CN102285794B - Lead-free piezoelectric ceramic composed of B-site complex perovskite-structured compounds - Google Patents

Lead-free piezoelectric ceramic composed of B-site complex perovskite-structured compounds Download PDF

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CN102285794B
CN102285794B CN2011101624225A CN201110162422A CN102285794B CN 102285794 B CN102285794 B CN 102285794B CN 2011101624225 A CN2011101624225 A CN 2011101624225A CN 201110162422 A CN201110162422 A CN 201110162422A CN 102285794 B CN102285794 B CN 102285794B
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杨华斌
周昌荣
周沁
成钧
袁昌来
陈国华
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Guilin University of Electronic Technology
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Abstract

The invention discloses a lead-free piezoelectric ceramic composed of B-site complex perovskite-structured compounds. The ingredients of the ceramic are shown in the general formula of (1-x)Bi(Li1/3Me2/3)O3-xBaTiO3+zMaOb, (1-x)Bi(Li1/3Me2/3)O3-x(Na1/2Bi1/2)TiO3+zMaOb, (1-x-y)Bi(Li1/3Me2/3)O3-xBaTiO3-y(Na1/2Bi1/2)TiO3+zMaOb, (1-x-y)Bi(Li1/3Me2/3)O3-xBaTiO3-y(Na1/2Bi1/2)TiO3+zMaOb or (1-x-y-v)Bi(Li1/3Me2/3)O3-xBaTiO3-y(Na1/2Bi1/2)TiO3-v(K1/2Bi1/2)TiO3+zMaOb, wherein x, y, z and v are the molar fractions, 0<x<1.0, 0<y<1, 0<v<1 and 0<=z<=0.1; Me is one or more of tetravalent metal elements; and MaOb is one or more oxides and M is an element which has a valence of +1 to +6 and can form a solid oxide with oxygen. The lead-free piezoelectric ceramic disclosed by the invention has very good piezoelectric and dielectric properties, and compared with the traditional lead-based piezoelectric ceramic, the lead-free piezoelectric ceramic has significant advantages, is green and environmentally-friendly and can meet the environmental protection requirements.

Description

The leadless piezoelectric ceramics that B position complex perovskite structure compound forms
Technical field
The present invention relates to piezoceramic material, specifically the leadless piezoelectric ceramics of B position complex perovskite structure compound composition.
Background technology
Piezoelectric ceramics is widely used in fields such as transverter, micro positioner, sensor, resonator and wave filters, is one of a kind of indispensable hi tech and new material.At present, the whole world is traditional lead piezoelectric ceramics (as lead zirconate titanate PZT) that contain at a large amount of piezoelectric ceramics that use, and in these materials, plumbous oxide content accounts for more than 60%.Due to the easy volatile of lead, all can cause great pollution to air, water source, environment etc. in production, preparation, use and waste treatment.It is very harmful that lead poisoning causes, and especially children's intelligence caused very macrolesion.Day by day deep along with environmental consciousness just actively forbidden leaded electronic product by forms such as law, rules, government's instructions in the world.Therefore developing green environment-friendly type piezoelectric ceramics becomes the focus of present research.In the leadless piezoelectric ceramics system of studying at present, bismuth-sodium titanate (Na 1/2Bi 1/2) TiO 3(being called for short NBT) and potassium-sodium niobate (K 0.5Na 0.5NbO 3, KNN) series piezoelectric ceramic is considered to the leadless piezoelectric material material of the most promising alternative PZT.A lot of scholars replace the A of the piezoelectric ceramics of this two individual system, B position, and doping vario-property, preparation method and process modification are done a lot of work, but the equidistant practical application of its theoretical investigation and technical problem also there is a big difference.Therefore also need develop new practicality environment-friendly type piezoceramic material system.
Because Bi is adjacent with Pb on the periodic table of elements, have identical electron distributions, close ionic radius and molecular weight, therefore, Bi base ferroelectrics is considered to have good piezoelectric property.Simultaneously, PZT base piezoelectric ceramic such as Pb (Ti, the Zr) O of the replacement of B position compound ion 3-Pb (Mg 1/3Nb 2/3) O 3Has good piezoelectric property.Therefore, the compound Bi base in novel B position FE compound also has the good piezoelectric property of similar PZT base pottery.Therefore, this patent puts forward a kind of B position complex perovskite structure Bi (Li 1/3Me 2/3) O 3Based leadless piezoelectric ceramics.But existing document does not also have B position complex perovskite structure Bi (Li 1/3Me 2/3) O 3The report of based leadless piezoelectric ceramics.
