CN101717251B - Modified lead titanate piezoelectric ceramic material and preparation method thereof - Google Patents
Modified lead titanate piezoelectric ceramic material and preparation method thereof Download PDFInfo
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- CN101717251B CN101717251B CN2009102422115A CN200910242211A CN101717251B CN 101717251 B CN101717251 B CN 101717251B CN 2009102422115 A CN2009102422115 A CN 2009102422115A CN 200910242211 A CN200910242211 A CN 200910242211A CN 101717251 B CN101717251 B CN 101717251B
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- piezoelectric ceramic
- lead titanate
- modified lead
- titanate piezoelectric
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Abstract
The invention discloses a modified lead titanate piezoelectric ceramic material, which takes Pb0.88 (La0.6Nd0.4) 0.08 (Mn1/3Sb2/3) 0.02Ti0.9803 system as a substrate, and Co203 as a doped oxide, wherein the doped amount of Co2O3 is 0.15 to 0.85 mass percent of the substrate. The invention also discloses a method for preparing the modified lead titanate piezoelectric ceramic material, which comprises the following steps of batching, mixing, roll forming, plastic removing and sintering the Pb0.88 (La0.6Nd0.4) 0.08 (Mn1/3Sb2/3) 0.02Ti0.9803 system serving as a substrate and the Co203. The piezoelectric ceramic material prepared by the invention has high Curie temperature and can meet the requirements on a lead-free welding process (such as reflow soldering); meanwhile piezoelectric coefficient d33 can reach 72 to 78 Pc/N, mechanical quality factor Qm can reach 2,000 to 2,200, and thickness mode electromechanical coupling coefficient kt can reach 42 to 49 percent; and application requirements on lead components, such as a high frequency device, a resonator, a filter and the like are met.
Description
Technical field
The present invention relates to a kind of modified lead titanate piezoelectric ceramic material and preparation method thereof, belong to the ceramic material field.
Background technology
The piezoelectricity ferro pottery has good ferroelectricity, piezoelectricity, dielectricity, pyroelectricity property etc.; Be to use one type very widely in the function ceramics; Like storer (ferroelectricity application), transmitter, transverter, wave filter (piezoelectricity application), infrared eye (pyroelectricity application), electrical condenser (dielectricity application) etc.; In national economy and national defense industry, play an important role, formed the mass-producing industry.Wherein lead titanate ceramics have good piezoelectric property, and through various replacements and adulterated mode, people have overcome the sintering difficulty, have obtained some and have been widely used in the prescription of different field, especially in the high frequency field, because PbTiO
3Pottery has thickness triple-frequency harmonics characteristic preferably, on high-frequency reonsator, wave filter lead elements and production method thereof, is widely used.Because weldprocedure is unleaded, welding temperature is brought up to 250~280 ℃ (like Reflow Solderings), and this Tc to element material is had higher requirement.Present domestic industry practicability PbTiO
3The Tc T of pottery
CNot high, the practicability PbTiO of industrially-advanced country such as Japan
3The ceramic T of base
CAbout 310 ℃, and China practicability PbTiO
3Pottery T
CAbout 250~270 ℃.Lower T
CHad a strong impact on PbTiO
3The application of pottery.Therefore, obtain high Tc T
C(>℃ 300C) and high mechanical quality factor Q
mPbTiO
3Pottery for the requirement of satisfying ceramic welding technology, improves the piezoelectric ceramics serviceability, and is with practical value.
Summary of the invention
The objective of the invention is; A kind of modified lead titanate piezoelectric ceramic material and preparation method thereof is provided; Selection has the foundational system of high-curie temperature; Under the prerequisite of dielectric properties that keep pottery as far as possible and piezoelectric property,, make lead titanate ceramics be adapted to new process environments through the mechanical quality factor of oxide-doped raising stupalith.
