CN104402425A - Preparation method of low-loss ferrite bismuth-barium titanate-based piezoelectric ceramic - Google Patents
Preparation method of low-loss ferrite bismuth-barium titanate-based piezoelectric ceramic Download PDFInfo
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Abstract
The invention discloses a low-loss BiFeO3-BaTiO3-based leadless piezoelectric ceramic and a preparation method thereof. The composition general formula of the low-loss BiFeO3-BaTiO3-based leadless piezoelectric ceramic is (1-x)(Bi1-tLat)FeO3-xBa(Ti1-uSnu)O3+0.5%BiMnO3+yBa(Cu1/3Nb2/3)O3+zLiBiO3+mBa(W1/2Cu1/2)O3, wherein t, x, u, y, z and m express mole fractions; t is larger than 0 and less than or equal to 0.02; x is larger than or equal to 0.15 and less than or equal to 0.30; u is larger than 0 and less than 0.05; y is larger than 0 and less than 0.05; z is larger than 0 and less than 0.05; m is larger than 0 and less than 0.05. The preparation method comprises the processes of preparing materials according to the composition general formula, ball milling, molding pills, discharging glue, sintering and the like. By adopting the technologies of reduction of sintering temperature, rapid heating and cooling and high pressure oxygen, volatilization of Bi element is reduced, oxygen vacancy is restrained, valence change of Fe<3+> is prevented in the cooling process, and therefore, the purpose of reducing dielectric loss is achieved, the high temperature leadless piezoelectric ceramic with the dielectric loss lower than 0.5% is prepared, and the leadless piezoelectric ceramic can be practically applied to the high temperature piezoelectric field.
Description
Technical field
The present invention relates to a kind of preparation method of leadless piezoelectric ceramics, the preparation method of the low-loss high-performance bismuth ferrite specifically adopting low temperature liquid phase Fast Sintering to prepare under hyperbaric oxygen condition-barium phthalate base high-temp leadless piezoelectric ceramics.
Background technology
Piezoelectric ceramics is widely used in high-tech sectors such as information, laser, navigation, electronic technology, communication, Measuring and testing, precision sizing and sensing technologies.Bismuth ferrite-barium titanate system piezoelectric ceramics is because it is unleaded, sintering temperature is low, high-curie temperature, high umpolarization temperature and good piezoelectric property receive very big concern, 2009, Serhiy O. Leontsev and Richard E. Eitel etc. reported this system obtainable piezoelectric constant under sintering condition in oxygen atmosphere
d 33=116
pC/N, umpolarization temperature
t d=469
othe piezoelectric ceramics of C, but because the dielectric loss of this system is always higher, the dielectric loss under 1KHZ is 4.6%, seriously limits its actual Application and Development, therefore how reducing the dielectric loss of this system, is the gordian technique that this system is able in high-temperature field application.
BiFeO
3-BaTiO
3the dielectric loss of system causes primarily of the factor of the following aspects: (1) is due to pure BiFeO
3sintering temperature be about 750 degree, and BaTiO
3sintering temperature be about 1450 degree, both reach 700 at difference
oc, therefore, in order to improve BiFeO
3-BaTiO
3the density of ceramic systems and performance, the sintering temperature of two-phase sosoloid is 1000
omore than C, and Bi element at high temperature highly volatile, therefore make the stoichiometric ratio of sintered products off-design; (2) Fe
3+appraising at the current rate of ion, at temperature-fall period, Fe
3+ion has part to be transformed into Fe
2+ion.In order to maintain valency balance, these two kinds of factors all can cause the generation of a large amount of Lacking oxygen, finally make the dielectric loss of sample higher, polarization difficulty.Therefore this system is the dielectric loss how controlling this system in the key that high-temperature piezoelectric field is applied.
Summary of the invention
The object of the invention is for BiFeO
3-BaTiO
3deficiency existing for system, and the preparation method of a kind of low-loss bismuth ferrite-barium titanate base piezoelectric ceramic is provided.Dielectric loss has effectively been reduced to less than 1.0% by this piezoelectric ceramic energy, makes it be applied in high-temperature field.
