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CN102249659B - Bismuth ferrite-based leadless piezoelectric ceramic with high Curie temperature and preparation method thereof - Google Patents

Bismuth ferrite-based leadless piezoelectric ceramic with high Curie temperature and preparation method thereof Download PDF

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CN102249659B
CN102249659B CN201110162432A CN201110162432A CN102249659B CN 102249659 B CN102249659 B CN 102249659B CN 201110162432 A CN201110162432 A CN 201110162432A CN 201110162432 A CN201110162432 A CN 201110162432A CN 102249659 B CN102249659 B CN 102249659B
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preparation
piezoelectric ceramics
curie temperature
leadless piezoelectric
ceramic
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CN102249659A (en
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周昌荣
岑侦勇
周沁
杨华斌
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 bismuth ferrite-based leadless piezoelectric ceramic with high Curie temperature and a preparation method thereof. The general formula for the piezoelectric ceramic is (1-x-y)(Bi1-z Mz)t(FeuM'1-u)O3-xBaTiO3-yBiMnO3, wherein, M is a trivalent metallic element with large ionic radius, M' is a trivalent metallic element with small ionic radius, and x, y, u, t and z represent mole content in a ceramic system and satisfy the following relations: 0<=x<=1.0, 0<=y<=0.1, 0<z<1, 0.85<t<1.2, 0<u<1 and x+y<1. The piezoelectric ceramic is prepared by a conventional ceramic preparation method through selection of proper technological parameters. The piezoelectric constant d33 of the ceramic can reach 140 pC/N, and Curie temperature can reach 490 DEG C. The preparation method has the advantages of a simple and stable process, and obtained leadless piezoelectric ceramic has excellent performance and is suitable for being used under high temperature.

Description

A kind of high-curie temperature ferrous acid bismuth base lead-free piezoelectric ceramics and preparation method thereof
Technical field
The present invention relates to lead-free piezoceramic material, specifically is the ABO of a kind of A, the compound substituting modification in B position 3High-curie temperature ferrous acid bismuth base lead-free piezoelectric ceramics of calcium titanium ore structure and preparation method thereof.
Background technology
The high-temperature piezoelectric pottery is widely used in many special dimensions such as aerospace, nuclear energy, metallurgy, petrochemical complex, geological prospecting; Such as the dynamic fuel injection nozzle operation temperature of in automobile, working up to 300 ℃; The sound wave well logging transducer working temperature that oil well uses down also reaches 200 ~ 300 ℃; As the high-temperature piezoelectric stupalith, must possess under comparatively high temps (> 400 ℃) structural phase transition does not appear to guarantee high temperature umpolarization phenomenon not taking place and the temperature stability of deterioration piezoelectric device.But at present the high-curie temperature piezoelectric ceramic of commercial applications is still with Pb-based lanthanumdoped zirconate titanates Pb (Zr, Ti) O of calcium titanium ore structure 3(being abbreviated as PZT) system is main, and the Tc of this type material is about degree more than 400, because the hot activation weathering process, its safe handling temperature is limited in 1/2 place of Tc, only is suitable for using under the normal condition.And plumbous oxide content accounts for about 70% in these materials, the preparation, use and discarded last handling process in all can bring serious harm to human environment.Therefore, from the condition of environmental protection and high temperature use, the high curie temperature leadless piezoelectric ceramal material of research and development excellent property is a problem that great society and economic implications are arranged.
