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CN118545997B - High-dielectric-property electronic ceramic and preparation method thereof - Google Patents

High-dielectric-property electronic ceramic and preparation method thereof Download PDF

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Publication number
CN118545997B
CN118545997B CN202410998778.XA CN202410998778A CN118545997B CN 118545997 B CN118545997 B CN 118545997B CN 202410998778 A CN202410998778 A CN 202410998778A CN 118545997 B CN118545997 B CN 118545997B
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high dielectric
dielectric ceramic
electronic ceramic
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sintering
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CN118545997A (en
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周淑英
曹建辉
刘平
谭燕飞
陈奕
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Xinxing Electronic Ceramics Co ltd
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Xinxing Electronic Ceramics Co ltd
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Abstract

The invention relates to the field of electronic ceramic materials, in particular to high dielectric property electronic ceramic and a preparation method thereof, wherein the chemical composition of the high dielectric property electronic ceramic comprises :Pb(ZrxTi1‑x)(MgyW1‑y)(SczTa1‑z)O3-αwt%Ba(AlqSb1‑q)O3-βwt%Bi4Ti3O12,x、y、z、q as atomic percent; alpha and beta respectively represent Ba (Al qSb1‑q)O3 and Bi 4Ti3O12 account for the mass percent of the whole electronic ceramic; the electronic ceramic prepared by the invention has good dielectric property and piezoelectric property.