The technical scheme realizing the object of the invention is:
A kind of low-loss bismuth ferrite-barium titanate base piezoelectric ceramic, its composition general formula is: (1-
x) (Bi
1-
t la
t ) FeO
3-
xba (Ti
1-
u sn
u ) O
3+ 0.5%BiMnO
3+
yba (Cu
1/3nb
2/3) O
3+
zliBiO
3+
mba (W
1/2cu
1/2) O
3, wherein
t,
x,
u, y, z, mrepresent molar fraction, and 0<
t≤ 0.02,0.15≤
x≤ 0.30,0<
u<0.05,0<
y<0.05,0<
z<0.05,0<
m<0.05.
A preparation method for low-loss bismuth ferrite-barium titanate base piezoelectric ceramic, comprises the steps:
(1) with analytical pure Fe
2o
3, Bi
2o
3, BaCO
3, TiO
2, La
2o
3, SnO
2, MnCO
3,cuO, WO
3, Nb
2o
5, Li
2cO
3for raw material, according to (1-
x) (Bi
1-
t la
t ) FeO
3-
xba (Ti
1-
u sn
u ) O
3+
zliBiO
3
+ 0.5%BiMnO
3+
yba (Cu
1/3nb
2/3) O
3+
mba (W
1/2cu
1/2) O
3carry out (the wherein 0< for preparing burden
t≤ 0.02,0.15≤
x≤ 0.30,0<
u<0.05,0<
y<0.05,0<
z<0.05,0<
m<0.05), take dehydrated alcohol as medium ball milling 24 hours, dried at 100 DEG C/12 hours, sieve, put into high alumina crucible to add a cover, put into airtight oxygen-supplying tube formula stove again with the temperature rise rate of 250 DEG C/h to 800 DEG C, add high pressure oxygen to 20MPa, is incubated synthesis in 4 hours, and cooling down to 200 rear taking-up below spending.
(2) (1-step 1 synthesized
x) (Bi
1-
t la
t ) FeO
3-
xba (Ti
1-
u sn
u ) O
3+ 0.5%BiMnO
3+
yba (Cu
1/3nb
2/3) O
3+
zliBiO
3 + mBa(W
1/2cu
1/2) O
3(wherein 0<
t≤ 0.02,0.15≤
x≤ 0.30,0<
u<0.05,0<
y<0.05,0<
z<0.05,0<
m<0.05) carrying out secondary ball milling, take dehydrated alcohol as medium ball milling 24 hours, dry, sieves;
(3) powder after sieving is added the granulation of 5%PVA solution, compression moulding under 100MPa in punching block, mould interior diameter is about 1cm;
(4) shaping plain sheet is slowly warming up to 600 DEG C with the temperature rise rate of 30 DEG C/h, and insulation 6h binder removal, takes out for subsequent use after furnace cooling;
(5) the plain sheet of binder removal directly being pushed 750 degree leads in the tube furnace of pure oxygen, sealing, and with the temperature rise rate of 20 DEG C/min to 840-860 DEG C, oxygenation high pressure is to 20MPa simultaneously, insulation 30min, and step-down, opens tube furnace, directly cools in taking-up sample to air;
(6) sample after sintering is processed into the thin slice that two sides is smooth, thickness is about 1mm, drapes over one's shoulders silver electrode, 600
ofor subsequent use after C/30min silver ink firing;
(7) polarized in silicone oil by the piezoelectric ceramic piece of preparation, polarized electric field 6000V/mm, temperature 150 DEG C, 30 minutes time, keeps electric field to be cooled to room temperature.
positively effect of the present invention is:
Preparation method of the present invention is successfully on the basis keeping excellent properties, and (1) reduces sintering temperature by interpolation sintering aid and employing is rapidly heated, and reduces the volatilization of Bi element in sintering process, ensures the balance of stoichiometric ratio; (2) adopt hyperbaric oxygen condition, suppress the generation of Lacking oxygen; (3) adopt the sintering technology of chilling, and adopt element doping to suppress Fe in sintering temperature-fall period
3+ion transit is Fe
2+ion, suppresses the generation of Lacking oxygen.By the combination of these three technology, being down to by dielectric loss can at less than 1.0% of high-temperature field application, and this is for BiFeO
3-BaTiO
3system piezoelectric ceramics, technically, has important breakthrough and technical innovation, and has practicality.
