CN102584195A - Bismuth-based perovskite type leadless piezoelectric ceramic and low-temperature preparation method thereof - Google Patents

Bismuth-based perovskite type leadless piezoelectric ceramic and low-temperature preparation method thereof Download PDF

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CN102584195A
CN102584195A CN2012100324590A CN201210032459A CN102584195A CN 102584195 A CN102584195 A CN 102584195A CN 2012100324590 A CN2012100324590 A CN 2012100324590A CN 201210032459 A CN201210032459 A CN 201210032459A CN 102584195 A CN102584195 A CN 102584195A
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CN102584195B (en
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周昌荣
杨华斌
周沁
袁昌来
陈国华
单旭
岑侦勇
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Guilin University of Electronic Technology
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Abstract

The invention discloses leadless piezoelectric ceramic of a perovskite structure sintered at the temperature of 900 DEG C under the non-pressure and low-temperature conditions and a preparation method. A general formula is (1-x)BiMeO3-xBa(Ti1-uZru)O3+Y, wherein the x and the u represent mole fractions, the Y represents low temperature frits, 0<x<0.5, 0<u<0.5 and 0<Y<0.1. In the formula, the M is a trivalent metal element. By means of a traditional ceramic preparation technology, the non-pressure low-temperature sintering and modification on piezoelectric property of the leadless piezoelectric ceramic at the temperature of 900 DEG C in the air are achieved. The bismuth-based perovskite type leadless piezoelectric ceramic and the low-temperature preparation method are suitable for novel low-temperature sintering materials and devices for piezoelectric ceramic multilayer drivers, transformers, transducers and the like and can use Ni, Cu and other base metal materials as electrode materials, thereby remarkably reducing the production cost.

Description

A kind of bismuthino perovskite typed leadless piezoelectric ceramics and low temperature preparation method thereof
Technical field
The present invention relates to lead-free piezoceramic material, particularly a kind of bismuthino perovskite typed leadless piezoelectric ceramics and low temperature preparation method thereof.
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.The sintering temperature of this conventional piezoelectric pottery is generally all more than 1000 ℃.In addition,, cause the stoichiometric ratio of material to depart from the prescription that is originally designed, its electrical property is descended because the part element volatilizees easily when high temperature sintering.Sintering method commonly used at present mainly contains the sealing sintering process, buries burning method, atmosphere method, overflow method, but these methods mainly are constant in order to ensure the stoichiometric ratio in the prescription, can not fundamentally solve plumbous volatilization.Therefore suppress the element volatilization actively and effective means is the low-temperature sintering that realizes piezoelectric ceramics.In addition, low-temperature sintering can cut down the consumption of energy.Particularly when preparation multilayer piezoelectric ceramic driving mechanism, can realize the common burning of low-temperature electrodes material, can reduce production costs.Therefore, the research and development low-temperature melt piezoelectric ceramic material has become the emphasis of domestic and international current research.
Document [Serhiy O, J Am Ceram Soc, 2009,92 (12): 2957-2961] has been reported the BiFeO with high-curie temperature and good piezoelectric property 3– BaTiO 3Based leadless piezoelectric ceramics, but need be in oxygen atmosphere sintering, sintering temperature is at 950-975 ℃, is difficult to and low-priced electrode materials Cu, Ni etc. realize burning altogether.Document [Ichiro Fujii, J J Appl Phys, 2011,50:09ND07] has been reported the adulterated BaTiO of a kind of Mn 3-Bi (Mg 1/2Ti 1/2) O 3-BiFeO 3Leadless piezoelectric ceramics, but sintering temperature is more than 975 ℃.
Summary of the invention
The purpose of this invention is to provide a kind of bismuthino perovskite typed leadless piezoelectric ceramics and low temperature preparation method thereof; This leadless piezoelectric ceramics is through adding polynary complex sintering aids; Adopt the traditional ceramics sintering technology, realize lead-free ceramics 900 ℃ of low-temperature sinterings of nothing pressure in air atmosphere.The new type low temperature that this technology is fit to devices such as piezoceramic multilayer driving mechanism, X-former, transverter burns material and device technology altogether, can adopt base metal materials such as Ni, Cu as electrode materials, reduces production costs significantly.
