CN1541978A - Bismuth sodium lithium titanate barium titanate strontium titanate calcium titanate based lead-free piezoelectric ceramics - Google Patents

Bismuth sodium lithium titanate barium titanate strontium titanate calcium titanate based lead-free piezoelectric ceramics Download PDF

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CN1541978A
CN1541978A CNA2003101108797A CN200310110879A CN1541978A CN 1541978 A CN1541978 A CN 1541978A CN A2003101108797 A CNA2003101108797 A CN A2003101108797A CN 200310110879 A CN200310110879 A CN 200310110879A CN 1541978 A CN1541978 A CN 1541978A
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piezoelectric ceramics
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leadless piezoelectric
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肖定全
赁敦敏
朱建国
余萍
李灵芝
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Sichuan University
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Abstract

The lead-free bismuth sodium lithium barium strontium titanate piezoelectric ceramic is one polycomponent perovskite type environment consistency piezoelectric ceramic composition. The composition has the general expression of (1-y-z-u)Bi1-w(Na1-xLix)wTiO3+yBaTiO3+zSrTiO3+uCaTiO3+aMalphaObeta, where x is 0-0.5, y 0-1, z 0-1, u 0-1, (y+z+u) 0-1, w 0.3-0.7; MalphaObeta is doping oxide(s) in the content an of 0-10 %; M is +1~+6 valent element capable of forming solid oxide, such as Na, K, Li, Ni, Zn, etc. with alpha and beta being atom number. The piezoelectric ceramic composition has d33 up to 200 pC/N, kp up to 35.0 % and stable technological process, may be produced via traditional piezoelectric ceramic preparation process and industrial material, and is practical.

Description

The bismuth sodium lithium titanate barium titanate strontium titanate calcium titanate based leadless piezoelectric ceramics
One, technical field
The present invention relates to a kind of novel polynary lead-free piezoelectric ceramics composition, belong to perovskite structure environment compatibility piezoelectric ceramics field.
Two, background technology
Find the piezoelectricity of barium titanate ceramics from middle 1940s after, constitutional features is ABO 3The research and development of the piezoelectric ceramics of type are very active, and the components and parts of piezoelectric ceramics and making have been widely used in particularly information industry field of industry.With Pb-based lanthanumdoped zirconate titanates (Pb (Ti, Zr) O 3) being the lead base two component system of representative, the A position is Pb; The B position is that (Ti is Zr) with Pb-based lanthanumdoped zirconate titanates (Pb (Ti, Zr) O 3) be base-material, add the 3rd constituent element, as with PMN-PT [Pb (Mg 1/3Nb 2/3) O 3-PbTiO 3] being representative, the A position is Pb, the B position is Mg 1/3Nb 2/3All have good piezoelectricity ferro performance and high Curie temperature with the lead base ternary system piezoelectric ceramic of Ti.The piezoelectric ceramics overwhelming majority who uses in the industrial production is such lead base piezoelectric ceramics.
But, PbO in the lead base piezoceramic material or Pb 3O 4Content accounts for 70% of raw material total amount.PbO or Pb 3O 4At high temperature volatile, cause severe contamination and harm for the mankind and ecotope thereby make in the treating processes of lead base piezoelectric ceramics after producing, use and discarding.In recent years, seek piezoelectric ceramics system lead-free, superior performance and be subjected to the pay attention to day by day of countries in the world.
Common leadless piezoelectric ceramics system has four classes: BaTiO at present 3Based leadless piezoelectric ceramics, bismuth laminated leadless piezoelectric ceramic, base metal niobate leadless piezoelectric ceramics and Bi 0.5Na 0.5TiO 3Based leadless piezoelectric ceramics.More than the characteristics of four class leadless piezoelectric ceramicss be: BaTiO 3The base piezoelectric ceramic Curie temperature is 120 ℃ only, and piezoelectric property is medium; The Curie temperature height of bismuth laminated leadless piezoelectric ceramic, but piezoelectric activity is low; The base metal niobate leadless piezoelectric ceramics then is difficult to sinter into fine and close pottery; Bi 0.5Na 0.5TiO 3Based leadless piezoelectric ceramics has the Curie temperature height, easily add other constituent element modification becomes the research focus of non-lead base piezoelectric ceramics to improve characteristics such as piezoelectric property.