A kind of modified lead titanate piezoelectric ceramic material of the present invention is characterized in that with Pb
0.88(La
0.6Nd
0.4)
0.08(Mn
1/3Sb
2/3)
0.02Ti
0.98O
3System is a matrix, C0
2O
3Be doping oxide;
Modified lead titanate piezoelectric ceramic of the present invention is characterized in that Co
2O
3Doping is the 0.15-0.85% mass ratio of matrix;
The preparation method of a kind of modified lead titanate piezoelectric ceramic material of the present invention is characterized in that adopting solid sintering technology to burn till porcelain body, may further comprise the steps:
(1) adopting tri-lead tetroxide, lanthanum sesquioxide, neodymium sesquioxide, manganous carbonate, Antimony Trioxide: 99.5Min, titanium oxide is basic raw material, by molecular formula Pb
0.88(La
0.6Nd
0.4)
0.08(Mn
1/3Sb
2/3)
0.02Ti
0.98O
3Join and get basic raw material; With Co
2O
3Material joins in the basic material Co as mixing
2O
3The mass percent that accounts for basic material is 0.15~0.85%;
(2) adopting water is medium, and with raw material ball milling 8~12 hours, discharging and dry back were squeezed into piece with the pressure of 30~50MPa with raw material, is raised to the temperature rise rate of 1~3 ℃/min and carries out syntheticly in advance under 850~900 ℃, is incubated 1~3 hour; The synthetic in advance material piece that obtains is ground to all through 40 mesh sieves; Be medium, ball milling 8~12 hours once more with the absolute ethyl alcohol, discharging is also dry; Add the binder solution (the Z 150PH mass concentration is 18% in the solution) of the mass percent 20% that accounts for powder in the powder,, obtain the diaphragm that thickness is 0.3~0.5mm through batch mixing and material, roughing and finish rolling.
(3) diaphragm is incubated 2~4 hours plastic removals down at 720~750 ℃, and temperature rise rate is 1~5 ℃/min; Then diaphragm is placed alumina crucible, airtight sintering, sintering temperature is 1170~1260 ℃, soaking time is 1~3 hour, promptly gets ceramic plate.
(4) ceramic plate lining silver electrode in two sides behind grinding and polishing, and 80~120 ℃ of polarization down in silicone oil, polarized electric field is 6000~8000V/mm, the time is 45~60 minutes.
This matrix is mixing Co
2O
3Back variable density is very little, keeps good sintering character.1230 ℃ of agglomerating Pb
0.88(La
0.6Nd
0.4)
0.08(Mn
1/3Sb
2/3)
0.02Ti
0.98O
3The sintered density and the Co of pottery
2O
3The relation of doping referring to Fig. 1, can find out that by figure this system is being mixed Co from figure
2O
3Back variable density is very little, keeps good sintering character.
The piezoceramic material that utilizes method provided by the invention to obtain has high Tc (320~330 ℃), can satisfy the requirement of pb-free solder technology (like Reflow Soldering), simultaneously, and piezoelectric coefficient d
33Can reach 72~78pC/N, the mechanical quality factor Q
mCan reach 2000~2200, thickness mode electromechanical coupling factor k
tCan reach 42~49%, meet the high frequency frequency device, like lead elements and production method thereof application requiring such as resonator, wave filters.
Description of drawings
Fig. 1 is 1230 ℃ of agglomerating Pb
0.88(La
0.6Nd
0.4)
0.08(Mn
1/3Sb
2/3)
0.02Ti
0.98O
3The sintered density and the Co of pottery
2O
3The relation of doping.
Embodiment
Further illustrate substantive distinguishing features of the present invention and remarkable advantage below by embodiment.Be noted that the present invention only is confined to the embodiment that is stated by no means.