Main contents of the present invention:
(1) prescription of the leadless piezoelectric ceramics of low temperature pressureless sintering:
(1- x) BiMeO 3- xBa (Ti 1-uZr u) O 3+ Y, wherein x, uThe expression x, Y representes polynary complex sintering aids.0< x<0.5，0< ?u?<0.5，0<Y<0.1。Me is a trivalent metallic element in the formula.Trivalent metallic element Me is one or more among Fe, Co, Ni, Sc, Mo, In, Al, Ga and the Mn, wherein contains Fe at least.Described sintering aid Y is Li 2CO 3, SrCO 3, CuO, V 2O 5, MnO 2, SnO 2, ZnO, SiO 2, Bi 2O 3, MoO 3, Ba (W 0.5Cu 0.5) O 3With B 2O 3In multiple, wherein contain CuO, SrCO at least 3, MnO 2The composition of the mol ratio m of wherein polynary complex sintering aids Y is respectively: 0≤m (Li 2CO 3)≤20%, 0<m (SrCO 3)≤50%, 0<m (CuO)≤50%, 0≤m (V 2O 5)≤15%, 0<m (MnO 2)≤20%, 0≤m (SnO 2)≤15%, 0≤m (ZnO)≤30%, 0≤m (SiO 2)≤30%, 0≤m (Bi 2O 3)≤20%, 0≤m (MoO 3)≤15%, 0≤m (B 2O 3)≤15%; 0≤m (Ba (W 0.5Cu 0.5) O 3)≤30%.
(2) the piezoelectric ceramics preparation method of above-mentioned (1) is a solid-phase synthesis, and the preparation method comprises the steps:
1. with analytical pure Li 2CO 3, V 2O 5, SnO 2, SiO 2, Bi 2O 3, MoO 3, Ba (W 0.5Cu 0.5) O 3, B 2O 3, CuO, SrCO 3, Bi 2O 3, Li 2CO 3,MnO 2With multiple among the ZnO be raw material, prepare burden according to the composition of Y, be the medium ball milling with the absolute ethyl alcohol, drying;
With the analytical pure raw material according to chemical formula (1- x) BiMeO 3- xBa (Ti 1-uZr u) O 3Preparing burden, is medium ball milling 24 hours with the absolute ethyl alcohol, 80 ℃ of oven dry, puts into the high alumina crucible and adds a cover, and synthesizes in 6 hours with temperature rise rate to the 850 ℃ insulation of 250 ℃/h; The synthetic powder adds the many first complex sintering aids of Y, is medium ball milling 24 hours with the absolute ethyl alcohol, 80 ℃ of oven dry, adds the granulation of 5%PVA solution;
In punching block in the moulding of 100MPa pressed;
4. the plain sheet of moulding at 600 ℃ of insulation 2h binder removals, again with temperature rise rate to the 900 ℃ insulation 2h sintering of 100 ℃/min, cools to 850 ℃ of insulation 2h with the speed of 2 ℃/min with the temperature rise rate of 100 ℃/h, and furnace cooling is to room temperature.Sample behind the sintering is processed into that the two sides is smooth, the thin slice of the about 1mm of thickness, drapes over one's shoulders silver electrode;
5. in silicone oil, polarize, polarized electric field 5000V/mm, 120 ℃ of temperature, keep electric field to be cooled to room temperature at 10 minutes time.
Advantage of the present invention is: this leadless piezoelectric ceramics adopts the traditional ceramics sintering technology through adding polynary complex sintering aids, realizes lead-free ceramics 900 ℃ of low-temperature sinterings of nothing pressure in air atmosphere.The new type low temperature that this technology is fit to devices such as piezoceramic multilayer driving mechanism, X-former, transverter burns material and device technology altogether, can adopt base metal materials such as Ni, Cu as electrode materials, reduces production costs significantly.
