CN102910902A - BNT-BT-BKT-based perovskite system multielement lead-free piezoelectric ceramic and production method thereof - Google Patents

BNT-BT-BKT-based perovskite system multielement lead-free piezoelectric ceramic and production method thereof Download PDF

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CN102910902A
CN102910902A CN2012104062224A CN201210406222A CN102910902A CN 102910902 A CN102910902 A CN 102910902A CN 2012104062224 A CN2012104062224 A CN 2012104062224A CN 201210406222 A CN201210406222 A CN 201210406222A CN 102910902 A CN102910902 A CN 102910902A
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戴叶婧
许威
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Tianjin University
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Abstract

The invention discloses a BNT-BT-BKT-based perovskite system multielement lead-free piezoelectric ceramic and a production method thereof. The BNT-BT-BKT-based perovskite multielement lead-free piezoelectric ceramic comprises the following raw material components by mole percent: (1-x)[a(Bi0.5Na0.5)TiO3-bBaTiO3-c(Bi0.5K0.5)TiO3]-x[(Na0.52K0.44Li0.04)(Nb0.88Sb0.08Ta0.04)O3], wherein in the formula, x is 0.001-0.05, a is 0.8-0.9, and b+c is 1-a and is more than 0.5 and less than 0.9. According to the BNT-BT-BKT-based perovskite multielement lead-free piezoelectric ceramic, the principal crystalline phase is of a perovskite structure, the piezoelectric performance is better, the maximum piezoelectric constant is 328pC/N, the maximum electromechanical coupling coefficient kp is 0.32, and the effects of stable production process, repeatability and practicality are obtained.

Description

A kind of BNT-BT-BKT based perovskite system multi-component leadless piezoelectric ceramics and preparation method thereof
Technical field
The present invention relates to a kind of ceramic composition take composition as feature, particularly relate to a kind of bismuth sodium titanate-barium titanate-Bismuth carbonate potassium (BNT-BT-BKT) base and mix polynary uhligite system piezoelectric ceramics of potassium-sodium niobate lithium tantalum antimony (KNNLST) mixing and preparation method thereof.
Background technology
Piezoelectric ceramics, as modern and important hi-tech functional materials, it is used and has spreaded all over military affairs, the every field, particularly ultrasonic transduction such as civilian, sensor, the fields such as nondestructive testing and mechanics of communication.In recent years, be accompanied by the whole world to the understanding of mankind itself's environment, take Pb-based lanthanumdoped zirconate titanates as main plumbous oxide or the tri-lead tetroxide of containing in the lead piezoelectric ceramics accounts for raw-materially more than 3/4ths, bring the risk that to estimate to environment.So, replace traditional lead base piezoceramic material in the urgent need to seeking leadless piezoelectric material material.
At present, the piezoelectric ceramics of research mainly contains the leadless piezoelectric ceramics of perovskite structure, bismuth laminated and tungsten bronze structure.In general, the bismuth laminated leadless piezoelectric ceramic Curie temperature is higher, and anisotropy is large and piezoelectric activity is lower.Tungsten bronze structure system piezoelectric ceramics has the characteristics such as spontaneous polarization strength is large, Curie temperature is high, specific inductivity is low, and its composition and structure has material impact to its ferroelectric properties.
The bismuth-sodium titanate leadless piezoelectric ceramics is found in nineteen sixty, it is one of stable complex perovskite structure few in number, it is strong that the BNT pottery has ferroelectricity, piezoelectric property is good, little and the acoustical behavior of specific inductivity waits well excellent characteristic, be considered to most probable and replace one of leadless piezoelectric ceramics system of lead base piezoelectric ceramics, just obtaining broad research.But the coercive field of pure BNT pottery is large, and is high in the ferroelectric phase region specific conductivity, thereby is difficult to polarization, and the firing range of pure BNT is narrower, so make ceramic dense not good enough.BNT-BT-BKT system " Hajime Nagata; Masaki Yoshida et e1.Jpn J Appl Phys, 42 (2003) 7404. " piezoelectric constant is larger, and Curie temperature is high, but the coercive field of this system and specific conductivity are still larger, and the field intensity that abundant polarization needs is up to 5 ~ 9kV/mm.