Comparative Examples
(1) adopting tri-lead tetroxide, lanthanum sesquioxide, neodymium sesquioxide, manganous carbonate, Antimony Trioxide: 99.5Min, titanium oxide is raw material, by molecular formula Pb
0.88(La
0.6Nd
0.4)
0.08(Mn
1/3Sb
2/3)
0.02Ti
0.98O
3Join and get basic raw material
(2) adopting water is medium, and raw material roughly grind in ball grinder 8 hours, and discharging and dry back are squeezed into piece with the pressure of 30MPa with powder, is raised to the temperature rise rate of 3 ℃/min and carries out under 850 ℃ synthesizing in advance, is incubated 2 hours; The synthetic in advance material piece that obtains is ground to 40 mesh sieves; Be the fine grinding 12 hours in ball grinder of medium, material piece with the absolute ethyl alcohol, discharging is also dry; Add the binder solution (polyvinyl alcohol concentration is 18%) of the mass percent 20% that accounts for powder in the powder,, obtain the diaphragm that thickness is 0.5mm through batch mixing and material, roughing and finish rolling.
(3) diaphragm insulation under 720 ℃ was carried out plastic removal in 4 hours, and temperature rise rate is 2 ℃/min; Then diaphragm is placed alumina crucible, airtight sintering, sintering temperature is 1230 ℃, soaking time is 2 hours, promptly gets ceramic plate;
(4) ceramic plate lining silver electrode in two sides behind grinding and polishing, and 110 ℃ of polarization down in silicone oil, polarized electric field is 7000V/mm, the time is 50 minutes.Its performance is seen table 1.
Embodiment 1
(1) adopting tri-lead tetroxide, lanthanum sesquioxide, neodymium sesquioxide, manganous carbonate, Antimony Trioxide: 99.5Min, titanium oxide is raw material, by molecular formula Pb
0.88(La
0.6Nd
0.4)
0.08(Mn
1/3Sb
2/3)
0.02Ti
0.98O
3Join and get basic raw material; With Co
2O
3Material joins in the basic material Co as mixing
2O
3The mass percent that accounts for basic material is 0.45%;
The same Comparative Examples of other conditions.Its performance is seen table 1.
Embodiment 2
(1) adopting tri-lead tetroxide, lanthanum sesquioxide, neodymium sesquioxide, manganous carbonate, Antimony Trioxide: 99.5Min, titanium oxide is raw material, by molecular formula Pb
0.88(La
0.6Nd
0.4)
0.08(Mn
1/3Sb
2/3)
0.02Ti
0.98O
3Join and get basic raw material; With Co
2O
3Material joins in the basic material Co as mixing
2O
3The mass percent that accounts for basic material is 0.65%;
The same Comparative Examples of other conditions.Its performance is seen table 1.
Table 1 is following by the performance comparison table test condition of the ceramics sample of Comparative Examples, embodiment 1 and 2 preparations:
Volume density is pressed the Archimedes drainage and is adopted Metler XS104 type precise electronic balance measurement;
Specific inductivity and dielectric loss: under the frequency of 1kHz, use the accurate LCR table of Agilent E4980 type to measure electric capacity and dielectric loss, and pass through formula
Calculate specific inductivity (C: capacitance, t: diaphragm thickness; A: membrance electrode area; ε
0: permittivity of vacuum).
Piezoelectric strain constant d
33: adopt ZJ-2A type quasistatic d
33Appearance is measured;
Plane mode electromechanical coupling factor k
p: resonance and anti-resonance frequency under the flexible pattern in plane of the accurate electric impedance analyzer measuring diaphragm of employing Agilent 4294A type, and by formula
Calculate.
Thickness mode electromechanical coupling factor k
t: resonance and anti-resonance frequency under the flexible pattern of thickness of the accurate electric impedance analyzer measuring diaphragm of employing Agilent 4294A type, by formula
Calculate.
The mechanical quality factor Q
m: resonance and antiresonance impedance and frequency under the flexible pattern in plane of the accurate electric impedance analyzer measuring diaphragm of employing Agilent 4294A type, and by formula
Calculate.