Bi 0.5Na 0.5TiO 3Be that the A position is by compound ion Bi 0.5Na 0.5The ABO that constitutes 3The perovskite typed ferroelectrics, A position compound ion Bi 0.5Na 0.5By Bi 3+(A1 position) and Na +(A2 position) constitutes.Simple Bi 0.5Na 0.5TiO 3The pottery coercive field is (73Kv/cm) greatly, and the polarization difficulty is difficult to practicability, must be to Bi 0.5Na 0.5TiO 3Carry out modification to obtain the leadless piezoelectric ceramics system that coercive field is low, the piezoelectricity ferro performance is good.At present common to Bi 0.5Na 0.5TiO 3Adding method that other constituent element carries out modification has merely with+divalent alkaline-earth metal ions and partly replaces A position ion Bi 0.5Na 0.5Or merely+1 the alkalimetal ion of valency partly replaces the Na of A2 position +Document 1 (JAPANESE JOURNAL OF APPLIED PHYSICS, Vol 30,9B, 1991,9, p2236-2239), to have provided composition formula be (1-x) Bi to document 2 (Journal of Inorganic Materials, Vol 15, No5,2000,12) 0.5Na 0.5TiO 3-xBaTiO 3The leadless piezoelectric ceramics system, d 33=125pC/N, k p=29%; It is Bi that document 3 (phys.stat.sol. (a) 157,499 (1996)) has provided composition formula 0.5Na 0.5TiO 3-Bi 0.5K 0.5TiO 3The leadless piezoelectric ceramics system, d 33=96pC/N, k p=21%; It is Bi that document 4 (Ferroelectrics.1997, Vol 196, p 175-178) and document 5 (KeyEngineering Materials Vols, 157-158 (1999) are p.57-64) have provided composition formula respectively 0.5Na 0.5TiO 3-1/2 (Bi 2O 3Sc 2O 3), Bi 0.5Na 0.5TiO 3-NaNbO 3The leadless piezoelectric ceramics system, d 33=71-92pC/N, k pBe about 15%; Document 6 (Ferroelectrics.1995, Vol 169, p 317-325) and 7 (Ferroelectrics.1990, Vol 106, and p375-380) having provided composition formula is (Bi 1/2Na 1/2) 1-x(Sr 1/2Ca 1/2) xTiO 3, (Bi 1/2Na 1/2) 1-x(Sra Pb bCa c) xTiO 3The leadless piezoelectric ceramics system, d 33=82pC/N, k p=12-20.3%.It is (1-x) Bi that patent CN85100513, JP2001-48642 provide composition formula 0.5Na 0.5TiO 3-xBaTiO 3Piezoelectric ceramic composition, k p=20.2%, ε 33/ ε 0=290, d 33=159pC/N; It is [Bi that patent JP11-217262, JP2000-22235 provide composition formula 0.5(Na 1-xK x) 0.5] TiO 3Piezoelectric ceramic composition, k p=21.1%, ε 33/ ε 0=611.It is Bi that patent DE19530592C2 has provided composition formula 0.5Na 0.5TiO 3-BaTiO 3-CaTiO 3Piezoelectric ceramic composition, said composition has thickness and big characteristics of electromechanical coupling factor anisotropy radially, k p=16%; It is [Bi that patent JP2000-44335 has provided composition formula 0.5(Na 1-xLi x) 0.5] TiO 3Piezoelectric ceramic composition, k p=23.4%, ε 33/ ε 0=432.