Potassium-sodium niobate system particularly document " Y.Saito; et al. " Lead-Free Piezoceramics "; nature; 432 (2004) 84-87. " adopts traditional solid-phase sintering method to prepare to have the relatively potassium-sodium niobate lithium tantalum antimony leadless piezoelectric ceramics of high tension performance, the piezoelectric ceramics sintering temperature of the method preparation is lower than 1100 ℃, but contain the volatile elements such as a large amount of lithiums, potassium and sodium, the more difficult densification of sintering process and sintering character are unstable.
Above-mentioned two kinds because intrinsic shortcoming separately also has a certain distance apart from practical application, existing electrical property and the preparation technology's report that yet there are no in the literature take BNT-BT-BKT as matrix doping KNNLST piezoelectric ceramics.
Summary of the invention
The object of the invention is to, overcome the shortcoming and defect of prior art, a kind of stable BNT-BT-BKT based perovskite system multicomponent system high tension performance piezoelectric ceramics preparation of good piezo-electric modulus, sintering character and preparation method thereof that has is provided.
The present invention is achieved by following technical solution.
A kind of BNT-BT-BKT based perovskite system multi-component leadless piezoelectric ceramics, its feed composition and molar percentage thereof are (1-x) [a (Bi 0.5Na 0.5) TiO 3-bBaTiO 3-c (Bi 0.5K 0.5) TiO 3]-x[(Na 0.52K 0.44Li 0.04) (Nb 0.88Sb 0.08Ta 0.04) O 3], x=0.001 in the formula ~ 0.05, a=0.8 ~ 0.9, b+c=1-a, 0.5＜b+c＜0.9.
The preparation method of above-mentioned BNT-BT-BKT based perovskite system multi-component leadless piezoelectric ceramics, step is:
(1) uses K 2CO 3, Na 2CO 3, TiO 2, Bi 2O 3With BaCO3 be initial feed, press a (Bi 0.5Na 0.5) TiO 3-bBaTiO 3-c (Bi 0.5K 0.5) TiO 3Be abbreviated as BNT-BT-BKT and prepare burden, a=0.8 in the formula ~ 0.9, b+c=1-a; Obtain the BNT-BT-BKT ceramic powder through ball milling mixing, pre-burning, wherein calcined temperature is 850 ℃;
(2) use Li 2CO 3, K 2CO 3, Na 2CO 3, Nb 2O 5, Ta 2O 5And Sb 2O 3Be initial feed, by (Na 0.52K 0.44Li 0.04) (Nb 0.88Sb 0.08Ta 0.04) O 3Be abbreviated as KNNLST and prepare burden, obtain the KNNLST ceramic powder through ball milling mixing, pre-burning, wherein calcined temperature is 850 ℃;
(3) by (1-x) (BNT-BT-BKT)-x(KNNLST), x=0.001 in the formula ~ 0.05 is mixed in proportion BNT-BT-BKT and the KNNLST ceramic powder of step (1) and step (2) preparation, mixes through ball milling, drying obtains the multicomponent system ceramic powder;
(4) the multicomponent system ceramic powder that obtains in step (3) drips polyvinyl alcohol dicarbaldehyde spirituous solution and grinds in mortar as binding agent, and wherein the mass percent of polyvinyl alcohol dicarbaldehyde is 1 ~ 10%;
(5) pour the BNT-BT-BKT-KNNLST mangcorn of step (4) into grinding tool, press mold is shaped to base substrate;
(6) base substrate with step (5) places retort furnace to carry out binder removal, is warming up to 600 ℃ with the temperature rise rate of 5 ℃/min, insulation 10min, furnace cooling;
(7) base substrate behind step (6) binder removal is placed retort furnace, be warming up to 1040～1140 ℃ of sintering with the temperature rise rate of 5 ℃/min, insulation 1 ~ 2h, furnace cooling obtains BNT-BT-BKT-KNNLST uhligite system multi-component leadless piezoelectric ceramics goods;
(8) the uhligite system multi-component leadless piezoelectric ceramics goods with step (7) apply the low-temperature silver slurry, in 700 ℃ of insulation 10min, make electrode;
(9) electrode slice that step (7) is prepared enters in the silicone oil and polarizes.
