CN118545997B - High-dielectric-property electronic ceramic and preparation method thereof - Google Patents
High-dielectric-property electronic ceramic and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 229910002117 Bi 4Ti3O12 Inorganic materials 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims description 22
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 11
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 10
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Inorganic materials O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052593 corundum Inorganic materials 0.000 claims description 5
- XMFOQHDPRMAJNU-UHFFFAOYSA-N lead(II,IV) oxide Inorganic materials O1[Pb]O[Pb]11O[Pb]O1 XMFOQHDPRMAJNU-UHFFFAOYSA-N 0.000 claims description 5
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium(III) oxide Inorganic materials O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 claims description 5
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 5
- YEAUATLBSVJFOY-UHFFFAOYSA-N tetraantimony hexaoxide Chemical compound O1[Sb](O2)O[Sb]3O[Sb]1O[Sb]2O3 YEAUATLBSVJFOY-UHFFFAOYSA-N 0.000 claims description 5
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 3
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 4
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 5
- 238000000498 ball milling Methods 0.000 description 14
- 238000010438 heat treatment Methods 0.000 description 13
- 238000001035 drying Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 238000002156 mixing Methods 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000011812 mixed powder Substances 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000003825 pressing Methods 0.000 description 5
- 238000004321 preservation Methods 0.000 description 4
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000005036 potential barrier Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
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
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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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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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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