Summary of the invention
Leadless piezoelectric ceramics that the novel B position complex perovskite structure compound that the purpose of this invention is to provide high-performance, practicality, is easy to prepare forms and preparation method thereof.
The technical scheme that realizes the object of the invention is: B position complex perovskite structure leadless piezoelectric ceramics is used respectively following general formula:
(1- x)Bi(Li 1/3Me 2/3)O 3- xBaTiO 3+ zM aO b；
(1- x)Bi(Li 1/3Me 2/3)O 3- x(Na 1/2Bi 1/2)TiO 3?+ zM aO b；
(1- x- y)?Bi(Li 1/3Me 2/3)O 3- xBaTiO 3- y(Na 1/2Bi 1/2)TiO 3+ zM aO b；
(1- x- y)Bi?(Li 1/3Me 2/3)O 3- xBaTiO 3- y(K 1/2Bi 1/2)TiO 3+ zM aO b；
(1- x- y- v) Bi (Li 1/3Me 2/3) O 3– xBaTiO 3- y(Na 1/2Bi 1/2) TiO 3- v(K 1/2Bi 1/2) TiO 3+ zM aO bRepresent, wherein x, y, zWith vThe expression molar fraction, 0＜ x＜1.0,0＜ y＜1,0＜ v＜1,0≤ z≤ 0.1, Me is the tetravalent metal element, M aO bBe one or more oxide compounds, wherein M is+1 ~+6 valency and can forms with oxygen the element of solid-oxide.
Quadrivalent element Me is one or more in Ti, Zr, Hf, Sn and Mn; One or more oxide Ms aO bM be selected from one or more in La, Sm, Mn, Ce, Nd, Pm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Ge, Sc, In, Y, Lu, Al, Cu, Li, Na, K, Ca, Sr, Mg, Zn, Ni, Ag, Mn, Fe, Co, Cr and Sn.
B of the present invention position complex perovskite structure leadless piezoelectric ceramics has good piezoelectric property, its piezoelectric constant d 33More than can reaching 220 pC/N, electromechanical coupling factor k tCan reach more than 0.4.Can adopt the preparation of process for electroceramics and conventional industrial raw material, technology stability is good, and need not to add any new installation can realize producing in electronic material producer, has practicality.
Embodiment
By embodiment given below, can further clearly understand content of the present invention, but they not limitation of the invention.
Embodiment 1:
Prepared composition is: (1- x- y- v) Bi (Li 1/3Me 2/3) O 3- xBaTiO 3- y(Na 1/2Bi 1/2) TiO 3- v(K 1/2Bi 1/2) TiO 3+ zM aO b, wherein x=0.05, y=0.78, v=0.12, z=0.01; Me=90%Ti+10%Zr, the leadless piezoelectric ceramics that the B position complex perovskite structure compound of M=Ce+La forms
The preparation method comprises the steps:
With analytical pure Bi 2O 3, Na 2CO 3, BaCO 3, K 2CO 3, Li 2CO 3, ZrO, CeO 2, La 2O 3And TiO 2Be raw material, respectively according to following chemical formula:
(1- x- y- v) Bi (Li 1/3Ti 2/3) O 3- xBaTiO 3- y(Na 1/2Bi 1/2) TiO 3- v(K 1/2Bi 1/2) TiO 3+ z(La 2O 3+ CeO 2) (wherein x=0.05, y=0.78, v=0.12, z=0.01)
accurately after weighing, take dehydrated alcohol as ball-milling medium ball milling 12 h, after drying, under 900 ℃, insulation 2 h are synthetic, add the PVA solution of 3 % as binding agent after the broken granulation of sieving of powder oven dry after synthetic, be pressed into diameter of phi 18 mm under the pressure of 100 MPa, the round base of thick 1～1.5 mm, heat up at a slow speed (3 ℃/min) to 600 ℃ of insulation 2 h binder removals, then with the heat-up rate of 200 ℃/h, at 1150 ℃ of lower sintered heat insulating 2 h, drape over one's shoulders silver electrode after the sample polishing, polarize in the silicone oil of 60～80 ℃, polarizing voltage is 3～4 kv/mm, polarization time is 15 min.Sample after polarization is placed 24 h and is tested its performance again.