In the leadless piezoelectric ceramics system of the alternative lead base high-curie temperature of studying at present, (the Na of calcium titanium ore structure 1/2Bi 1/2) TiO 3-(K 1/2Bi 1/2) TiO 3(being called for short NBT-BKT) is a kind of leadless piezoelectric material material that gets a good chance of, and its Tc is about 320 ℃.Another calcium titanium ore structure leadless piezoelectric ceramics is with K 0.5Na 0.5NbO 3(being called for short KNN) is main, and the Tc of pure KNN can reach 400 oMore than the C, but this system volatile and very difficult fine and close difficulty when having sintering.In order to improve piezoelectric property and compactness, through adding LiSbO 3Deng, simultaneously through adding BiFeO 3Etc. the low-temperature sintering auxiliary agent, can improve sintering character and piezoelectric property, make d 33Reach about 300pC/N, but LiSbO 3Adding, make Curie temperature drop to 370 again oAbout C, the KNN pottery of the template grain growth utilized technology preparation is also arranged, d 33Can reach more than the 400pC/N, but complex manufacturing that should technology, cost is very high, is not suitable for suitability for industrialized production.Over the past two years to BiAlO 3The high-temp leadless piezoelectric ceramics of system also has a lot of researchs, but still has preparation difficulty, the problem that piezoelectric property is lower.Other unleaded high-curie temperature systems also comprise blue steel structure leadless piezoelectric ceramics and bismuth laminated leadless piezoelectric ceramic or the like, but all there is the very low problem of piezoelectric constant in these systems, can't satisfy the demand of actual use.
Reported BiFeO in 2009 by people such as Serhiy 3– BaTiO 3The based perovskite ferroelectrics, through sintering in pure oxygen, the leadless piezoelectric ceramics of preparation, its Tc is up to 600 oC is considered to a kind of high-curie temperature leadless piezoelectric material material that gets a good chance of.But its piezoelectric constant d 33The highest have only 116pC/N, and its must be in purity oxygen sintering, preparation technology is complicated, also there is a big difference in its performance distance practical application, therefore studies new BiFeO 3Based leadless piezoelectric ceramics is significant.Therefore see from the angle of investigation of materials, can pass through A and B position selectivity control performance, at the BiFeO of better performances 3– BaTiO 3The ABO that is constituted 3In the type calcium titanium ore structure, be a kind of effective way through recently improving piezoelectric property and improve preparation technology in A, the compound substituting modification in B position and nonstoichiometry.
But, at present at BiFeO 3– BaTiO 3– BiMnO 3In also do not appear in the newspapers through leadless piezoelectric ceramics of recently improving piezoelectric property and improve preparation technology in A, the compound substituting modification in B position and nonstoichiometry and preparation method thereof.
Summary of the invention
The purpose of this invention is to provide high (Tc>=490 of a kind of Tc oC), be easy to polarization, novel ferrous acid bismuth base lead-free piezoelectric ceramics that density is high, piezoelectric property is good and preparation method thereof.
The object of the invention technical scheme is: at BiFeO 3– BaTiO 3– BiMnO 3Through recently improving piezoelectric property and improve preparation technology, can use general formula (1-in the leadless piezoelectric ceramics that constitutes in A, the compound substituting modification in B position and nonstoichiometry x- y) (Bi zM 1-z) t(Fe uM ' 1-u) O 3– xBaTiO 3– yBiMnO 3Represent.M is trivalent metallic element (a heavy ion radius) in the formula, be selected from Nd, Ce, La, Pr, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Y, Er and Tm one or both and more than.M ' is trivalent metallic element (a small ion radius), be selected from Ga, Sc, Cr, Mo, Al, Mn, Co, Rh, Ni, Cu, In, Yb and Sb one or both and more than. x, y, u, t , zMolar content in the expression ceramic systems, wherein 0≤ x≤1.0,0≤ y≤0.1,0< z<1,0.85<t<1.2,0< u<1, x+ y<1.At least contain two or more substituted element in the prescription.The preparation method of described leadless piezoelectric ceramics is characterized in that comprising the steps:
(1) with raw material according to chemical formula (1- x- y) (Bi zM 1-z) t(Fe uM ' 1-u) O 3– xBaTiO 3– yBiMnO 3Preparing burden, is medium high-energy ball milling 8-10 hour with the absolute ethyl alcohol, dry back in alumina crucible (adding a cover) with 850-900 ° of C roasting 1-6 hour; When being medium high-energy ball milling 12-24 with the absolute ethyl alcohol after the roasting, dry back obtains powder;
(2) the powder oven dry that step (1) is obtained, the PVA solution granulation of adding 5% (weight percent) concentration is in the moulding of 100MPa pressure pressed;
(3) with the sintering in air of the biscuit after the moulding, the speed of 200 ℃/h is warming up to 800 ℃ of insulations 1-6 hour, and the speed with 100-300 ℃/h is warmed up to 950-1000 ℃ of insulation 2-8 hour again; With the rate of cooling to 900 of 10-120 ℃/h ℃ insulation 2-8 hour, cool to 600 ℃ of insulations 2-8 hour again with the furnace behind the sintering, cool to room temperature subsequently with the furnace;
(4) 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, in silicone oil, polarizes polarized electric field 3000-8000V/mm, temperature 30-60 then °C, time 5-30 minute.