Description

High-dielectric-property electronic ceramic and preparation method thereof
Technical Field
The invention relates to the field of electronic ceramic materials, in particular to high-dielectric-property electronic ceramic and a preparation method thereof.
Background
Conventional electronic ceramic materials are limited in application because of low dielectric constant. In recent years, as piezoelectric electroacoustic devices are being miniaturized and thinned, electronic ceramic materials having higher dielectric constants and lower dielectric losses are required.
Disclosure of Invention
The invention aims to: aiming at the technical problems, the invention provides high-dielectric-property electronic ceramic and a preparation method thereof.
The technical scheme adopted is as follows:
A high dielectric performance electronic ceramic comprising the chemical composition of:
Pb(ZrxTi1-x)(MgyW1-y)(SczTa1-z)O3-αwt%Ba(AlqSb1-q)O3-βwt%Bi4Ti3O12
x, y, z, q is atomic percent;
Alpha and beta respectively represent Ba (Al qSb1-q)O3 and Bi 4Ti3O12 account for the mass percent of the whole electronic ceramic;
x is 0.4-0.6, y is 0.4-0.6, z is 0.4-0.6, q is 0.4-0.6;
Alpha is 5-10, beta is 0.1-1.
Further, x is 0.45-0.55, y is 0.45-0.55, z is 0.45-0.55, and q is 0.45-0.55.
Further, x is 0.48, y is 0.5, z is 0.5, and q is 0.5.
Further, alpha is 6-8 and beta is 0.4-0.8.
Further, α is 6.5 and β is 0.5.
The invention also provides a preparation method of the high dielectric property electronic ceramic, which comprises the following steps:
Mixing Pb3O4、ZrO2、TiO2、MgO、WO3、Sc2O3、Ta2O5、BaCO3、Al2O3、Sb2O3 and Bi 4Ti3O12, ball milling, drying, pre-pressing to prepare a green sheet, pre-sintering, crushing a pre-sintered product, ball milling again, drying, adding a binder into the obtained powder, granulating, pressing to prepare a green body, placing the green body in a sintering furnace, heating to 550-650 ℃ for heat preservation and glue discharging for 1-3 hours, heating to 1150-1300 ℃ for heat preservation and sintering for 2-4 hours.
Further, the presintering temperature is 800-900 ℃, and the presintering time is 1-3h.
Further, the binder is polyvinyl alcohol and/or polyvinyl butyral.
Further, sintering is performed under an oxygen atmosphere.
Further, the first stage heating rate is 0.5-20 ℃/min, and the second stage heating rate is 0.5-20 ℃/min.
The invention has the beneficial effects that:
The invention provides high dielectric property electronic ceramics, PZT is taken as an extremely important piezoelectric ceramics, in order to improve the piezoelectric and dielectric properties of the piezoelectric ceramics, PZT-PMW-PST is widely researched, PZT-series multielement electronic ceramics are positioned near quasi-isomorphic phase boundary (MPB), an electronic ceramic material structure is positioned near quasi-isomorphic phase boundary (MPB), and the coexistence of a trigonal phase and a tetragonal phase is realized, the potential barrier between the trigonal phase and the tetragonal phase is reduced, the macroscopic dielectric and piezoelectric effect of the electronic ceramics are better, ba (Al qSb1-q)O3 is a perovskite structure and can form a good solid solution with PZT-PMW-PST), ions Ba 2+,Cu2+,Sb3+ contained in the PZT-PMW-PST can play a better modifying role, so that various properties of the electronic ceramics are improved, bi 4Ti3O12 is taken as a composite oxide to reduce the sintering temperature, a large amount of liquid phase is generated in the sintering densification in the sintering process, and the sintering in the oxygen atmosphere can obtain the high-performance electronic ceramics.
Drawings
FIG. 1 is an SEM image of the electronic ceramic prepared in example 1.
Detailed Description
The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention. The technology not mentioned in the present invention refers to the prior art, and unless otherwise indicated, the following examples and comparative examples are parallel tests, employing the same processing steps and parameters.
Example 1: a high dielectric performance electronic ceramic comprising the chemical composition of:
Pb(Zr0.48Ti0.52)(Mg0.5W0.5)(Sc0.5Ta0.5)O3-6.5wt%Ba(Al0.5Sb0.5)O3-0.5wt%Bi4Ti3O12
The preparation method of the high dielectric property electronic ceramic comprises the following steps:
Weighing Pb3O4、ZrO2、TiO2、MgO、WO3、Sc2O3、Ta2O5、BaCO3、Al2O3、Sb2O3 and Bi 4Ti3O12 according to chemical composition, mixing, adding into a ball milling tank of a planetary ball mill, ball milling with absolute ethyl alcohol for 10 hours, drying, prepressing under 10MPa to prepare a green sheet, heating the green sheet to 850 ℃ for presintering for 2 hours, crushing the presintered product, adding into the ball milling tank of the planetary ball mill again, ball milling with absolute ethyl alcohol for 5 hours, drying to obtain mixed powder, dissolving binder polyvinyl alcohol in water to obtain 8% polyvinyl alcohol solution, mixing the mixed powder and the polyvinyl alcohol solution for granulation, sieving, pressing under 200MPa to obtain a green body, placing the green body into a sintering furnace under air atmosphere, heating to 600 ℃ for 2 hours at a speed of 1 ℃/min, replacing air in the sintering furnace with high-purity oxygen, heating to 1250 ℃ for 3 hours at a speed of 5 ℃/min, and sintering.
Example 2: a high dielectric performance electronic ceramic comprising the chemical composition of:
Pb(Zr0.48Ti0.52)(Mg0.5W0.5)(Sc0.5Ta0.5)O3-6.5wt%Ba(Al0.5Sb0.5)O3-0.5wt%Bi4Ti3O12
The preparation method of the high dielectric property electronic ceramic comprises the following steps:
Weighing Pb3O4、ZrO2、TiO2、MgO、WO3、Sc2O3、Ta2O5、BaCO3、Al2O3、Sb2O3 and Bi 4Ti3O12 according to chemical composition, mixing, adding into a ball milling tank of a planetary ball mill, ball milling with absolute ethyl alcohol for 10 hours, drying, prepressing under 10MPa to prepare a green sheet, heating the green sheet to 900 ℃ for presintering for 3 hours, crushing the presintered product, adding into the ball milling tank of the planetary ball mill again, ball milling with absolute ethyl alcohol for 5 hours, drying to obtain mixed powder, dissolving binder polyvinyl alcohol in water to obtain a polyvinyl alcohol solution with the mass concentration of 8%, mixing the mixed powder and the polyvinyl alcohol solution for granulation, sieving, pressing under 200MPa to prepare a green body, placing the green body into a sintering furnace under an air atmosphere, heating to 650 ℃ for heat preservation and glue discharging for 2 hours at a speed of 5 ℃/min, replacing air in the sintering furnace with high-purity oxygen, heating to 1300 ℃ for 2 hours at a speed of 10 ℃/min, and then performing heat preservation and sintering.
Example 3: a high dielectric performance electronic ceramic comprising the chemical composition of:
Pb(Zr0.48Ti0.52)(Mg0.5W0.5)(Sc0.5Ta0.5)O3-6.5wt%Ba(Al0.5Sb0.5)O3-0.5wt%Bi4Ti3O12
The preparation method of the high dielectric property electronic ceramic comprises the following steps:
Weighing Pb3O4、ZrO2、TiO2、MgO、WO3、Sc2O3、Ta2O5、BaCO3、Al2O3、Sb2O3 and Bi 4Ti3O12 according to chemical composition, mixing, adding into a ball milling tank of a planetary ball mill, ball milling with absolute ethyl alcohol for 10 hours, drying, prepressing under 10MPa to prepare a green sheet, heating the green sheet to 800 ℃ for presintering for 1 hour, crushing the presintered product, adding into the ball milling tank of the planetary ball mill again, ball milling with absolute ethyl alcohol for 5 hours, drying to obtain mixed powder, dissolving binder polyvinyl alcohol in water to obtain a polyvinyl alcohol solution with the mass concentration of 8%, mixing the mixed powder and the polyvinyl alcohol solution for granulation, sieving, pressing under 200MPa to prepare a green body, placing the green body into a sintering furnace under the air atmosphere, firstly heating to 550 ℃ at a speed of 0.5 ℃/min, preserving heat for 3 hours, replacing air in the sintering furnace with high-purity oxygen, and then heating to 1150 ℃ for 2 hours at a second stage at a speed of 0.5 ℃/min.
Comparative example 1:
substantially the same as in example 1, except that Ba (Al 0.5Sb0.5)O3 was not added.
Comparative example 2:
Substantially the same as in example 1, except that Bi 4Ti3O12 was not added.
Comparative example 3:
substantially the same as in example 1, except that the air in the sintering furnace was not replaced with high-purity oxygen, and sintering was continued while maintaining the air atmosphere.
Performance test:
Polishing the high dielectric electronic ceramics prepared in the embodiments 1-3 and the comparative examples 1-3, brushing silver paste on the upper surface and the lower surface, curing at 600 ℃ for 30min, immersing in silicon oil at 70 ℃ and applying a DC electric field of 3kv/mm for 30min as a sample for performance test;
Measuring the piezoelectric constant of the sample by using a ZJ-3A quasi-static d 33 tester, measuring the relative dielectric constant epsilon r (room temperature 100 kHz), dielectric loss tan delta (room temperature 100 kHz), resonant frequency and antiresonant frequency and corresponding impedance of the sample by using an HP4192 precise impedance analyzer of Agilent company, and calculating the electromechanical coupling coefficient k p of the sample;
the test results are shown in table 1 below:
table 1:
As can be seen from Table 1, the electronic ceramic prepared by the method has good dielectric property and piezoelectric property, and the addition of Ba (Al 0.5Sb0.5)O3、Bi4Ti3O12 and sintering under oxygen atmosphere play a positive role in improving the dielectric property and piezoelectric property of the electronic ceramic.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims (10)