The Ball-milling Time of described step (1) and (2) is 6h.
The pressure of described step (5) press mold moulding is 65～130MPa.
The preferred sintering temperature of described step (7) is 1300～1400 ℃.
The polarization time of described step (9) is 10 ~ 30min, and polarized electric field is 2 ~ 4KV/mm.
The invention has the beneficial effects as follows, adopting bismuth sodium titanate-barium titanate-bismuth potassium titanate is the uhligite system leadless piezoelectric ceramics that the preparation of matrix doping potassium-sodium niobate lithium tantalum antimony contains nine kinds of elements, only comprise perovskite structure, occur without dephasign, piezoelectric constant d33 is 167 ~ 238pC/N.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of example 1 of the present invention;
Fig. 2 is the scanning electron microscope picture of example 2 of the present invention.
Embodiment
Barium carbonate (BaCO used in the present invention 3), bismuth oxide (Bi 2O 3), titanium dioxide (TiO 2), Quilonum Retard (Li 2CO 3), yellow soda ash (Na 2CO 3), salt of wormwood (K 2CO 3), Niobium Pentxoxide (Nb 2O 5), antimony peroxide (Sb 2O 5), tantalum pentoxide (Ta 2O 5) etc. raw material be commercially available chemically pure reagent.Specific embodiment is as follows.
Embodiment 1
Present embodiment matrix component be 0.88 (Bi 0.5Na 0.5) TiO 3-0.0305BaTiO 3-0.0895 (Bi 0.5K 0.5) TiO 3, another component is (Na 0.52K 0.44Li 0.04) (Nb 0.88Sb 0.08Ta 0.04) O 3
The first step is B with analytical pure level mass percent 2IO 3, TiO 2, Na 2CO 3, K 2CO 3, and BaCO 3By 0.88 (Bi 0.5Na 0.5) TiO 3-0.0305BaTiO 3-0.0895 (Bi 0.5K 0.5) TiO 3Stoichiometric ratio is prepared burden.With the raw material ball milling 6h in dehydrated alcohol for preparing, 100 ℃ of lower insulation 2h, behind the oven dry powder, 850 ℃ of pre-burnings, insulation 2h obtains the BNT-BT-BKT powder.Use Li 2CO 3, K 2CO 3, Na 2CO 3, Nb 2O 5, Ta 2O 5And Sb 2O 3By (Na 0.52K 0.44Li 0.04) (Nb 0.88Sb 0.08Ta 0.04) O 3Stoichiometric ratio is prepared burden, with the raw material ball milling 6h in anhydrous ethanol medium for preparing, and 100 ℃ of lower insulation 2h, after the oven dry, in 850 ℃ of pre-burnings, insulation 2h obtains the KNNLST powder.
Second step, the preparation (1-x) (BNT-BT-BKT)-the xKNNLST powder.The BNT-BT-BKT that obtains with the first step and KNNLST are in the weighing of x=0.02 ratio, and ball milling 6h in anhydrous ethanol medium in 100 ℃ of lower insulation 2h, is dried powder, obtains 0.98 (BNT-BT-BKT)-0.02KNNLST powder.
The 3rd step: moulding.The powder weighing that second step obtains is poured in the mortar, pressed powder: PVB spirituous solution=1g:2g drips 6%PVB spirituous solution, granulation, compression moulding under the pressure of 100MPa.
The 4th step: sintering.With ceramic green dry 10min under 600 ℃ in the 3rd step, binder removal; In 1140 ℃ of sintering, insulation 2h, furnace cooling obtains the BNT-BT-BKT-KNNLST leadless piezoelectric ceramics.
