CN110655402A (en) * 2019-10-14 2020-01-07 天津大学 Medium-temperature sintered rutile-like microwave dielectric ceramic material
CN113860867A (en) * 2021-10-11 2021-12-31 天津大学 Barium titanate-based dielectric ceramic material with high tuning rate and preparation method thereof
CN114478007A (en) * 2022-02-17 2022-05-13 同济大学 Sodium niobate-based ceramic material with good process tolerance, high piezoelectric property and high dielectric property, and preparation method and application thereof

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CN102093044A (en) * 2011-01-13 2011-06-15 天津大学 Low-loss microwave dielectric ceramic and preparation method thereof
CN103073281A (en) * 2013-01-31 2013-05-01 天津大学 Lithium-zinc-titanium-tin series microwave dielectric ceramics material and preparation method thereof
CN104961460A (en) * 2015-07-01 2015-10-07 西北工业大学 Tin barium titanate ceramic and preparation method thereof
CN106495687A (en) * 2016-10-27 2017-03-15 西安交通大学 A kind of existing fringing field, dielectric ceramic of high-energy-density and preparation method thereof
CN106957173A (en) * 2017-03-30 2017-07-18 广东工业大学 A kind of tin barium titanate thick film ceramic and its application

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102093044A (en) * 2011-01-13 2011-06-15 天津大学 Low-loss microwave dielectric ceramic and preparation method thereof
CN103073281A (en) * 2013-01-31 2013-05-01 天津大学 Lithium-zinc-titanium-tin series microwave dielectric ceramics material and preparation method thereof
CN104961460A (en) * 2015-07-01 2015-10-07 西北工业大学 Tin barium titanate ceramic and preparation method thereof
CN106495687A (en) * 2016-10-27 2017-03-15 西安交通大学 A kind of existing fringing field, dielectric ceramic of high-energy-density and preparation method thereof
CN106957173A (en) * 2017-03-30 2017-07-18 广东工业大学 A kind of tin barium titanate thick film ceramic and its application

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108689703A (en) * 2018-06-26 2018-10-23 桂林电子科技大学 A kind of Lead-free ferroelectric ceramics material and preparation method thereof for adjusting characteristic with huge dielectric constant and electricity
CN108689703B (en) * 2018-06-26 2021-01-05 桂林电子科技大学 Lead-free ferroelectric ceramic material with giant dielectric constant and electric tuning characteristics and preparation method thereof
CN109133913A (en) * 2018-07-27 2019-01-04 广东工业大学 A kind of high dielectric constant tin calcium acid barium titanium and its preparation method and application
CN109133913B (en) * 2018-07-27 2021-03-26 广东工业大学 High-dielectric-constant barium titanium stannate-calcium acid, and preparation method and application thereof
CN110655402A (en) * 2019-10-14 2020-01-07 天津大学 Medium-temperature sintered rutile-like microwave dielectric ceramic material
CN113860867A (en) * 2021-10-11 2021-12-31 天津大学 Barium titanate-based dielectric ceramic material with high tuning rate and preparation method thereof
CN114478007A (en) * 2022-02-17 2022-05-13 同济大学 Sodium niobate-based ceramic material with good process tolerance, high piezoelectric property and high dielectric property, and preparation method and application thereof

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