Description of drawings
Fig. 1 is the SEM figure of the leadless piezoelectric ceramics of embodiment 1;
Fig. 2 is the XRD figure of the leadless piezoelectric ceramics of embodiment 1.
Embodiment
Embodiment 1:
The composition general formula is: 0.78Bi (Fe 0.96Co 0.01Mn 0.03) O 3-0.22Ba (Ti 0.90Zr 0.10) O 3+ 0.01Y; Wherein: Y=30%CuO+40%SrCO 3+ 10%MnO 2+ 15%Bi 2O 3+ 5%Li 2CO 3
The preparation method comprises the steps:
1. with analytical pure CuO, SrCO 3, Bi 2O 3, Li 2CO 3,MnO and ZnO are raw material, according to Y=30%CuO+40%SrCO 3+ 10%MnO 2+ 15%Bi 2O 3+ 5%Li 2CO 3Preparing burden, is medium ball milling 24h with the absolute ethyl alcohol, 80 ℃ of dryings;
2. with analytical pure BaCO 3, TiO 2, ZrO 2, Bi 2O 3, Fe 2O 3, Co 2O 3, MnO 2According to chemical formula 0.78Bi (Fe 0.96Co 0.01Mn 0.03) O 3-0.22Ba (Ti 0.90Zr 0.10) O 3Preparing burden, is medium ball milling 24 hours with the absolute ethyl alcohol, 80 ℃ of oven dry, puts into the high alumina crucible and adds a cover, and synthesizes in 2 hours with temperature rise rate to the 750 ℃ insulation of 250 ℃/h; The synthetic powder adds the many first complex sintering aids of 0.01Y, is medium ball milling 24 hours with the absolute ethyl alcohol, 80 ℃ of oven dry, adds the granulation of 5%PVA solution.
In punching block in the moulding of 100MPa pressed;
4. the plain sheet of moulding at 600 ℃ of insulation 2h binder removals, again with temperature rise rate to the 900 ℃ insulation 2h sintering of 100 ℃/min, cools to 850 ℃ of insulation 2h with the speed of 2 ℃/min with the temperature rise rate of 100 ℃/h, and furnace cooling is to room temperature.Sample behind the sintering is processed into that the two sides is smooth, the thin slice of the about 1mm of thickness, drapes over one's shoulders silver electrode;
5. in silicone oil, polarize, polarized electric field 5000V/mm, 120 ℃ of temperature, keep electric field to be cooled to room temperature at 10 minutes time.
The gained sample is placed after 24 hours and by the IRE standard piezoelectric ceramics of processing is carried out the piezoelectric property measurement.
The performance measurement result is following:
d 33(pC/N) Q m k p ε r tanδ(%)
150 39 0.32 522 2.55
Embodiment 2:
The composition general formula is: 0.86Bi (Fe 0.97Mn 0.03) O 3-0.14Ba (Ti 0.80Zr 0.20) O 3+ 0.01Y; Wherein: Y=30%CuO+35%SrCO 3+ 10%MnO 2+ 15%Bi 2O 3+ 10%ZnO
The preparation method is with embodiment 1,
The performance measurement result is following:
d 33(pC/N) Q m k p ε r tanδ(%)
129 52 0.275 475 2.81
Embodiment 3:
The composition general formula is: 0.85Bi (Fe 0.97Ga 0.03) O 3-0.15Ba (Ti 0.80Zr 0.20) O 3+ 0.02Y; Wherein: Y=40%CuO+20%SrCO 3+ 15%MnO 2+ 15%Bi 2O 3+ 10%V 2O 5
The preparation method is with embodiment 1,