Embodiment
Embodiment 1:
Composition general formula: 0.75 (Bi
0.99la
0.01) FeO
3-0.25Ba (Ti
0.98sn
0.02) O
3-0.5%BiMnO
3+ 0.6%LiBiO
3+ 0.6%Ba (Cu
1/3nb
2/3) O
3+ 0.5% Ba (W
1/2cu
1/2) O
3, preparation method comprises the steps:
(1) with analytical pure Fe
2o
3, Bi
2o
3, BaCO
3, TiO
2, La
2o
3, SnO
2, MnCO
3,cuO, WO
3, Nb
2o
5, Li
2cO
3for raw material, according to 0.75 (Bi
0.99la
0.01) FeO
3-0.25Ba (Ti
0.98sn
0.02) O
3-
0.5%BiMnO
3+ 0.8%LiBiO
3+ 0.6%Ba (Cu
1/3nb
2/3) O
3+ 0.5% Ba (W
1/2cu
1/2) O
3prepare burden, take dehydrated alcohol as medium ball milling 24 hours, dried at 100 DEG C/12 hours, sieve, put into high alumina crucible to add a cover, then put into airtight oxygen-supplying tube formula stove with the temperature rise rate of 250 DEG C/h to 800 DEG C, the oxygen that adds high pressure is to 20MPa, be incubated synthesis in 4 hours, and cooling down to 200 rear taking-up below spending.
(2) 0.75 (Bi step 1 synthesized
0.99la
0.01) FeO
3-0.25Ba (Ti
0.98sn
0.02) O
3-0.5%BiMnO
3+ 0.8%LiBiO
3+ 0.6%Ba (Cu
1/3nb
2/3) O
3+ 0.5% Ba (W
1/2cu
1/2) O
3carrying out secondary ball milling, take dehydrated alcohol as medium ball milling 24 hours, dry;
(3) powder after sieving is added the granulation of 5%PVA solution, compression moulding under 100MPa in punching block, mould interior diameter is about 1cm;
(4) shaping plain sheet is slowly warming up to 600 DEG C with the temperature rise rate of 30 DEG C/h, and insulation 6h binder removal, takes out for subsequent use after furnace cooling;
(5) the plain sheet of binder removal directly being pushed 750 degree leads in the tube furnace of pure oxygen, and sealing, is rapidly heated 860 DEG C with the temperature rise rate of 20 DEG C/min, oxygenation high pressure is to 20MPa simultaneously, insulation 30min, step-down, open tube furnace, directly take out in sample to air and cool;
(6) sample after sintering is processed into the thin slice that two sides is smooth, thickness is about 1mm, drapes over one's shoulders silver electrode, 600
ofor subsequent use after C/30min silver ink firing;
(7) polarized in silicone oil by the piezoelectric ceramic piece of preparation, polarized electric field 6000V/mm, temperature 150 DEG C, 30 minutes time, keeps electric field to be cooled to room temperature.
Performance measurements is as follows:
| d 33(pC/N) | Q m | k p | ε r | tanδ(%) |
| 161 | 43.2 | 0.31 | 788 | 0.913 |
Embodiment 2:
Composition: 0.75 (Bi
0.99la
0.01) FeO
3-0.25Ba (Ti
0.99sn
0.01) O
3-0.5%BiMnO
3+ 0.6%LiBiO
3+
0.6%Ba(Cu
1/3Nb
2/3)O
3+0.8% Ba(W
1/2Cu
1/2)O
3
Preparation method is with embodiment 1.