The 5th step: detect.The leadless piezoelectric ceramics surface-coated low-temperature silver slurry that makes in the 4th step, 700 ℃ of insulation 10min make electrode, the leadless piezoelectric ceramics electrode slice are immersed the 10min that polarizes in the room temperature silicone oil again, and polarized electric field is 2kV.
The performance test results of embodiment 1 is as follows:
d33(pC/N) Kp εr Kt
238 0.312 1725 0.479
Fig. 1 is the X ray diffracting spectrum of embodiment 1 uhligite multicomponent system piezoelectric ceramics.Show that this ceramic plate is perovskite structure.
Embodiment 2
Present embodiment matrix component be 0.8325 (Bi 0.5Na 0.5) TiO 3-0.0426BaTiO 3-0.1249 (Bi 0.5K 0.5) TiO 3, another component is (Na 0.52K 0.44Li 0.04) (Nb 0.88Sb 0.08Ta 0.04) O 3
The first step is B with analytical pure level mass percent 2IO 3, TiO 2, Na 2CO 3, K 2CO 3, and BaCO 3By 0.8325 (Bi 0.5Na 0.5) TiO 3-0.0426BaTiO 3-0.1249 (Bi 0.5K 0.5) TiO 3Stoichiometric ratio is prepared burden.With the raw material ball milling 6h in dehydrated alcohol for preparing, 100 ℃ of lower insulation 2h, behind the oven dry powder, 850 ℃ of pre-burnings, insulation 2h obtains the BNT-BT-BKT powder.Use Li 2CO 3, K 2CO 3, Na 2CO 3, Nb 2O 5, Ta 2O 5And Sb 2O 3By (Na 0.52K 0.44Li 0.04) (Nb 0.88Sb 0.08Ta 0.04) O 3Stoichiometric ratio is prepared burden, and with the raw material ball milling 6h in anhydrous ethanol medium for preparing, 100 ℃ of lower insulation 2h behind the oven dry powder, at 850 ℃ of pre-burning 2h, obtain the KNNLST powder.
Second step, the preparation (1-x) (BNT-BT-BKT)-the xKNNLST powder.The BNT-BT-BKT that obtains with the first step and KNNLST are in the weighing of x=0.005 ratio, and ball milling 6h in anhydrous ethanol medium in 100 ℃ of lower insulation 2h, is dried powder, obtains 0.98 (BNT-BT-BKT)-0.02KNNLST powder.
The 3rd step: moulding.The powder weighing that second step obtains is poured in the mortar, pressed powder: PVB spirituous solution=1g:2g drips 6%PVB spirituous solution, granulation, compression moulding under the pressure of 100MPa.
The 4th step: sintering.With ceramic green dry 10min under 600 ℃ in the 3rd step, binder removal.In 1100 ℃ of sintering, insulation 2h, furnace cooling obtains the BNT-BT-BKT-KNNLST leadless piezoelectric ceramics.
The 5th step: detect.The leadless piezoelectric ceramics surface-coated low-temperature silver slurry that makes in the 4th step, 700 ℃ of insulation 10min make electrode.The leadless piezoelectric ceramics electrode is immersed the 10min that polarizes in the room temperature silicone oil, polarized electric field is 2.4kV again.
The performance test results of embodiment 2 is as follows:
d33(pC/N) Kp εr Kt
190 0.274 1546 0.415
Fig. 2 is the scanning electron microscope picture of embodiment 2 piezoelectric ceramics, and by picture as can be known, this ceramic plate has fine and close structure.