The performance measurement result is following:
d 33(pC/N) Q m k p ε r tanδ(%)
133 36 0.296 482 2.59
Embodiment 4:
The composition general formula is: 0.75Bi (Fe 0.97Ga 0.03) O 3-0.25Ba (Ti 0.80Zr 0.20) O 3+ 0.018Y; Wherein: Y=40%CuO+40%SrCO 3+ 10%MnO 2+ 5%Li 2CO 3+ 5%ZnO
The preparation method is with embodiment 1, and different is 820 ℃ of calcined temperatures,
The performance measurement result is following:
d 33(pC/N) Q m k p ε r tanδ(%)
166 35 0.341 618 3.57
Embodiment 5:
The composition general formula is: 0.75Bi (Fe 0.97Ga 0.03) O 3-0.25Ba (Ti 0.80Zr 0.20) O 3+ 0.018Y; Wherein: Y=40%CuO+30%SrCO 3+ 10%MnO 2+ 5%Bi 2O 3+ 5%Li 2CO 3+ 5%ZnO+10%Ba (W 0.5Cu 0.5) O 3
The preparation method is with embodiment 4,
The performance measurement result is following:
d 33(pC/N) Q m k p ε r tanδ(%)
176 51 0.348 661 2.26
Embodiment 6:
The composition general formula is: 0.75Bi (Fe 0.97Ga 0.03) O 3-0.25Ba (Ti 0.80Zr 0.20) O 3+ 0.018Y; Wherein: Y=30%CuO+40%SrCO 3+ 5%MnO 2+ 5%Bi 2O 3+ 10%Ba (W 0.5Cu 0.5) O 3+ 5%V 2O 5+ %SnO 2
The preparation method is with embodiment 4,
The performance measurement result is following:
d 33(pC/N) Q m k p ε r tanδ(%)
136 28 0.30 521 3.01
Embodiment 7:
The composition general formula is: 0.72Bi (Fe 0.90Sc 0.10) O 3-0.28Ba (Ti 0.88Zr 0.12) O 3+ 0.015Y; Wherein: Y=30%CuO+40%SrCO 3+ 10%MnO 2+ 10%Bi 2O 3+ 5%MoO 3+ 5%Bi 2O 3
The preparation method is with embodiment 1, and different is 850 ℃ of calcined temperatures
The performance measurement result is following:
d 33(pC/N) Q m k p ε r tanδ(%)
170 72 0.34 672 3.49
Embodiment 8:
The composition general formula is: 0.77Bi (Fe 0.90In 0.05Sc 0.05) O 3-0.23Ba (Ti 0.98Zr 0.02) O 3+ 0.012Y; Wherein: Y=30%CuO+40%SrCO 3+ 15%MnO 2+ 5%B 2O 3+ 5%ZnO+5%Li 2CO 3
The preparation method is with embodiment 1,
The performance measurement result is following:
d 33(pC/N) Q m k p ε r tanδ(%)
155 69 0.316 528 2.82
Embodiment 9:
The composition general formula is: 0.70Bi (Fe 0.90Ni 0.02Al 0.05Ga 0.03) O 3-0.30Ba (Ti 0.90Zr 0.10) O 3+ 0.025Y; Wherein: Y=30%CuO+30%SrCO 3+ 15%MnO 2+ 15%ZnO+5%MoO 3+ 5%B 2O 3
The preparation method is with embodiment 7,
The performance measurement result is following:
d 33(pC/N) Q m k p ε r tanδ(%)
165 52 0.322 535 2.52
Embodiment 10:
The composition general formula is: 0.85Bi (Fe 0.90Co 0.02Al 0.05Ga 0.03) O 3-0.15Ba (Ti 0.90Zr 0.10) O 3+ 0.01Y; Wherein: Y=30%CuO+30%SrCO 3+ 10%MnO 2+ 10%SnO 2+ 10%SiO 2+ 10%B 2O 3
The preparation method is with embodiment 1.
The performance measurement result is following:
d 33(pC/N) Q m k p ε r tanδ(%)
105 92 0.212 437 2.72
Bound, the interval value of the bound of the composition that the present invention is cited, interval value and processing parameter can both realize the present invention, do not enumerate enforcement one by one at this.