The performance measurement result is as follows:
d 33(pC/N) Q m K t ε r tanδ(%) K p
220 87 0.483 1403 3.23 0.39
Embodiment 2:
Prepared composition is: (1- x- y) Bi (Li 1/3Me 2/3) O 3- xBaTiO 3- y(Na 1/2Bi 1/2) TiO 3+ zM aO b, wherein x=0.06, y=0.82, v=0.12, z=0.01; Me=90%Ti+10%Sn, the leadless piezoelectric ceramics that the B position complex perovskite structure compound of M=In+Yb forms
The preparation method:
With analytical pure Bi 2O 3, Na 2CO 3, BaCO 3, Li 2CO 3, SnO, Yb 2O 3, In 2O 3And TiO 2Be raw material, respectively according to following chemical formula:
(1- x- y) Bi (Li 1/3Me 2/3) O 3- xBaTiO 3- y(Na 1/2Bi 1/2) TiO 3+ zM aO b+ z(Yb 2O 3+ In 2O 3) (wherein x=0.06, y=0.82, v=0.12, z=0.01)
accurately after weighing, take dehydrated alcohol as ball-milling medium ball milling 12 h, after drying, under 850 ℃, insulation 2 h are synthetic, add the PVA solution of 3 % as binding agent after the broken granulation of sieving of powder oven dry after synthetic, be pressed into diameter of phi 18 mm under the pressure of 100 MPa, the round base of thick 1～1.5 mm, heat up at a slow speed (3 ℃/min) to 600 ℃ of insulation 2 h binder removals, then with the heat-up rate of 200 ℃/h, at 1120 ℃ of lower sintered heat insulating 2 h, the sample polishing is rear by silver electrode, polarize in the silicone oil of 60～80 ℃, polarizing voltage is 3～4 kv/mm, polarization time is 15 min.Sample after polarization is placed 24 h and is tested its performance again.
The performance measurement result is as follows:
d 33(pC/N) Q m K t ε r tanδ(%) K p
165 153 0.460 1260 3.07 0.355
Embodiment 3:
Prepared composition is: (1- x- y- v) Bi (Li 1/3Me 2/3) O 3- xBaTiO 3- y(Na 1/2Bi 1/2) TiO 3- v(K 1/2Bi 1/2) TiO 3+ zM aO b, wherein x=0.02, y=0.05, v=0.02, z=0.03; Me=95%Ti+5%Mn, the leadless piezoelectric ceramics that the B position complex perovskite structure compound of M=La forms
The preparation method is with embodiment 1.
The performance measurement result is as follows:
d 33(pC/N) Q m K t ε r tanδ(%) K p
83 212 0.22 738 2.11 0.145
Embodiment 4:
Prepared composition is: (1- x- y- v) Bi (Li 1/3Me 2/3) O 3- xBaTiO 3- y(Na 1/2Bi 1/2) TiO 3- v(K 1/2Bi 1/2) TiO 3+ zM aO b, wherein x=0.02, y=0.1, v=0.06, z=0.03; Me=85%Ti+10%Zr+5%Sn, the leadless piezoelectric ceramics that the B position complex perovskite structure compound of M=La forms
The preparation method is with embodiment 1.
The performance measurement result is as follows:
d 33(pC/N) Q m K t ε r tanδ(%) K p
90 276 0.20 785 2.54 0.142
Embodiment 5:
Prepared composition is: (1- x- y- v) Bi (Li 1/3Me 2/3) O 3- xBaTiO 3- y(Na 1/2Bi 1/2) TiO 3- v(K 1/2Bi 1/2) TiO 3+ zM aO b, wherein x=0.02, y=0.1, v=0.90, z=0.03; Me=95%Ti+5%Sn, the leadless piezoelectric ceramics that the B position complex perovskite structure compound of M=Sm forms
The preparation method is with embodiment 1.
The performance measurement result is as follows:
d 33(pC/N) Q m K t ε r tanδ(%) K p
75 313 0.253 812 4.17 0.175
Embodiment 6:
Prepared composition is: (1- x- y) Bi (Li 1/3Me 2/3) O 3- xBaTiO 3- y(K 1/2Bi 1/2) TiO 3+ zM aO b, wherein x=0.27, y=0.10, z=0.008; Me=95%Ti+5%Zr, the leadless piezoelectric ceramics that the B position complex perovskite structure compound of M=Pr forms
The preparation method is with embodiment 1.