1. A high dielectric electronic ceramic, characterized by a chemical composition comprising:
Pb(ZrxTi1-x)(MgyW1-y)(SczTa1-z)O3-αwt%Ba(AlqSb1-q)O3-βwt%Bi4Ti3O12
x, y, z, q is atomic percent;
Alpha and beta respectively represent Ba (Al qSb1-q)O3 and Bi 4Ti3O12 account for the mass percent of the whole electronic ceramic;
x is 0.4-0.6, y is 0.4-0.6, z is 0.4-0.6, q is 0.4-0.6;
Alpha is 5-10, beta is 0.1-1.
2. The high dielectric ceramic of claim 1 wherein x is 0.45 to 0.55, y is 0.45 to 0.55, z is 0.45 to 0.55, and q is 0.45 to 0.55.
3. The high dielectric ceramic of claim 1 wherein x is 0.48, y is 0.5, z is 0.5, and q is 0.5.
4. The high dielectric ceramic of claim 1 wherein α is from 6 to 8 and β is from 0.4 to 0.8.
5. The high dielectric ceramic of claim 1 wherein α is 6.5 and β is 0.5.
6. A method for preparing the high dielectric ceramic according to any one of claims 1 to 5, wherein Pb3O4、ZrO2、TiO2、MgO、WO3、Sc2O3、Ta2O5、BaCO3、Al2O3、Sb2O3 and Bi 4Ti3O12 are mixed, ball-milled, dried, pre-pressed into green sheets, pre-sintered, crushed, ball-milled again, dried, granulated by adding a binder into the obtained powder, pressed into a green body, and the green body is placed in a sintering furnace, the first stage is heated to 550 to 650 ℃, the temperature is kept for 1 to 3 hours, and the second stage is heated to 1150 to 1300 ℃ and the temperature is kept for sintering for 2 to 4 hours.
7. The method for producing high dielectric ceramic according to claim 6, wherein the burn-in temperature is 800 to 900 ℃ and the burn-in time is 1 to 3 hours.
8. The method of manufacturing high dielectric ceramic according to claim 6, wherein the binder is polyvinyl alcohol and/or polyvinyl butyral.
9. The method for producing high dielectric ceramic according to claim 6, wherein the sintering is performed under an oxygen atmosphere.
10. The method for producing high dielectric ceramic according to claim 6, wherein the first stage is heated at a rate of 0.5 to 20 ℃/min and the second stage is heated at a rate of 0.5 to 20 ℃/min.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1790568A (en) * 2003-12-18 2006-06-21 Tdk株式会社 Dielectric ceramic composition, electronic component, and method for producing the same
CN107311643A (en) * 2017-07-06 2017-11-03 湖北大学 The leadless electronic ceramic material and preparation method of wide operation temperature area high dielectric property

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1986245B1 (en) * 2007-04-26 2015-08-26 FUJIFILM Corporation Piezoelectric body, piezoelectrc device, and liquid discharge apparatus
WO2021026297A1 (en) * 2019-08-06 2021-02-11 University Of South Florida Composite materials and filaments composed of the same for printing three dimensional articles

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1790568A (en) * 2003-12-18 2006-06-21 Tdk株式会社 Dielectric ceramic composition, electronic component, and method for producing the same
CN107311643A (en) * 2017-07-06 2017-11-03 湖北大学 The leadless electronic ceramic material and preparation method of wide operation temperature area high dielectric property

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