Claims (4)

1. low temperature sintering perovskite structure leadless piezoelectric ceramics is characterized in that: forming general formula is (1- x) BiMeO 3- xBa (Ti 1-uZr u) O 3+ Y, wherein x, uThe expression x, Y representes polynary complex sintering aids, 0< x<0.5,0< u<0.5,0<y<0.1 M is a trivalent metallic element in the formula.
2. like claim 1, described calcium titanium ore structure leadless piezoelectric ceramics is characterized in that: described trivalent metallic element M is one or more among Fe, Co, Ni, Sc, Mo, In, Al, Ga and the Mn, wherein contains Fe at least.
3. like claim 1, described calcium titanium ore structure leadless piezoelectric ceramics is characterized in that: described polynary sintering aid Y is Li 2CO 3, SrCO 3, CuO, V 2O 5, MnO 2, SnO 2, ZnO, SiO 2, Bi 2O 3, Ba (W 0.5Cu 0.5) O 3, MoO 3With B 2O 3In multiple, wherein contain CuO, SrCO at least 3, MnO 2Wherein the composition of the mol ratio m of Y is respectively: 0≤m (Li 2CO 3)≤20%, 0<m (SrCO 3)≤50%, 0<m (CuO)≤50%, 0≤m (V 2O 5)≤15%, 0<m (MnO 2)≤20%, 0≤m (SnO 2)≤15%, 0≤m (ZnO)≤30%, 0≤m (SiO 2)≤30%, 0≤m (Bi 2O 3)≤20%, 0≤m (MoO 3)≤15%, 0≤m (B 2O 3)≤15%, 0≤m (Ba (W 0.5Cu 0.5)≤30%.
4. like the preparation method of the described calcium titanium ore structure leadless piezoelectric ceramics of claim 1-3, it is characterized in that: adopt the solid-phase synthesis of traditional ceramics, key step is following:
(1) with analytical pure Li 2CO 3, V 2O 5, SnO 2, SiO 2, Bi 2O 3, MoO 3, Ba (W 0.5Cu 0.5) O 3, B 2O 3, CuO, SrCO 3, Bi 2O 3, Li 2CO 3,MnO 2With multiple among the ZnO be raw material, prepare burden according to the composition of Y, be the medium ball milling with the absolute ethyl alcohol, drying;
(2) with the analytical pure raw material according to chemical formula (1- x) BiMeO 3- xBa (Ti 1-uZr u) O 3Preparing burden, is medium ball milling 24 hours with the absolute ethyl alcohol, 80 ℃ of oven dry, puts into the high alumina crucible and adds a cover, synthetic to 750-850 ℃ of insulation 2 hours with the temperature rise rate of 250 ℃/h; The synthetic powder adds the many first complex sintering aids of Y, is medium ball milling 24 hours with the absolute ethyl alcohol, 80 ℃ of oven dry, adds the granulation of 5%PVA solution;
(3) in punching block in the moulding of 100MPa pressed;
(4) the plain sheet of moulding is incubated the 2h binder removals with the temperature rise rate of 100 ℃/h at 600 ℃; Again with the temperature rise rate to 900 of 100 ℃/min ℃ insulation 2h sintering; Speed with 2 ℃/min cools to 850 ℃ of insulation 2h; Furnace cooling is to room temperature, and the sample behind the sintering is processed into that the two sides is smooth, the thin slice of the about 1mm of thickness, drapes over one's shoulders silver electrode;
(5) in silicone oil, polarize, polarized electric field 5000V/mm, 120 ℃ of temperature, keep electric field to be cooled to room temperature at 10 minutes time.