The performance measurement result is as follows:
d 33(pC/N) Q m K t ε r tanδ(%) K p
88 298 0.231 655 2.17 0.164
Embodiment 7:
Prepared composition is: (1- x- y) Bi (Li 1/3Me 2/3) O 3- xBaTiO 3- y(Na 1/2Bi 1/2) TiO 3+ zM aO b, wherein x=0.03, y=0.90, z=0.012; Me=90%Ti+10%Zr, the leadless piezoelectric ceramics that the B position complex perovskite structure compound of M=Dy forms
The preparation method is with embodiment 1.
The performance measurement result is as follows:
d 33(pC/N) Q m K t ε r tanδ(%) K p
125 183 0.43 1128 2.59 0.23
Embodiment 8:
Prepared composition is: (1- x- y) Bi (Li 1/3Me 2/3) O 3- xBaTiO 3- y(Na 1/2Bi 1/2) TiO 3+ zM aO b, wherein x=0.75, y=0.12, z=0.01; Me=98%Ti+2%Sn, the leadless piezoelectric ceramics that the B position complex perovskite structure compound of M=Nd forms
The preparation method is with embodiment 1.
The performance measurement result is as follows:
d 33(pC/N) Q m K t ε r tanδ(%) K p
103 236 0.35 905 2.53 0.21
Embodiment 9:
Prepared composition is: (1- x) Bi (Li 1/3Me 2/3) O 3- x(Na 1/2Bi 1/2) TiO 3+ zM aO b, wherein x=0.98, z=0.01.Me=95%Ti+5%Zr, the leadless piezoelectric ceramics that the B position complex perovskite structure compound of M=Y forms
The preparation method is with embodiment 1.
The performance measurement result is as follows:
d 33(pC/N) Q m K t ε r tanδ(%) K p
116 212 0.421 686 3.77 0.140
Embodiment 10:
Prepared composition is: (1- x) Bi (Li 1/3Me 2/3) O 3- x(Na 1/2Bi 1/2) TiO 3+ zM aO b, wherein x=0.10, z=0.01; Me=95%Ti+5%Zr, the leadless piezoelectric ceramics that the B position complex perovskite structure compound of M=Sc forms
The preparation method is with embodiment 1.
The performance measurement result is as follows:
d 33(pC/N) Q m K t ε r tanδ(%) K p
63 421 0.37 506 5.12 0.153

Claims (6)

1. leadless piezoelectric ceramics that B position complex perovskite structure compound forms, it is characterized in that: forming general formula is (1- x) Bi (Li 1/3Me 2/3) O 3- x(Na 1/2Bi 1/2) TiO 3+ zM aO b, in formula, Me is one or more tetravalent metal elements; M aO bBe one or more oxide compounds, wherein M is+1 ~+6 valency and can forms with oxygen the element of solid-oxide; xWith zMolar content in the expression ceramic systems, wherein 0＜ x＜1.0,0≤ z≤ 0.1, the preparation method of described pottery comprises wet-milling, dries, burns till porcelain, ball milling, bonding are pressed into disk sintering in disk, air, sand milling, two-sidedly drape over one's shoulders silver, polarization for the second time, specifically:
Take dehydrated alcohol as ball-milling medium ball milling 12 h, after drying, under 850-900 ℃, insulation 2 h are synthetic, add the PVA solution of 3 % as binding agent after the broken granulation of sieving of powder oven dry after synthetic, be pressed into round base under the pressure of 100 MPa, be warming up at a slow speed 600 ℃ of insulation 2 h binder removals with 3 ℃/min, then with the heat-up rate of 200 ℃/h, at 1120-1150 ℃ of lower sintered heat insulating 2 h, drape over one's shoulders silver electrode after the sample polishing, polarize in the silicone oil of 60～80 ℃, polarizing voltage is 3～4 kv/mm, and the polarization time is 15 min.
2. leadless piezoelectric ceramics that B position complex perovskite structure compound forms, it is characterized in that: forming general formula is (1- x- y) Bi (Li 1/3Me 2/3) O 3- xBaTiO 3- y(Na 1/2Bi 1/2) TiO 3+ zM aO b, in formula, Me is one or more tetravalent metal elements; M aO bBe one or more oxide compounds, wherein M is+1 ~+6 valency and can forms with oxygen the element of solid-oxide; x, yWith zMolar content in the expression ceramic systems, wherein 0＜ x＜1.0,0＜ y＜1.0,0≤ z≤ 0.1, x+ y＜1, the preparation method of described pottery comprises wet-milling, dries, burns till porcelain, ball milling, bonding are pressed into disk sintering in disk, air, sand milling, two-sidedly drape over one's shoulders silver, polarization for the second time, specifically:
Take dehydrated alcohol as ball-milling medium ball milling 12 h, after drying, under 850-900 ℃, insulation 2 h are synthetic, add the PVA solution of 3 % as binding agent after the broken granulation of sieving of powder oven dry after synthetic, be pressed into round base under the pressure of 100 MPa, be warming up at a slow speed 600 ℃ of insulation 2 h binder removals with 3 ℃/min, then with the heat-up rate of 200 ℃/h, at 1120-1150 ℃ of lower sintered heat insulating 2 h, drape over one's shoulders silver electrode after the sample polishing, polarize in the silicone oil of 60～80 ℃, polarizing voltage is 3～4 kv/mm, and the polarization time is 15 min.
