CN108467267A - A kind of three layers of composite dielectric materials of temperature-stable - Google Patents

A kind of three layers of composite dielectric materials of temperature-stable Download PDF

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Publication number
CN108467267A
CN108467267A CN201810246513.9A CN201810246513A CN108467267A CN 108467267 A CN108467267 A CN 108467267A CN 201810246513 A CN201810246513 A CN 201810246513A CN 108467267 A CN108467267 A CN 108467267A
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temperature
layers
dielectric materials
stable
composite dielectric
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李玲霞
郭千瑜
孙正
郑浩然
罗伟嘉
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Tianjin University
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Tianjin University
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    • 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
    • C04B35/495—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 vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
    • 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
    • C04B35/64—Burning or sintering processes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/002—Details
    • H01G4/018—Dielectrics
    • H01G4/06—Solid dielectrics
    • H01G4/08—Inorganic dielectrics
    • H01G4/12—Ceramic dielectrics
    • H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
    • H01G4/1254—Ceramic dielectrics characterised by the ceramic dielectric material based on niobium or tungsteen, tantalum oxides or niobates, tantalates
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/30—Stacked capacitors
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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
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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    • 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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3213—Strontium oxides or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3298—Bismuth oxides, bismuthates or oxide forming salts thereof, e.g. zinc bismuthate

Abstract

The present invention, which discloses, carrys out a kind of three layers of composite dielectric materials of temperature-stable, and the chemical formula of every layer of composite dielectric materials is respectively Bi2Mg2/3Nb4/3O7、Bi2Mg8/15Sr2/15Nb4/3O7、Bi2Mg4/ 15Sr2/5Nb4/3O7, first by raw material Bi2O3、Nb2O5、SrCO3, MgO weigh dispensing respectively by chemical formula, through ball milling, drying, sieving, calcined at 740~760 DEG C, synthesize principal crystalline phase；The polyvinyl alcohol that additional mass percent is 0.75% again, again after ball milling, drying, sieving, three kinds of powders of phase homogenous quantities are weighed respectively, and pressure forming is three layers of composite body in a manner of lamination, three layers of composite dielectric materials of temperature-stable are made in 940~960 DEG C of sintering in green body.The sintering temperature of the present invention is 950 DEG C, dielectric constant 200, and temperature coefficient of capacitance TCC is 29 × 10‑6/ DEG C, it can be used for the preparation of multiple-layer sheet ceramic capacitor (MLCC), reduce the production cost of multilayer device.