Three, summary of the invention
Purpose of the present invention is exactly in order to overcome the inherent defective of existing lead base piezoelectric ceramics system own, to improve existing BaTiO 3Base lead-free battery performance, proposed a class novel form leadless piezoelectric ceramics by the polynary lead-free material.This piezoelectric ceramics adopts the traditional ceramics prepared, and technology stability is good, has good piezoelectricity ferro performance, has approached the product performance of lead base pottery, has practicality.
For realizing purpose of the present invention, the present invention is directed to ABO 3Perovskite typed piezoelectrics (the Bi of structure 0.5Na 0.5) TiO 3, a class A position compound ion Bi has been proposed 0.5Na 0.5By alkaline-earth metal ions Ba 2+Or Sr 2+Or Ba 2+And Sr 2+The compound ion or the Ba that form 2+And Ca 2+The compound ion or the Ba that form 2+, Sr 2+, Ca 2+The compound ion of forming partly replaces, simultaneously A2 position ion Na +By alkalimetal ion Li +Part replaces formed novel lead-free piezoceramic material, can use general formula (1-y-z-u) Bi (1-w)(Na 1-xLi x) wTiO 3+ yBaTiO 3+ zSrTiO 3+ uCaTiO 3Represent that the x in the formula, y, z, u and w represent the shared atomicity (being atomic percent) in each constituent element of respective element material in the compound ion.0＜x in the formula＜0.5,0≤y＜1,0≤z＜1,0≤u＜1,0＜(y+z+u)＜1,0.3≤w≤0.7.
The piezoceramic material that the present invention proposes can also be added other metals by the base-material that the front general formula is represented as hotchpotch, and promptly base-material+hotchpotch is formed, and its performance is optimized more.Can be expressed as with general formula: (1-y-z-u) Bi (1-w)(Na 1-xLi x) wTiO 3+ yBaTiO 3+ zSrTiO 3+ uCaTiO 3+ M αO β(wt%), M in general formula αO βThe expression hotchpotch, the shared ratio of hotchpotch is 0-10wt%; The shared ratio of base-material is 90-100wt%.M αO βBe one or more doping oxides, M is for+1-+6 valency and can form the element of solid-oxide with oxygen, as Na, K, Li, Ni, Zn, Cr, Co, Nb, Ta, Al, Cu, Fe, Ce, Pr, Nd, Sm, Gd, Dy, Er, Yb, In, Y, Sc, La, Ho, Lu, Sn, Sb, Mn, Ca, Ba, Sr, Mg, Si etc.; α and β represent the atomicity of corresponding element M and oxygen in the relevant oxide compound respectively.
Polynary lead-free piezoelectric ceramics of the present invention has good piezoelectricity ferro performance, detects the piezoelectric constant d of this system piezoelectric ceramics through material property 33Can reach more than the 200pC/N percentage coupling k pCan reach more than 35.0% residual polarization P rVery big (40.4 μ C/cm 2), coercive field low (32.4Kv/cm), ferroelectric hysteresis loop rectangle degree good (as shown in Figure 1).Advantage of the present invention is: the leadless piezoelectric ceramics excellent property has had the performance level of Industrial products; Its process stabilizing can adopt conventional piezoelectric ceramics processing and industrial starting material to obtain, and sintering temperature is about sintering temperature and is about 1100-1150 ℃, than low about 100-150 ℃ of lead base piezoelectric ceramics, has practicality.
Four, description of drawings
Fig. 1 is the leadless piezoelectric ceramics ferroelectric hysteresis loop figure at normal temperatures that the present invention records.
Five, embodiment
Prepare leadless piezoelectric ceramics of the present invention and can adopt technical pure or chemical pure Bi 2O 3, Na 2CO 3, Li 2CO 3, BaCO 3, SrTiO 3, CaCO 3, TiO 2, M αO βBe raw material, press general formula (1-y-z-u) Bi (1-w)(Na 1-xLi x) wTiO 3+ yBaTiO 3+ zSrTiO 3+ uCaTiO 3The stoichiometric ratio raw materials weighing, behind abundant ball milling mixing, in the alumina crucible of packing into, carry out pre-burning at 800-900 ℃, soaking time is 2-6 hour.Add property-modifying additive M in the pre-burning synthetic powder αO βWt%, levigate through ball milling again, thorough mixing, adding additives, moulding, plastic removal are at last at 1050-1150 ℃ of following sintering 2-3 hour.Ceramic plate behind the sintering is by last silver electrode, and in 60-120 ℃ silicone oil, polarization is 10-20 minute under the voltage of 3-4kV/mm.