Compared with present technology, characteristic of the present invention is embodied in:
1. it is a kind of environmentally friendly piezoelectric ceramics that pottery of the present invention is formed, and can realize alternative to the existing lead base piezoelectric ceramics of part, and its Curie temperature can reach more than 490 ℃.
2. with original compared with techniques, the present invention adopts sintering in the air, can simplify sintering process, reduces production costs.
3. compare with original prescription, the leadless piezoelectric ceramics of present method preparation has better properties, the piezoelectric constant d of this system 33Can reach more than the 140pC/N, planar electromechanical coupling factor kp can reach 0.30, K tCan reach more than 0.50.
4, the present invention can adopt the conventional piezoelectric ceramics processing, and raw material obtains from industrial raw material, and preparation technology is simple, stable, need not add specific installation, can be in factory direct production, have practicality.
Embodiment
Embodiment 1:
Prepared composition is: (1- x- y) (Bi zM 1-z) t(Fe uM ' 1-u) O 3– xBaTiO 3– yBiMnO 3, wherein x=0.33, y=0.008, z=0.004, u=0.004, M=70%La+30%Nd, M '=50%Al+50%Yb, the high-curie temperature ferrous acid bismuth base lead-free piezoelectric ceramics of t=1.08.
The preparation method:
With analytical pure Bi 2O 3, Fe 2O 3, BaCO 3, TiO 2, MnO 2, Nd 2O 3, Yb 2O 3, La 2O 3And Al 2O 3Be raw material, respectively according to following chemical formula:
(1- x- y) (Bi zM 1-z) t(Fe uM ' 1-u) O 3– xBaTiO 3– yBiMnO 3, wherein x=0.33, y=0.008, z=0.004, u=0.004, M=70%La+30%Nd, M '=50%Al+50%Yb, t=1.08
Prepare burden, absolute ethyl alcohol is the medium wet-milling, synthesizes porcelain in 3-6 hour in advance 850-900 ° of C insulation after 80 ℃ of oven dry; The synthetic porcelain is medium secondary wet-milling 24 hours with the absolute ethyl alcohol; 250 mesh sieves are crossed in the oven dry back; The PVA solution that adds 5% concentration then is as sticker, presses down at 100MPa pressure and processes diameter 18 mm, the disk of thickness 1.1 ~ 1.2mm; With the temperature rise rate to 800 of 200 ℃/h ℃ insulation 3 hours, the speed with 100 ℃/h was warmed up to 970 ℃ of insulations 5 hours again; With the rate of cooling to 900 of 50 ℃/h ℃ insulation 8 hours, cool to 600 ℃ of insulations 6 hours again with the furnace behind the sintering, cool to room temperature subsequently with the furnace.The two-sided silver that drapes over one's shoulders polarizes in 60 ℃ of silicone oil behind the silver ink firing, and polarized electric field is 5 kV/mm, and the polarization time is 15 min, removes electric field after the maintenance electric field is cooled to room temperature, takes out sample.Again the piezoelectric ceramics of processing being carried out piezoelectric property measures.