Description

A kind of three layers of composite dielectric materials of temperature-stable
Technical field
The ceramic composition that the invention belongs to a kind of characterized by ingredient, more particularly to a kind of three layers of temperature-stable are compound The preparation method of dielectric material.
Background technology
As the continuous development of modern communication technology, especially mobile communication and satellite communication are towards highly reliable and small size Direction is developed, and to Dielectric Materials at Radio Frequencies, more stringent requirements are proposed.Dielectric Materials at Radio Frequencies be used as in modern communications resonator, Filter, dielectric substrate, diectric antenna, medium wave circuit etc..The performance requirement of media ceramic is:(l) material is with respect to dielectric Constant should be big, in order to device miniaturization；(2) dielectric loss answers temperature coefficient of permittivity of the very little (3) close to zero.More In layer electronic market ceramic capacitor (MLCC), NP0 capacitors have the multi-layer ceramic capacitance (MLCC) of temperature compensation characteristic, Dielectric constant and dielectric loss are most stable.Using the NP0 characteristic ceramic materials of MLCC technologies with small, specific volume is big, moisture resistance Wet, long-life, chip type, many advantages, such as parasitic inductance is low, high frequency characteristics is good, circuit integration, micromation, Gao Ke can be met By the requirement of property and low cost, it has also become most adapt to one of the element of electronic technology rapid development.
Bi-based pyrochlor dielectric material has higher dielectric qualities, causes more next as a kind of emerging ceramic material More scholars study, and are applied in high-frequency element.There are two according to ceramic chemical formula difference for Bi-based pyrochlor system Kind structure, wherein (Bi1.5Zn0.5)(Zn0.5Nb1.5)O7(α-BZN) cubic pyrochlore (εr≈150,tanδ≤4×10-4,TCC ≈-400×10-6/ DEG C), have dielectric constant high, dielectric loss is relatively low, the adjustable characteristic of temperature coefficient of permittivity.To meet The temperature coefficient of capacitance of practical application, regulation system meets ± 30 × 10-6/ DEG C, severe application environment is adapted to, researcher is become The direction of effort.
Invention content
The purpose of the present invention is to overcome the shortcomings that dielectric loss improves after the carry out ion doping of the prior art, providing A kind of preparation method of three layers of composite dielectric materials of temperature-stable.
The present invention is achieved by following technical solution.
A kind of three layers of composite dielectric materials of temperature-stable, the chemical formula of every layer of composite dielectric materials are respectively Bi2Mg2/3Nb4/3O7、Bi2Mg8/15Sr2/15Nb4/3O7、Bi2Mg4/15Sr2/5Nb4/3O7。
The preparation method of three layers of composite dielectric materials of temperature-stable has following steps：
(1) by raw material Bi2O3、Nb2O5、SrCO3, MgO press Bi2Mg2/3Nb4/3O7、Bi2Mg8/15Sr2/15Nb4/3O7、 Bi2Mg4/15Sr2/5Nb4/3O7Chemical formula weighs dispensing respectively；
(2) powder that step (1) is prepared is respectively put into three ball grinders, zirconia ball and deionized water, ball is added Mill 4 hours；Raw material after ball milling is placed in infrared drying oven and is dried, 40 mesh sieve is crossed after drying, obtains evengranular powder；
(3) by step (2), treated that powder is calcined 4 hours at 740~760 DEG C, synthesizes principal crystalline phase；
(4) polyvinyl alcohol that additional mass percent is 0.75% in the powder that step (3) synthesizes principal crystalline phase, is put into ball In grinding jar, zirconia ball and deionized water is added, ball milling 12 hours crosses 80 mesh sieve, weighs the three of phase homogenous quantities respectively after drying Kind powder, three layers of composite body are pressed into a manner of lamination with powder compressing machine with the pressure of 4MPa；
(5) step (4) green body after molding is kept the temperature 4 hours, three layers of temperature-stable is made in 940~960 DEG C of sintering Composite dielectric materials.
The raw material of the step (2) or (4) is 1: 1: 2 with zirconia ball and the mass ratio of deionized water.
The calcination temperature of the step (3) is 750 DEG C.
The sintering temperature of the step (5) is 950 DEG C.
The present invention provides a kind of three layers of composite dielectric materials of temperature-stable and preparation method thereof, the composite dielectric materials Sintering temperature be 950 DEG C, dielectric constant 200, temperature coefficient of capacitance TCC be 29 × 10-6/ DEG C, it can be used for multilayer sheet type The preparation of ceramic capacitor (MLCC) greatly reduces the production cost of multilayer device since it is with lower sintering temperature.
Description of the drawings
Fig. 1 is the structural schematic diagram of three layers of composite dielectric materials of temperature-stable of the present invention.
Specific implementation mode
Below by specific embodiment, the invention will be further described, and raw materials used in embodiment is that commercially available analysis is pure Reagent, specific embodiment are as follows.
Embodiment 1
(1) by raw material Bi2O3、Nb2O5、SrCO3, MgO press Bi2Mg2/3Nb4/3O7、Bi2Mg8/15Sr2/15Nb4/3O7、 Bi2Mg4/15Sr2/5Nb4/3O7Chemical formula weighs dispensing；
(2) powder by above-mentioned preparation is put into ball grinder, and zirconia ball and deionized water, ball milling 4 hours, powder is added Mass ratio with zirconia ball, deionized water is 1: 1: 2；Raw material after ball milling is placed in infrared drying oven at 100 DEG C and is dried It is dry, 40 mesh sieve is crossed after drying, obtains evengranular powder；
(3) above-mentioned uniformly mixed powder is calcined 4 hours at 750 DEG C, synthesizes principal crystalline phase；
(4) polyvinyl alcohol that additional mass percent is 0.75% in powder after firing, is put into ball grinder, is added The mass ratio of zirconia ball and deionized water, powder and zirconia ball, deionized water is 1: 1: 2, ball milling 12 hours, mistake after drying 80 mesh sieve, then weigh 0.2g raw materials respectively, then are pressed into the green body of Φ 10mm × 1mm with the pressure of 4MPa with powder compressing machine；
(5) above-mentioned green body after molding is kept the temperature 4 hours, three layers of complex media of temperature-stable is made in 950 DEG C of sintering Material；
(6) its dielectric properties is tested using Agilent 4278A impedance analyzers, under 1MHz, measures εr=200, tan δ =23, TCC=29 × 10-6/℃。
Fig. 1 is the structural schematic diagram of three layers of composite dielectric materials of temperature-stable of the present invention, be can see in right figure, by upper To lower respectively Bi2Mg2/3Nb4/3O7Layer 1, Bi2Mg8/15Sr2/15Nb4/3O73 and Bi of layer2Mg4/15Sr2/5Nb4/3O7Layer 3.