Preparation system (1-y-z-u) Bi (1-w)(Na 1-xLi x) wTiO 3+ yBaTiO 3+ zSrTiO 3+ uCaTiO 3(92-100wt%) or add hotchpotch M αO βThe prescription and the performance index of leadless piezoelectric ceramics (0-8wt%) are as follows:
Embodiment 1:
Prescription: [0.87Bi 0.5(Na 0.925Li 0.075) 0.5TiO 3+ 0.06BaTiO 3+ 0.01SrTiO 3+ 0.06CaTiO 3] (97wt%)+Li 2O (1wt%)+Y 2O 3(2wt%)
Performance: d 33(pC/N) tg δ (%) ε 33/ ε 0k p(%) Qm Poisson's ratio
208 4.3 989 36.67 78 0.302
Embodiment 2:
Prescription: [0.84Bi 0.5(Na 0.925Li 0.075) 0.5TiO 3+ 0.08BaTiO 3+ 0.02SrTiO 3+ 0.06CaTiO 3] (97wt%)+Li 2O (1wt%)+Fe 2O 3(2wt%)
Performance: d 33(pC/N) tg δ (%) ε 33/ ε 0k p(%) Qm Poisson's ratio
168 3.8 1185 17.3 82 0.297
When u=0, constitute composition formula (1-y-z) Bi (1-w)(Na 1-xLi x) wTiO 3+ yBaTiO 3+ zSrTiO 3Or interpolation hotchpotch M αO β(wt%) leadless piezoelectric ceramics.
Embodiment 3:
Prescription: 0.92Bi 0.6(Na 0.90Li 0.10) 0.4TiO 3+ 0.06BaTiO 3+ 0.02SrTiO 3
Performance: d 33(pC/N) tg δ (%) ε 33/ ε 0k p(%) Qm Poisson's ratio
200 3.6 940 32.1 109 0.296
Embodiment 4:
Prescription: 0.94Bi 0.5(Na 0.90Li 0..10) 0.5TiO 3+ 0.04BaTiO 3+ 0.02SrTiO 3
Performance: d 33(pC/N) tg δ (%) ε 33/ ε 0k p(%) Qm Poisson's ratio
134 2.9 603 31.9 195 0.302
Embodiment 5:
Prescription: [0.90Bi 0.4(Na 0.925Li 0..075) 0.6TiO 3+ 0.06BaTiO 3+ 0.04SrTiO 3] (98wt%)+Na 2O (2wt%)
Performance: d 33(pC/N) tg δ (%) ε 33/ ε 0k p(%) Qm Poisson's ratio
165 2.2 913 19.7 139 0.29
Embodiment 6:
Prescription: [0.92Bi 0.5(Na 0.9Li 0.1) 0.5TiO 3+ 0.06BaTiO 3+ 0.02SrTiO 3] (98%)+Y 2O 3(2%)
Performance: d 33(pC/N) tg δ (%) ε 33/ ε 0k p(%) Qm Poisson's ratio
169 4.5 1426 17.1 76 0.283
When y=0, constitute composition formula (1-z) Bi (1-w)(Na 1-xLi x) wTiO 3+ zSrTiO 3+ uCaTiO 3+ M αO β(wt%) leadless piezoelectric ceramics.