Tc T
C: utilize the corresponding curve of specific inductivity that the Agilent E4980 of supporting GW-I type high temperature service (Xi'an Communications University's system) measures and temperature, confirm the Tc T of pottery according to the temperature of specific inductivity maximum on the curve
C
Embodiment 3
(1) adopting tri-lead tetroxide, lanthanum sesquioxide, neodymium sesquioxide, manganous carbonate, Antimony Trioxide: 99.5Min, titanium oxide is raw material, by molecular formula Pb
0.88(La
0.6Nd
0.4)
0.08(Mn
1/3Sb
2/3)
0.02Ti
0.98O
3Join and get basic raw material; With Co
2O
3Material joins in the basic material Co as mixing
2O
3The mass percent that accounts for basic material is 0.15%;
(2) adopting water is medium, and raw material ball milling 12 hours presses down at 50MPa after the discharging drying and processes piece, and synthesis temperature is 900 ℃ in advance, and temperature rise rate is 1 ℃/min, is incubated 1 hour.The material piece is ball milling 10 hours once more, obtains powder.
(3) plastic removal was carried out in diaphragm insulation under 740 ℃ in 3 hours.Sintering temperature is 1170 ℃, and soaking time is 3 hours.
(4) polarized electric field 8000V/mm, 120 ℃ of polarization temperature, the same Comparative Examples of other condition of polarization time 60min.
This embodiment sample d
33=68pC/N, k
t=38%, Q
m=1053.
Embodiment 4
(1) adopting tri-lead tetroxide, lanthanum sesquioxide, neodymium sesquioxide, manganous carbonate, Antimony Trioxide: 99.5Min, titanium oxide is raw material, by molecular formula Pb
0.88(La
0.6Nd
0.4)
0.08(Mn
1/3Sb
2/3)
0.02Ti
0.98O
3Join and get basic raw material; With Co
2O
3Material joins in the basic material Co as mixing
2O
3The mass percent that accounts for basic material is 0.75%;
(2) adopting water is medium, and raw material ball milling 10 hours presses down at 40MPa after the discharging drying and processes piece, and synthesis temperature is 880 ℃ in advance, be incubated 3 hours, synthesizes the material piece that obtains in advance and is ground to 40 mesh sieves; Be the fine grinding 8 hours in ball grinder of medium, material piece with the absolute ethyl alcohol, discharging is also dry; Add the powder of sticker,, obtain the diaphragm that thickness is 0.3mm through batch mixing and material, roughing and finish rolling.
(3) diaphragm carries out plastic removal under 730 ℃.Sintering temperature is 1200 ℃, and soaking time is 1 hour
(4) polarized electric field 6000V/mm, 100 ℃ of polarization temperature, polarization time 45min.The same Comparative Examples of other condition.
This embodiment sample d
33=76pC/N, k
t=42%, Q
m=1681
Embodiment 5
(1) adopting tri-lead tetroxide, lanthanum sesquioxide, neodymium sesquioxide, manganous carbonate, Antimony Trioxide: 99.5Min, titanium oxide is raw material, by molecular formula Pb
0.88(La
0.6Nd
0.4)
0.08(Mn
1/3Sb
2/3)
0.02Ti
0.98O
3Join and get basic raw material; With Co
2O
3Material joins in the basic material Co as mixing
2O
3The mass percent that accounts for basic material is 0.3%;
(2) powder presses down at 50MPa and processes piece, and synthesis temperature is 850 ℃ in advance, and temperature rise rate is 2 ℃/min, is incubated 1 hour.
(3) diaphragm insulation under 750 ℃ was carried out plastic removal in 3 hours, and temperature rise rate is 5 ℃/min; Sintering temperature is 1260 ℃, and soaking time is 2 hours.
(4) polarized electric field 7000V/mm, 80 ℃ of polarization temperature, polarization time 50min.
The same Comparative Examples of other condition.
This embodiment sample d
33=73pC/N, k
t=45%, Q
m=1642
Embodiment 6
(1) adopting tri-lead tetroxide, lanthanum sesquioxide, neodymium sesquioxide, manganous carbonate, Antimony Trioxide: 99.5Min, titanium oxide is raw material, by molecular formula Pb
0.88(La
0.6Nd
0.4)
0.08(Mn
1/3Sb
2/3)
0.02Ti
0.98O
3Join and get basic raw material; With Co
2O
3Material joins in the basic material Co as mixing
2O
3The mass percent that accounts for basic material is 0.85%;
(2) powder presses down at 50MPa and processes piece, and synthesis temperature is 850 ℃ in advance.