Claims (4)

1. a kind of three layers of composite dielectric materials of temperature-stable, the chemical formula of every layer of composite dielectric materials is respectively Bi2Mg2/ 3Nb4/3O7、Bi2Mg8/15Sr2/15Nb4/3O7、Bi2Mg4/15Sr2/5Nb4/3O7。
The preparation method of three layers of composite dielectric materials of temperature-stable has following steps：
(1) by raw material Bi2O3、Nb2O5、SrCO3, MgO press Bi2Mg2/3Nb4/3O7、Bi2Mg8/15Sr2/15Nb4/3O7、Bi2Mg4/15Sr2/ 5Nb4/3O7Chemical formula weighs dispensing respectively；
(2) powder that step (1) is prepared is respectively put into three ball grinders, zirconia ball is added and deionized water, ball milling 4 are small When；Raw material after ball milling is placed in infrared drying oven and is dried, 40 mesh sieve is crossed after drying, obtains evengranular powder；
(3) by step (2), treated that powder is calcined 4 hours at 740~760 DEG C, synthesizes principal crystalline phase；
(4) polyvinyl alcohol that additional mass percent is 0.75% in the powder that step (3) synthesizes principal crystalline phase, is put into ball grinder In, zirconia ball and deionized water is added, ball milling 12 hours crosses 80 mesh sieve, weighs three kinds of powder of phase homogenous quantities respectively after drying Material, three layers of composite body are pressed into a manner of lamination with powder compressing machine with the pressure of 4MPa；
(5) step (4) green body after molding is kept the temperature 4 hours, it is compound that three layers of temperature-stable is made in 940~960 DEG C of sintering Dielectric material.
2. three layers of composite dielectric materials of a kind of temperature-stable according to claim 1, which is characterized in that the step (2) or the raw material of (4) and zirconia ball and the mass ratio of deionized water are 1: 1: 2.
3. three layers of composite dielectric materials of a kind of temperature-stable according to claim 1, which is characterized in that the step (3) calcination temperature is 750 DEG C.
4. three layers of composite dielectric materials of a kind of temperature-stable according to claim 1, which is characterized in that the step (5) sintering temperature is 950 DEG C.
CN201810246513.9A 2018-03-23 2018-03-23 A kind of three layers of composite dielectric materials of temperature-stable Pending CN108467267A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109231983A (en) * 2018-10-18 2019-01-18 天津大学 A kind of preparation method of the barium zirconate titanate-based ceramics of bilayer
CN111499382A (en) * 2020-04-28 2020-08-07 天津大学 High-temperature-stability double-layer energy storage ceramic and preparation method thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050234154A1 (en) * 2004-04-18 2005-10-20 Polyram Ram-On Industries Star-like polyolefin having high propylene content and polar derivatives thereof and method for its production
CN101863154A (en) * 2010-06-17 2010-10-20 天津大学 Multilayer gradient Ba1-xSrxTiO3 (BST) dielectric ceramic material and preparation method
CN103232242A (en) * 2013-04-22 2013-08-07 江苏大学 BMN (bismuth magnesium niobate)-based microwave dielectric ceramic material and preparation method thereof
CN103601495A (en) * 2013-11-14 2014-02-26 天津大学 NP0 low-temperature sintered ceramic capacitor dielectric material and preparation method thereof
CN104029432A (en) * 2014-06-26 2014-09-10 天津大学 Preparation method of BST(barium strontium titanate)/BMN (bismuth magnesium niobate)/BST multilayer composite film
CN107459351A (en) * 2017-08-31 2017-12-12 天津大学 A kind of temperature-stable Dielectric Materials at Radio Frequencies

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050234154A1 (en) * 2004-04-18 2005-10-20 Polyram Ram-On Industries Star-like polyolefin having high propylene content and polar derivatives thereof and method for its production
CN101863154A (en) * 2010-06-17 2010-10-20 天津大学 Multilayer gradient Ba1-xSrxTiO3 (BST) dielectric ceramic material and preparation method
CN103232242A (en) * 2013-04-22 2013-08-07 江苏大学 BMN (bismuth magnesium niobate)-based microwave dielectric ceramic material and preparation method thereof
CN103601495A (en) * 2013-11-14 2014-02-26 天津大学 NP0 low-temperature sintered ceramic capacitor dielectric material and preparation method thereof
CN104029432A (en) * 2014-06-26 2014-09-10 天津大学 Preparation method of BST(barium strontium titanate)/BMN (bismuth magnesium niobate)/BST multilayer composite film
CN107459351A (en) * 2017-08-31 2017-12-12 天津大学 A kind of temperature-stable Dielectric Materials at Radio Frequencies

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109231983A (en) * 2018-10-18 2019-01-18 天津大学 A kind of preparation method of the barium zirconate titanate-based ceramics of bilayer
CN111499382A (en) * 2020-04-28 2020-08-07 天津大学 High-temperature-stability double-layer energy storage ceramic and preparation method thereof

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