Results of property is following:
d 33(pC/N) Q m kp εr T c（℃） tanδ(%)
143 56 0.33 691.7 495 4.90
Embodiment 2:
Prepared composition is (1- x- y) (Bi zM 1-z) t(Fe uM ' 1-u) O 3– xBaTiO 3– yBiMnO 3, its x=0.30, y=0.008, z=0.007, u=0.007, M=60%Y+40%Dy, M '=50Ga%+50%Sc, the high-curie temperature ferrous acid bismuth base lead-free piezoelectric ceramics of t=1.05.
The preparation method:
With analytical pure Bi 2O 3, Fe 2O 3, BaCO 3, TiO 2, MnO 2, Dy 2O 3, Sc 2O 3, Ga 2O 3, Y 2O 3And Al 2O 3Be raw material, respectively according to following chemical formula:
(1- x- y) (Bi zM 1-z) t(Fe uM ' 1-u) O 3– xBaTiO 3– yBiMnO 3, wherein x=0.30, y=0.008, z=0.007, u=0.007, M=60%Y+40%Dy, M '=50Ga%+50%Sc, t=1.05.
Preparing burden, is the medium wet-milling with the absolute ethyl alcohol, synthesizes porcelain in 3-6 hour in advance 850-900 ℃ of insulation after 80 ℃ of oven dry; The synthetic porcelain is medium secondary wet-milling 24 hours with the absolute ethyl alcohol; 250 mesh sieves are crossed in the oven dry back; The PVA solution that adds 5% concentration then is as sticker, presses down at 100MPa pressure and processes diameter 18 mm, the disk of thickness 1.1 ~ 1.2mm; With the temperature rise rate to 800 of 200 ℃/h ℃ insulation 2 hours, the speed with 100 ℃/h was warmed up to 1000 ℃ of insulations 5 hours again; With the rate of cooling to 900 of 20 ℃/h ℃ insulation 8 hours, cool to 600 ℃ of insulations 6 hours again with the furnace behind the sintering, cool to room temperature subsequently with the furnace.The two-sided silver that drapes over one's shoulders polarizes in 60 ℃ of silicone oil behind the silver ink firing, and polarized electric field is 5 kV/mm, and the polarization time is 15 min, removes electric field after the maintenance electric field is cooled to room temperature, takes out sample.It is following again the piezoelectric ceramics of processing to be carried out the piezoelectric property measuring result:
d 33(pC/N) Q m kp εr T c（℃） tanδ(%)
137 58 0.28 686 490 5.80
Embodiment 3:
Prepared composition is (1-x-y) (Bi zM 1-z) t(Fe uM ' 1-u) O 3– xBaTiO 3– yBiMnO 3, x=0.33 wherein, y=0.008, z=0.006, u=0.006, M=70%Sm+30%Nd, M '=In, the high-curie temperature ferrous acid bismuth base lead-free piezoelectric ceramics of t=1.03.
The preparation method:
With analytical pure Bi 2O 3, Fe 2O 3, BaCO 3, TiO 2, MnO 2, Dy 2O 3, Sc 2O 3, Ga 2O 3, Y 2O 3And Al 2O 3Be raw material, respectively according to following chemical formula:
(1-x-y) (Bi zM 1-z) t(Fe uM ' 1-u) O 3– xBaTiO 3– yBiMnO 3, x=0.33 wherein, y=0.008, z=0.006, u=0.006, M=70%Sm+30%Nd, M '=In, t=1.03.