Embodiment 7:
Prescription: [0.81Bi 0.5(Na 0.90Li 0.10) 0.5TiO 3+ 0.13SrTiO 3+ 0.06CaTiO 3] (93wt%)+La 2O 3(4wt%)+Fe 2O 3(3wt%)
Performance: d 33(pC/N) tg δ (%) ε 33/ ε 0k p(%) Qm Poisson's ratio
123 2.9 671 27.6 193 0.313
Embodiment 8:
Prescription: [0.80Bi 0.5(Na 0.925Li 0.075) 0.5TiO 3+ 0.15SrTiO 3+ 0.05CaTiO 3] (93wt%)+La 2O 3(4wt%)+Y 2O 3(3wt%)
Performance: d 33(pC/N) tg δ (%) ε 33/ ε 0k p(%) Qm Poisson's ratio
126 2.2 633 30.3 232 0.369
When z=0, constitute composition formula (1-y-u) Bi (1-w)(Na 1-xLi x) wTiO 3+ yBaTiO 3+ uCaTiO 3+ M αO β(wt%) leadless piezoelectric ceramics.
Embodiment 9:
Prescription: [0.80Bi 0.5(Na 0.90Li 0.10) 0.5TiO 3+ 0.12BaTiO 3+ 0.08CaTiO 3] (96wt%)+Nb 2O 5(4wt%)
Performance:
d 33(pC/N) tg δ (%) ε 33/ ε 0k p(%) Qm Poisson's ratio
129 3.3 720 28.7 196 0.325
Embodiment 10:
Prescription: [0.88Bi 0.5(Na 0.875Li 0.125) 0.5TiO 3+ 0.06BaTiO 3+ 0.06CaTiO 3] (96wt%)+Yb 2O 3(4wt%)
Performance: d 33(pC/N) tg δ (%) ε 33/ ε 0k p(%) Qm Poisson's ratio
143 4.0 747 29.5 135 0.306

Claims (10)

1. bismuth sodium lithium titanate barium titanate strontium titanate calcium titanate based leadless piezoelectric ceramics is at ABO 3The A position is compound ion Bi in the structure 0.5Na 0.5, it is characterized in that A position compound ion Bi 0.5Na 0.5By alkaline-earth metal ions Ba 2+Or Sr 2+Or Ba 2+And Sr 2+The compound ion or the Ba that form 2+And Ca 2+The compound ion or the Ba that form 2+, Sr 2+, Ca 2+The compound ion of forming partly replaces, simultaneously A2 position ion Na +By alkalimetal ion Li +Part replaces the formation leadless piezoelectric ceramics.
2. leadless piezoelectric ceramics as claimed in claim 1 is characterized in that with general formula (1-y-z-u) Bi (1-w)(Na 1-xLi x) wTiO 3+ yBaTiO 3+ zSrTiO 3+ uCaTiO 3Represent 0＜x in the formula＜0.5,0≤y＜1,0≤z＜1,0≤u＜1,0＜(y+z+u)＜1,0.3≤w≤0.7.
3. as the leadless piezoelectric ceramics of claim 1 or 2, it is characterized in that having added one or more doping oxides, hotchpotch content is 0-10wt%, and the content of all the other base material is 90-100wt%, is expressed as (1-y-z-u) Bi with general formula (1-w)(Na 1-xLi x) wTiO 3+ yBaTiO 3+ zSrTiO 3+ uCaTiO 3+ M αO β(wt%), M αO βBe one or more doping oxides, M is for+1-+6 valency and can form the element of solid-oxide with oxygen, as Na, K, Li, Ni, Zn, Cr, Co, Nb, Ta, Al, Cu, Fe, Ce, Pr, Nd, Sm, Gd, Dy, Er, Yb, In, Y, Sc, La, Ho, Lu, Sn, Sb, Mn, Ca, Ba, Sr, Mg, Si.