Performance measurements is as follows:
| d 33(pC/N) | Q m | k p | ε r | tanδ(%) |
| 157 | 41 | 0.30 | 764 | 0.961 |
Embodiment 3:
Composition: 0.75 (Bi
0.99la
0.01) FeO
3-0.25Ba (Ti
0.99sn
0.01) O
3-0.5%BiMnO
3+ 0.8%LiBiO
3+
0.6%Ba (Cu
1/3nb
2/3) O
3+ 1.0% Ba (W
1/2cu
1/2) O
3preparation method with embodiment 1, unlike sintering temperature 850 DEG C/4h
Performance measurements is as follows:
| d 33(pC/N) | Q m | k p | ε r | tanδ(%) |
| 138 | 37 | 0.296 | 730 | 0.984 |
Embodiment 4:
Composition: 0.80 (Bi
0.99la
0.01) FeO
3-0.20Ba (Ti
0.98sn
0.02) O
3-0.5%BiMnO
3+ 0.8%LiBiO
3+
0.9%Ba(Cu
1/3Nb
2/3)O
3+1.0% Ba(W
1/2Cu
1/2)O
3
Preparation method with embodiment 1, unlike sintering temperature 840 DEG C.
Performance measurements is as follows:
| d 33(pC/N) | Q m | k p | ε r | tanδ(%) |
| 136 | 29 | 0.25 | 429 | 0.99 |
Bound, the interval value of the bound of the composition cited by the present invention, interval value and processing parameter can realize the present invention, do not enumerate enforcement at this.
Claims (2)
1. low-loss bismuth ferrite-barium titanate base piezoelectric ceramic, is characterized in that: its composition general formula is: (1-
x) (Bi
1-
t la
t ) FeO
3-
xba (Ti
1-
u sn
u ) O
3+ 0.5%BiMnO
3+
yba (Cu
1/3nb
2/3) O
3+
zliBiO
3+
mba (W
1/2cu
1/2) O
3, wherein
t,
x,
u, y, z, mrepresent molar fraction, and 0<
t≤ 0.02,0.15≤
x≤ 0.30,0<
u<0.05,0<
y<0.05,0<
z<0.05,0<
m<0.05.
2. a preparation method for low-loss bismuth ferrite-barium titanate base piezoelectric ceramic, is characterized in that: comprise the steps:
(1) with analytical pure Fe
2o
3, Bi
2o
3, BaCO
3, TiO
2, La
2o
3, SnO
2, MnCO
3,cuO, WO
3, Nb
2o
5, Li
2cO
3for raw material, according to (1-
x) (Bi
1-
t la
t ) FeO
3-
xba (Ti
1-
u sn
u ) O
3+
zliBiO
3
+ 0.5%BiMnO
3+
yba (Cu
1/3nb
2/3) O
3+
mba (W
1/2cu
1/2) O
3carry out (the wherein 0< for preparing burden
t≤ 0.02,0.15≤
x≤ 0.30,0<
u<0.05,0<
y<0.05,0<
z<0.05,0<
m<0.05), take dehydrated alcohol as medium ball milling 24 hours, dried at 100 DEG C/12 hours, sieve, put into high alumina crucible to add a cover, put into airtight oxygen-supplying tube formula stove again with the temperature rise rate of 250 DEG C/h to 800 DEG C, add high pressure oxygen to 20MPa, is incubated synthesis in 4 hours, and cooling down to 200 rear taking-up below spending;
(2) (1-step 1 synthesized
x) (Bi
1-
t la
t ) FeO
3-
xba (Ti
1-
u sn
u ) O
3+ 0.5%BiMnO
3+
yba (Cu
1/3nb
2/3) O
3+
zliBiO
3 + mBa(W
1/2cu
1/2) O
3(wherein 0<
t≤ 0.02,0.15≤
x≤ 0.30,0<
u<0.05,0<
y<0.05,0<
z<0.05,0<
m<0.05) carrying out secondary ball milling, take dehydrated alcohol as medium ball milling 24 hours, dry, sieves;
(3) powder after sieving is added the granulation of 5%PVA solution, compression moulding under 100MPa in punching block, mould interior diameter is about 1cm;
(4) shaping plain sheet slowly heats up to 600 DEG C with the temperature rise rate of 30 DEG C/h, is incubated 6h binder removal, takes out for subsequent use after furnace cooling;
(5) the plain sheet of binder removal directly being pushed 750 degree leads in the tube furnace of pure oxygen, sealing, and with the temperature rise rate of 20 DEG C/min to 840-860 DEG C, oxygenation high pressure is to 20MPa simultaneously, insulation 30min, and step-down, opens tube furnace, directly cools in taking-up sample to air;
(6) sample after sintering is processed into the thin slice that two sides is smooth, thickness is about 1mm, drapes over one's shoulders silver electrode, 600
ofor subsequent use after C/30min silver ink firing;
(7) polarized in silicone oil by the piezoelectric ceramic piece of preparation, polarized electric field 6000V/mm, temperature 150 DEG C, 30 minutes time, keeps electric field to be cooled to room temperature.