Embodiment 3
Present embodiment matrix component be 0.80 (Bi 0.5Na 0.5) TiO 3-0.0509BaTiO 3-0.1491 (Bi 0.5K 0.5) TiO 3, another component is (Na 0.52K 0.44Li 0.04) (Nb 0.88Sb 0.08Ta 0.04) O 3
Carry out BNT-BT-BKT and KNNLST batching by stoichiometric ratio, ball milling 6h is dried respectively, and 850 ℃ of pre-burning 2h obtain BNT-BT-BKT and KNNLST powder.In the weighing of x=0.05 ratio, ball milling 6h is dried, and obtains 0.95 (BNT-BT-BKT)-0.05KNNLST powder with the BNT-BT-BKT that obtains and KNNLST.The powder weighing that obtains is poured in the mortar, dripped the PVB spirituous solution, granulation, compression moulding under the pressure of 100MPa.With 600 ℃ of lower dry 10min of ceramic green, binder removal.In 1040 ℃ of heat preservation sinterings, 2h, furnace cooling obtains the BNT-BT-BKT-KNNLST pottery.Apply the silver slurry at ceramic surface, 700 ℃ of insulation 10min.The ceramic plate polarization 10min that makes, polarized electric field is 2.4kV.
Other processing parameter of present embodiment is same as embodiment 1.
The performance test results of embodiment 3 is as follows:
d33(pC/N) Kp εr Kt
157 0.252 1324 0.376
Embodiment 4
Present embodiment matrix component be 0.8625 (Bi 0.5Na 0.5) TiO 3-0.0350BaTiO 3-0.1025 (Bi 0.5K 0.5) TiO 3, another component is (Na 0.52K 0.44Li 0.04) (Nb 0.88Sb 0.08Ta 0.04) O 3
Carry out BNT-BT-BKT and KNNLST batching by stoichiometric ratio, ball milling 6h is dried respectively, and 850 ℃ of pre-burning 2h obtain BNT-BT-BKT and KNNLST powder.BNT-BT-BKT and KNNLST powder are pressed the x=0.015 weighing, ball milling 6h, oven dry obtains 0.985 (BNT-BT-BKT)-0.015KNNLST powder.Powder is poured in the mortar, dripped the PVB spirituous solution, granulation, the compression moulding of 100MPa pressure.With 600 ℃ of dry 10min of green compact, binder removal.In 1140 ℃ of sintering, insulation 2h, furnace cooling obtains the BNT-BT-BKT-KNNLST pottery.Apply the silver slurry at ceramic surface, 700 ℃ of insulation 10min.The ceramic plate polarization 9min that makes, polarized electric field is 2.2kV/mm.
Other processing parameter of present embodiment is same as embodiment 1.
The performance test results of embodiment 4 is as follows:
d33(pC/N) Kp εr Kt
212 0.297 1628 0.408

Claims (5)

1. BNT-BT-BKT based perovskite system multi-component leadless piezoelectric ceramics, its feed composition and molar percentage thereof are (1-x) [a (Bi 0.5Na 0.5) TiO 3-bBaTiO 3-c (Bi 0.5K 0.5) TiO 3]-x[(Na 0.52K 0.44Li 0.04) (Nb 0.88Sb 0.08Ta 0.04) O 3], x=0.001 in the formula ~ 0.05, a=0.8 ~ 0.9, b+c=1-a, 0.5＜b+c＜0.9.