Preparing burden, is the medium wet-milling with the absolute ethyl alcohol, synthesizes porcelain in 3-6 hour in advance 850-900 ℃ of insulation after 80 ℃ of oven dry; The synthetic porcelain is medium secondary wet-milling 24 hours with the absolute ethyl alcohol; 250 mesh sieves are crossed in the oven dry back; The PVA solution that adds 5% concentration then is as sticker, presses down at 100MPa pressure and processes diameter 18 mm, the disk of thickness 1.1 ~ 1.2mm; With the temperature rise rate to 800 of 200 ℃/h ℃ insulation 2 hours, the speed with 100 ℃/h was warmed up to 975 ℃ of insulations 4 hours again; With the rate of cooling to 900 of 20 ℃/h ℃ insulation 8 hours, cool to 600 ℃ of insulations 6 hours again with the furnace behind the sintering, cool to room temperature subsequently with the furnace.The two-sided silver that drapes over one's shoulders polarizes in 60 ℃ of silicone oil behind the silver ink firing, and polarized electric field is 5 kV/mm, and the polarization time is 15 min, removes electric field after the maintenance electric field is cooled to room temperature, takes out sample.It is following again the piezoelectric ceramics of processing to be carried out the piezoelectric property measuring result:
d33(pC/N) Qm kp εr Tc（℃） tanδ(%)
113 57 0.32 642 490 5.32
Embodiment 4:
Prepared composition is (1-x-y) (Bi zM 1-z) t(the O of FeuM ' 1-u) 3– xBaTiO 3– yBiMnO 3, x=0.33 wherein, y=0.008, z=0.004; U=0.004, M=70%La+30%Nd, M '=50%Al+50%Yb; Is the high-curie temperature ferrous acid bismuth base lead-free piezoelectric ceramics of t=1.08 1000 ℃ except that sintering temperature among the preparation method, (different with which of embodiment 1)? Other is with embodiment 1.
Test performance is following:
d33(pC/N) Qm kp εr Tc（℃） tanδ(%)
103 48 0.37 631 495 4.37
Embodiment 5:
The composition expression formula is with embodiment 1:
Prepared composition: (1-x-y) (Bi zM 1-z) t(Fe uM ' 1-u) O 3– xBaTiO 3– yBiMnO 3
X=0.33, y=0.008, z=0.004, u=0.004, M=70%La+30%Nd, M '=50%Al+50%Yb, the high-curie temperature ferrous acid bismuth base lead-free piezoelectric ceramics of t=1.08.
Be 950 ℃ except that sintering temperature among the preparation method, other is with embodiment 1,
Test performance is following:
d33(pC/N) Qm kp εr Tc（℃） tanδ(%)
101 68 0.24 611 485 5.81

Claims (4)

1. high-curie temperature ferrous acid bismuth base lead-free piezoelectric ceramics is characterized in that: forming general formula is: (1-x-y) (BizM1-z) t (O of FeuM ' 1-u) 3– xBaTiO 3– yBiMnO 3, M is the trivalent metallic element of heavy ion radius in the formula, and M ' is the trivalent metallic element of small ion radius, and x, y, u, t, z represent molar content in the ceramic systems, wherein 0≤x≤1.0,0≤y≤0.1,0<z<1,0.85<t<1.2,0<u<1, x+y<1, be prepared from through conventional ceramic preparation.
2. leadless piezoelectric ceramics as claimed in claim 1 is characterized in that: more than one or both that described trivalent element M is La, Nd, Ce, Y, Pr, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er and Tm reach.
3. leadless piezoelectric ceramics as claimed in claim 1 is characterized in that: described trivalent element M ' be Ga, Sc, Cr, Mo, Mn, Co, Rh, Ni, Cu, In, Al, Yb and Sb one or both and more than.
4. like the preparation method of the described leadless piezoelectric ceramics of one of claim 1-3, comprise wet-milling, dry, burn till porcelain, ball milling, bonding are pressed into disk sintering in disk, the air, sand milling, two-sidedly drape over one's shoulders silver, polarization for the second time, it is characterized in that:
(1) sintered wafer is warming up to 800 ℃ of insulations 1-6 hour with the speed of 200 ℃/h in the air, and the speed with 100-300 ℃/h is warmed up to 950-1000 ℃ of insulation 2-8 hour again;
(2) behind the agglomerating disk sintering with the rate of cooling to 900 of 10-120 ℃/h ℃ insulation 2-8 hour, cool to 600 ℃ of insulations 2-8 hour again with the furnace, cool to room temperature subsequently with the furnace.
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