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|---|---|---|---|
| CN201410691071.0A CN104402425B (en) | 2014-11-27 | 2014-11-27 | A kind of preparation method of low-loss bismuth ferrite-barium titanate base piezoelectric ceramic |
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| CN104402425A true CN104402425A (en) | 2015-03-11 |
| CN104402425B CN104402425B (en) | 2016-08-17 |
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| CN109503152A (en) * | 2018-12-29 | 2019-03-22 | 内蒙古大学 | Solid solution membrane and preparation method thereof with segregation particle |
| CN110272286A (en) * | 2019-07-23 | 2019-09-24 | 中国科学技术大学 | A method of improving ferrous acid bismuth-based ceramics ferromagnetism and magneto-electric coupled coefficient |
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| CN111138177A (en) * | 2020-01-09 | 2020-05-12 | 桂林电子科技大学 | Bismuth ferrite-bismuth zinc titanate high-temperature lead-free piezoelectric ceramic with high-temperature stability and preparation method thereof |
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| CN102249659A (en) * | 2011-06-16 | 2011-11-23 | 桂林电子科技大学 | Bismuth ferrite-based leadless piezoelectric ceramic with high Curie temperature and preparation method thereof |
| CN102584194A (en) * | 2012-02-14 | 2012-07-18 | 桂林电子科技大学 | Perovskite leadless piezoelectric ceramic used at high temperature and preparation method thereof |
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| CN102249659A (en) * | 2011-06-16 | 2011-11-23 | 桂林电子科技大学 | Bismuth ferrite-based leadless piezoelectric ceramic with high Curie temperature and preparation method thereof |
| CN102584194A (en) * | 2012-02-14 | 2012-07-18 | 桂林电子科技大学 | Perovskite leadless piezoelectric ceramic used at high temperature and preparation method thereof |
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| WO2020062618A1 (en) * | 2018-09-28 | 2020-04-02 | 东北大学 | Ferroelectric material with good temperature stability, preparation method therefor and use thereof |
| CN109336185A (en) * | 2018-12-03 | 2019-02-15 | 广东先导稀材股份有限公司 | The production method of micron order mangaic acid bismuth meal body |
| CN109503152A (en) * | 2018-12-29 | 2019-03-22 | 内蒙古大学 | Solid solution membrane and preparation method thereof with segregation particle |
| CN109503152B (en) * | 2018-12-29 | 2021-06-15 | 内蒙古大学 | Solid solution film with meta-aggregated particles and preparation method thereof |
| CN111454054A (en) * | 2019-01-22 | 2020-07-28 | Tdk株式会社 | Piezoelectric composition and piezoelectric element |
| CN111454054B (en) * | 2019-01-22 | 2022-07-01 | Tdk株式会社 | Piezoelectric composition and piezoelectric element |
| CN110272286A (en) * | 2019-07-23 | 2019-09-24 | 中国科学技术大学 | A method of improving ferrous acid bismuth-based ceramics ferromagnetism and magneto-electric coupled coefficient |
| CN110272286B (en) * | 2019-07-23 | 2020-10-27 | 中国科学技术大学 | Method for improving ferromagnetic and magnetoelectric coupling coefficient of bismuth ferrite-based ceramic |
| CN111138177A (en) * | 2020-01-09 | 2020-05-12 | 桂林电子科技大学 | Bismuth ferrite-bismuth zinc titanate high-temperature lead-free piezoelectric ceramic with high-temperature stability and preparation method thereof |
| CN114262225A (en) * | 2021-12-29 | 2022-04-01 | 湖南省嘉利信陶瓷科技有限公司 | High-purity nano electronic ceramic and preparation method thereof |
| CN114262225B (en) * | 2021-12-29 | 2022-10-21 | 湖南省嘉利信陶瓷科技有限公司 | High-purity nano electronic ceramic and preparation method thereof |
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