(3) diaphragm insulation under 750 ℃ was carried out plastic removal in 2 hours, and temperature rise rate is 1 ℃/min; Sintering temperature is 1230 ℃, and soaking time is 2 hours
(4) polarized electric field 6000V/mm, 90 ℃ of polarization temperature, polarization time 50min.
The same Comparative Examples of other condition.
This embodiment sample d
33=76pC/N, k
t=45%, Q
m=2073
The performance comparison of table 1 Comparative Examples and embodiment 1,2
Claims (4)
1. a modified lead titanate piezoelectric ceramic material is characterized in that with Pb
0.88(La
0.6Nd
0.4)
0.08(Mn
1/3Sb
2/3)
0.02Ti
0.98O
3System is a matrix, with Co
2O
3Add in the matrix Co as doping oxide
2O
3Doping is the 0.15-0.85% mass ratio of matrix.
2. a method for preparing modified lead titanate piezoelectric ceramic is characterized in that, may further comprise the steps:
(1) adopting tri-lead tetroxide, lanthanum sesquioxide, neodymium sesquioxide, manganous carbonate, Antimony Trioxide: 99.5Min, titanium oxide is raw material, by molecular formula Pb
0.88(La
0.6Nd
0.4)
0.08(Mn
1/3Sb
2/3)
0.02Ti
0.98O
3Join and get basic raw material; With Co
2O
3Material joins in the basic material Co as mixing
2O
3The mass percent that accounts for basic material is 0.15~0.85%;
(2) adopting water is medium ball milling 8~12 hours, and discharging and dry back are squeezed into piece with the pressure of 30~50MPa with powder, is raised to the temperature rise rate of 1~3 ℃/min and carries out syntheticly in advance under 850~900 ℃, is incubated 1~3 hour; The synthetic in advance material piece that obtains is ground to all through 40 mesh sieves; Be medium, ball milling 8~12 hours once more with the absolute ethyl alcohol, discharging is also dry; Add the binder solution that accounts for powder quality 20% in the powder,, obtain the diaphragm that thickness is 0.3~0.5mm through batch mixing and material, roughing and finish rolling;
(3) diaphragm is incubated 2~4 hours plastic removals down at 720~750 ℃, and temperature rise rate is 1~5 ℃/min; Then diaphragm is placed alumina crucible, airtight sintering, sintering temperature is 1170~1260 ℃, soaking time is 1~3 hour, promptly gets ceramic plate;
(4) ceramic plate lining silver electrode in two sides behind grinding and polishing, and 80~120 ℃ of polarization down in silicone oil, polarized electric field is 6000~8000V/mm, the time is 45~60 minutes.
3. by the described method for preparing modified lead titanate piezoelectric ceramic of claim 2, it is characterized in that said sticker is a Z 150PH, the polyvinyl alcohol solution mass concentration is 18%.
4. by the described modified lead titanate piezoelectric ceramic of claim 1, be used for piezoelectric filter, piezo-resonator and transverter.
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CN103588478A (en) * | 2013-11-15 | 2014-02-19 | 中船重工海声科技有限公司 | Lead titanate piezoelectric ceramics and preparation method |
CN107892567B (en) * | 2017-11-03 | 2020-12-04 | 北京工业大学 | (Bi)1/2K1/2)TiO3Base binary leadless piezoelectric ceramic and preparation thereof |
CN107999053B (en) * | 2017-11-06 | 2020-06-16 | 哈尔滨理工大学 | Lead lanthanum titanate/bismuth vanadate and preparation method thereof |
CN109180180B (en) * | 2018-10-25 | 2021-07-02 | 北京工业大学 | Preparation method for synthesizing piezoelectric ceramic material with submicron crystal size by one-step pressureless sintering |
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2009
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EP0156312A2 (en) * | 1984-03-21 | 1985-10-02 | NGK Spark Plug Co. Ltd. | A piezo-electric ceramic composition for resonator in electrical wave filters |
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