3. leadless piezoelectric ceramics that B position complex perovskite structure compound forms, it is characterized in that: forming general formula is (1- x- y) Bi (Li 1/3Me 2/3) O 3- xBaTiO 3- y(K 1/2Bi 1/2) TiO 3+ zM aO b, in formula, Me is one or more tetravalent metal elements; M aO bBe one or more oxide compounds, wherein M is+1 ~+6 valency and can forms with oxygen the element of solid-oxide; x, yWith zMolar content in the expression ceramic systems, wherein 0＜ x＜1.0,0＜ y＜1.0,0≤ z≤ 0.1, x+ y＜1, the preparation method of described pottery comprises wet-milling, dries, burns till porcelain, ball milling, bonding are pressed into disk sintering in disk, air, sand milling, two-sidedly drape over one's shoulders silver, polarization for the second time, specifically:
Take dehydrated alcohol as ball-milling medium ball milling 12 h, after drying, under 850-900 ℃, insulation 2 h are synthetic, add the PVA solution of 3 % as binding agent after the broken granulation of sieving of powder oven dry after synthetic, be pressed into round base under the pressure of 100 MPa, be warming up at a slow speed 600 ℃ of insulation 2 h binder removals with 3 ℃/min, then with the heat-up rate of 200 ℃/h, at 1120-1150 ℃ of lower sintered heat insulating 2 h, drape over one's shoulders silver electrode after the sample polishing, polarize in the silicone oil of 60～80 ℃, polarizing voltage is 3～4 kv/mm, and the polarization time is 15 min.
4. leadless piezoelectric ceramics that B position complex perovskite structure compound forms, it is characterized in that: forming general formula is (1- x- y- v) Bi (Li 1/3Me 2/3) O 3- xBaTiO 3- y(Na 1/2Bi 1/2) TiO 3- v(K 1/2Bi 1/2) TiO 3+ zM aO b, in formula, Me is one or more tetravalent metal elements; M aO bBe one or more oxide compounds, wherein M is+1 ~+6 valency and can forms with oxygen the element of solid-oxide; x, yWith zMolar content in the expression ceramic systems, wherein 0＜ x＜1.0,0＜ y＜1,0＜ v＜1,0≤ z≤ 0.1, x+ y+ v＜1, the preparation method of described pottery comprises wet-milling, dries, burns till porcelain, ball milling, bonding are pressed into disk sintering in disk, air, sand milling, two-sidedly drape over one's shoulders silver, polarization for the second time, specifically:
Take dehydrated alcohol as ball-milling medium ball milling 12 h, after drying, under 850-900 ℃, insulation 2 h are synthetic, add the PVA solution of 3 % as binding agent after the broken granulation of sieving of powder oven dry after synthetic, be pressed into round base under the pressure of 100 MPa, be warming up at a slow speed 600 ℃ of insulation 2 h binder removals with 3 ℃/min, then with the heat-up rate of 200 ℃/h, at 1120-1150 ℃ of lower sintered heat insulating 2 h, drape over one's shoulders silver electrode after the sample polishing, polarize in the silicone oil of 60～80 ℃, polarizing voltage is 3～4 kv/mm, and the polarization time is 15 min.
5. leadless piezoelectric ceramics as described in one of claim 1-4, it is characterized in that: described quadrivalent element is one or more in Ti, Zr, Hf, Sn and Mn.
6. leadless piezoelectric ceramics as described in one of claim 1-4 is characterized in that: described+1 ~+6 valencys and the element that can form solid-oxide with oxygen are one or more in La, Sm, Mn, Ce, Nd, Pm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Ge, Sc, In, Y, Lu, Al, Cu, Li, Na, K, Ca, Sr, Mg, Zn, Ni, Ag, Mn, Fe, Co, Cr and Sn.
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