4. piezoelectric ceramics as claimed in claim 3 is characterized in that with general formula (1-y-z) Bi (1-w)(Na 1-xLi x) wTiO 3+ yBaTiO 3+ zSrTiO 3Or interpolation hotchpotch M αO β(wt%) Biao Shi leadless piezoelectric ceramics, 0＜x in the formula＜0.5,0≤y＜1,0≤z＜1,0＜(y+z)＜1,0.3≤w≤0.7; Hotchpotch is Na 2O or Y 2O 3
5. leadless piezoelectric ceramics as claimed in claim 3 is characterized in that with general formula (1-z-u) Bi (1-w)(Na 1-xLi x) wTiO 3+ zSrTiO 3+ uCaTiO 3+ M αO β(wt%) Biao Shi leadless piezoelectric ceramics, 0＜x in the formula＜0.5,0≤z＜1,0≤u＜1,0＜(z+u)＜1,0.3≤w≤0.7.Hotchpotch M αO βBe La 2O 3+ Fe 2O 3Or Y 2O 3+ La 2O 3
6. piezoelectric ceramics as claimed in claim 3 is characterized in that with general formula (1-y-u) Bi (1-w)(Na 1-xLi x) wTiO 3+ yBaTiO 3+ uCaTiO 3+ M αO β(wt%) represent 0＜x in the formula＜0.5,0≤y＜1,0≤u＜1,0＜(y+u)＜1,0.3≤w≤0.7; Hotchpotch M αO βBe Nb 2O 5Or Yb 2O 3
7. leadless piezoelectric ceramics as claimed in claim 3 is characterized in that by composition formula [0.87Bi 0.5(Na 0.925Li 0.075) 0.5TiO 3+ 0.06BaTiO 3+ 0.01SrTiO 3+ 0.06CaTiO 3] (97wt%)+Li 2O (1wt%)+Y 2O 3(2wt%) or [0.84Bi 0.5(Na 0.925Li 0.075) 0.5TiO 3+ 0.08BaTiO 3+ 0.02SrTiO 3+ 0.06CaTiO 3] (97wt%)+Li 2O (1wt%)+Fe 2O 3(2wt%) material of expression constitutes.
8. leadless piezoelectric ceramics as claimed in claim 4 is characterized in that by composition formula 0.92Bi 0.6(Na 0.90Li 0.10) 0.4TiO 3+ 0.06BaTiO 3+ 0.02SrTiO 3Or 0.94Bi 0.5(Na 0.90Li 0.10) 0.5TiO 3+ 0.04BaTiO 3+ 0.02SrTiO 3Or [0.90Bi 0.4(Na 0.925Li 0.075) 0.6TiO 3+ 0.06BaTiO 3+ 0.04SrTiO 3] (98wt%)+Na 2O (2wt%) or [0.92Bi 0.5(Na 0.9Li 0.1) 0.5TiO 3+ 0.06BaTiO 3+ 0.02SrTiO 3] (98%)+Y 2O 3(2%) material of expression constitutes.
9. leadless piezoelectric ceramics as claimed in claim 5 is characterized in that by composition formula [0.81Bi 0.5(Na 0.90Li 0.10) 0.5TiO 3+ 0.13SrTiO 3+ 0.06CaTiO 3] (93wt%)+La 2O 3(4wt%)+Fe 2O 3(3wt%) or [0.80Bi 0.5(Na 0.925Li 0.075) 0.5TiO 3+ 0.15SrTiO 3+ 0.05CaTiO 3] (93wt%)+La 2O 3(4wt%)+Y 2O 3(3wt%) material of expression constitutes.
10 leadless piezoelectric ceramicss as claimed in claim 6 is characterized in that by composition formula [0.80Bi 0.5(Na 0.90Li 0.10) 0.5TiO 3+ 0.12BaTiO 3+ 0.08CaTiO 3] (96wt%)+Nb 2O 5(4wt%) or [0.88Bi 0.5(Na 0.875Li 0.125) 0.5TiO 3+ 0.06BaTiO 3+ 0.06CaTiO 3] (96wt%)+Yb 2O 3(4wt%) material of expression constitutes.
CN 200310110879 2003-11-07 2003-11-07 Bismuth sodium lithium titanate barium titanate strontium titanate calcium titanate based lead-free piezoelectric ceramics Expired - Fee Related CN1260170C (en)

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