The preparation method of above-mentioned BNT-BT-BKT based perovskite system multi-component leadless piezoelectric ceramics, step is:
(1) uses K 2CO 3, Na 2CO 3, TiO 2, Bi 2O 3And BaCO 3Be initial feed, press a (Bi 0.5Na 0.5) TiO 3-bBaTiO 3-c (Bi 0.5K 0.5) TiO 3Be abbreviated as BNT-BT-BKT and prepare burden, a=0.8 in the formula ~ 0.9, b+c=1-a; Obtain the BNT-BT-BKT ceramic powder through ball milling mixing, pre-burning, wherein calcined temperature is 850 ℃;
(2) use Li 2CO 3, K 2CO 3, Na 2CO 3, Nb 2O 5, Ta 2O 5And Sb 2O 3Be initial feed, by (Na 0.52K 0.44Li 0.04) (Nb 0.88Sb 0.08Ta 0.04) O 3Be abbreviated as KNNLST and prepare burden, obtain the KNNLST ceramic powder through ball milling mixing, pre-burning, wherein calcined temperature is 850 ℃;
(3) by (1-x) (BNT-BT-BKT)-x(KNNLST), x=0.001 in the formula ~ 0.05 is mixed in proportion BNT-BT-BKT and the KNNLST ceramic powder of step (1) and step (2) preparation, mixes through ball milling, drying obtains the multicomponent system ceramic powder;
(4) the multicomponent system ceramic powder that obtains in step (3) drips polyvinyl alcohol dicarbaldehyde spirituous solution and grinds in mortar as binding agent, and wherein the mass percent of polyvinyl alcohol dicarbaldehyde is 1 ~ 10%;
(5) pour the BNT-BT-BKT-KNNLST mangcorn of step (4) into grinding tool, press mold is shaped to base substrate;
(6) base substrate with step (5) places retort furnace to carry out binder removal, is warming up to 600 ℃ with the temperature rise rate of 5 ℃/min, insulation 10min, furnace cooling;
(7) base substrate behind step (6) binder removal is placed retort furnace, be warming up to 1040～1140 ℃ with the temperature rise rate of 5 ℃/min, insulation 1 ~ 2h sintering, furnace cooling obtains BNT-BT-BKT-KNNLST uhligite system multi-component leadless piezoelectric ceramics goods;
(8) the uhligite system multi-component leadless piezoelectric ceramics goods with step (7) apply the low-temperature silver slurry, in 700 ℃ of insulation 10min, make electrode;
(9) electrode slice that step (7) is prepared enters in the silicone oil and polarizes.
2. according to claim 1 a kind of BNT-BT-BKT based perovskite system multi-component leadless piezoelectric ceramics is characterized in that the Ball-milling Time of described step (1) and (2) is 6h.
3. according to claim 1 a kind of BNT-BT-BKT based perovskite system multi-component leadless piezoelectric ceramics is characterized in that the pressure of described step (5) press mold moulding is 65～130MPa.
4. according to claim 1 a kind of BNT-BT-BKT based perovskite system multi-component leadless piezoelectric ceramics is characterized in that, the preferred sintering temperature of described step (7) is 1080 ℃.
5. according to claim 1 a kind of BNT-BT-BKT based perovskite system multi-component leadless piezoelectric ceramics is characterized in that the polarization time of described step (9) is 10 ~ 30min, and polarized electric field is 2 ~ 4KV/mm.
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CN113853362A (en) * 2019-05-22 2021-12-28 赛尔科技有限公司 Method for preparing solid solution ceramic materials with increased electromechanical strain and ceramic materials obtainable therefrom

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KR20150129389A (en) * 2014-05-12 2015-11-20 울산대학교 산학협력단 Lead-free piezoelectric ceramic composition and Preparation method thereof
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CN105130419A (en) * 2015-08-26 2015-12-09 同济大学 High electrostrictive leadless piezoelectric ceramic material and preparation method therefor and application thereof
CN105837205A (en) * 2016-03-24 2016-08-10 天津大学 Sodium bismuth titanate-system lead-free piezoelectric ceramic and preparation method thereof
CN106007706A (en) * 2016-05-12 2016-10-12 天津大学 High-performance sodium bismuth titanate-based leadless piezoelectric ceramic and preparation method thereof
CN106045499A (en) * 2016-05-27 2016-10-26 西北工业大学 Preparation method of zirconium-doped and lanthanum-doped sodium titanate-barium titanate ceramics
CN107935586A (en) * 2017-11-13 2018-04-20 陕西科技大学 BT KBT base energy storage ceramics that a kind of potassium niobate is modified and preparation method thereof
CN110128169A (en) * 2019-05-10 2019-08-16 济南大学 The SiO adulterated using calcium ion2The method and its application that film is modified piezoelectric ceramics surface
CN110128169B (en) * 2019-05-10 2021-05-18 济南大学 SiO doped with calcium ions2Method for modifying piezoelectric ceramic surface by membrane and application thereof
CN113853362A (en) * 2019-05-22 2021-12-28 赛尔科技有限公司 Method for preparing solid solution ceramic materials with increased electromechanical strain and ceramic materials obtainable therefrom

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