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CN103304235A (en) * 2013-03-01 2013-09-18 苏州市职业大学 Production method of fine-grain high-strength PMN-PZT (lead zirconate titanate) piezoelectric ceramic material
CN104387049A (en) * 2014-11-27 2015-03-04 桂林电子科技大学 Leadless piezoelectric ceramic and method for preparing leadless piezoelectric ceramic by virtue of low-temperature liquid phase sintering
CN106518050A (en) * 2016-10-09 2017-03-22 常州亚环环保科技有限公司 Preparation method of piezoelectric ceramic transformer material
CN107032786A (en) * 2017-05-11 2017-08-11 桂林电子科技大学 It is a kind of while having low fever's leadless piezoelectric ceramics of high tension performance and high mechanical quality factor and preparation method thereof
CN110511018A (en) * 2019-08-13 2019-11-29 华南师范大学 A kind of high energy density ceramic capacitor dielectric and preparation method thereof
CN110511043A (en) * 2019-09-18 2019-11-29 昆明贵研新材料科技有限公司 It is a kind of to use normal pressure-sintered bismuth ferrite ceramics of low-melting-point glass auxiliary agent and preparation method thereof
CN111068659A (en) * 2019-12-13 2020-04-28 中山大学 Composite piezoelectric catalytic material, preparation method thereof and sludge dewatering application
CN111320468A (en) * 2020-03-03 2020-06-23 北京科技大学 Preparation method of doped bismuth ferrite-barium titanate lead-free piezoelectric ceramic material
CN112151667A (en) * 2020-09-10 2020-12-29 广州凯立达电子股份有限公司 Leadless multi-layer piezoelectric ceramic piece with high piezoelectric constant of base metal electrode

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CN101200370A (en) * 2007-10-18 2008-06-18 桂林电子科技大学 Ternary system sodium-bismuth titanate lead-free piezoelectric ceramics
CN102320828A (en) * 2011-06-16 2012-01-18 桂林电子科技大学 Unleaded piezoelectric ceramic consisting of B-site composite Bi-based compound and preparation method thereof

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CN101024574A (en) * 2007-01-30 2007-08-29 合肥工业大学 Sodium-potassium niobate series substituted by bismuth-base calcium-titanium ore and preparing method
CN101200370A (en) * 2007-10-18 2008-06-18 桂林电子科技大学 Ternary system sodium-bismuth titanate lead-free piezoelectric ceramics
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CN103304235A (en) * 2013-03-01 2013-09-18 苏州市职业大学 Production method of fine-grain high-strength PMN-PZT (lead zirconate titanate) piezoelectric ceramic material
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CN104387049A (en) * 2014-11-27 2015-03-04 桂林电子科技大学 Leadless piezoelectric ceramic and method for preparing leadless piezoelectric ceramic by virtue of low-temperature liquid phase sintering
CN106518050A (en) * 2016-10-09 2017-03-22 常州亚环环保科技有限公司 Preparation method of piezoelectric ceramic transformer material
CN107032786A (en) * 2017-05-11 2017-08-11 桂林电子科技大学 It is a kind of while having low fever's leadless piezoelectric ceramics of high tension performance and high mechanical quality factor and preparation method thereof
CN107032786B (en) * 2017-05-11 2020-07-17 桂林电子科技大学 Low-firing lead-free piezoelectric ceramic with high piezoelectric performance and high mechanical quality factor and preparation method thereof
CN110511018A (en) * 2019-08-13 2019-11-29 华南师范大学 A kind of high energy density ceramic capacitor dielectric and preparation method thereof
CN110511043A (en) * 2019-09-18 2019-11-29 昆明贵研新材料科技有限公司 It is a kind of to use normal pressure-sintered bismuth ferrite ceramics of low-melting-point glass auxiliary agent and preparation method thereof
CN111068659A (en) * 2019-12-13 2020-04-28 中山大学 Composite piezoelectric catalytic material, preparation method thereof and sludge dewatering application
CN111068659B (en) * 2019-12-13 2021-02-05 中山大学 Composite piezoelectric catalytic material, preparation method thereof and sludge dewatering application
CN111320468A (en) * 2020-03-03 2020-06-23 北京科技大学 Preparation method of doped bismuth ferrite-barium titanate lead-free piezoelectric ceramic material
CN112151667A (en) * 2020-09-10 2020-12-29 广州凯立达电子股份有限公司 Leadless multi-layer piezoelectric ceramic piece with high piezoelectric constant of base metal electrode

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