CN101265091A - Praseodymium doping lead zirconate titanate piezoelectric ceramic and preparation method thereof - Google Patents

Praseodymium doping lead zirconate titanate piezoelectric ceramic and preparation method thereof Download PDF

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Publication number
CN101265091A
CN101265091A CNA2008100528267A CN200810052826A CN101265091A CN 101265091 A CN101265091 A CN 101265091A CN A2008100528267 A CNA2008100528267 A CN A2008100528267A CN 200810052826 A CN200810052826 A CN 200810052826A CN 101265091 A CN101265091 A CN 101265091A
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China
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lead zirconate
zirconate titanate
piezoelectric ceramics
piezoelectric ceramic
praseodymium
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CNA2008100528267A
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孙清池
马卫兵
张伟
陆翠敏
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Tianjin University
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Tianjin University
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Abstract

The invention discloses a Pr-doped lead zirconate titanate piezoelectric ceramic, which has the following chemical formula: Pb1-1.5xPrx(ZryTi1-y) O3, wherein x is the range of 0.02-0.08 and y is the range of 0.51-0.60. Raw materials of the piezoelectric ceramic include Pb3O4, ZrO2, TiO2, and Pr6O11. The invention also discloses a production method of the piezoelectric ceramic. The method comprises the following steps: (1) material compounding, (2) granulation, (3) molding, (4) adhesive removal, (5) sintering and (6) silver burning and polarization. The piezoelectric ceramic provided in the invention is a novel binary piezoelectric ceramic with low price, good overall performance and wide application range, and can be used for a brake, cavity compensation in a laser gyroscope, and a whipping wheel of a laser gyroscope.

Description

Piezoelectric ceramics of praseodymium doping lead zirconate titanate and preparation method thereof
Technical field
The present invention relates to a kind of piezoelectric ceramics, relate in particular to the piezoelectric ceramics of praseodymium doping lead zirconate titanate.
Background technology
Along with development of science and technology, three, four-component-system piezoelectric ceramics obtained widely using, but two component system still has its unique advantage: can under higher temperature, use, form simple etc. as Curie temperature height, material.Pb-based lanthanumdoped zirconate titanates (PZT) binary system piezoelectric ceramics is carried out doping vario-property, some performance of material is improved.The doping of rare earth makes the specific inductivity of PZT or piezoelectric ceramics raise, and electromechanical coupling factor increases, and frequency constant reduces, and mechanical quality factor reduces.Ajai Garg, D.C.Agrawal studies with the piezoelectric property of rare earth Er, Gd, Eu, Nd and La doping PZT, the domestic Y that uses 2O 3The ultrasonic performance of piezoelectric ceramics of doping PZT is studied, and A.K.ARORA is to Pb (Zr xTi 1-x) O 3System mixes lanthanum (4mol%) and studies.But, at present for the effect of praseodymium in piezoelectric ceramics, state, inside and outside also few people research.China's rare earth resources is abundant, low price.Praseodymium is a rare earth element, and with the same cycle of lanthanum, so the PZT piezoelectric ceramics for the doping praseodymium is attempted, to obtain the good comprehensive properties piezoceramic material, this exploitation to domestic, external piezoelectric ceramics novel material is one and remedies, also will play promoter action for the expansion in piezoelectric ceramics market.
Summary of the invention
The objective of the invention is to develop trial, the piezoceramic material of a kind of low price, good combination property is provided, remedy a blank of domestic, external piezoelectric ceramics novel material, promote expansion for piezoelectric ceramics market to the praseodymium doping lead zirconate titanate piezoelectric ceramics.
The present invention is achieved by following technical solution.
The piezoelectric ceramics of praseodymium doping lead zirconate titanate, its composition and molar content are Pb 1-1.5xPr x(Zr yTi 1-y) O 3, x=0.02～0.08 wherein, y=0.51～0.60.
The raw material of described composition is Pb 3O 4, ZrO 2, TiO 2, Pr 6O 11, its purity is all greater than 99%.
Preparation process is as follows:
(1) batching: with Pb 3O 4, ZrO 2, TiO 2, Pr 6O 11Be raw material, press Pb 1-1.5xPr x(Zr yTi 1-y) O 3, x=0.02～0.08 wherein, the stoichiometric ratio of y=0.51～0.60 is mixed, and wet ball grinding 4 hours sieves after the drying;
(2) granulation: at Al 2O 3Seal 900 ℃ of pre-burnings in the crucible and be incubated 2 hours, ball milling 4 hours, synthetic material oven dry are added 7% polyvinyl alcohol (PVA), 100MPa precompressed granulation after sieving once more;
(3) moulding:, make disk through the 300MP extrusion forming;
(4) in 750 ℃ of binder removals;
(5) burn till: bury material in 1200 ℃～1280 ℃ row sealings and burn till, insulation 2h;
(6) after goods burnt till, the silver electrode that is covered after grinding, ultrasonic cleaning in 850 ℃ of silver ink firings, polarized in 150 ℃ of silicone oil again, makes the piezoelectric ceramics of praseodymium doping lead zirconate titanate.
The goods grinding thickness of described step (6) is 1mm, and the polarization time is 30 minutes, and field intensity is 2500V/mm.
The invention has the beneficial effects as follows the piezoceramic material that a kind of low price, good combination property are provided, remedied a blank of domestic, external piezoelectric ceramics novel material.
Embodiment
The present invention is with Pb 3O 4, ZrO 2, TiO 2, Pr 6O 11Be raw material, its purity is all greater than 99%.Press Pb 1-1.5xPr x(Zr yTi 1-y) O 3, x=0.02～0.08 wherein, the stoichiometric ratio of y=0.51～0.60 is mixed, and wet ball grinding 4 hours sieves after the drying; At Al 2O 3Seal 900 ℃ of pre-burnings in the crucible and be incubated 2 hours, ball milling 4 hours adds 7% polyvinyl alcohol after oven dry is sieved, after the 100MPa precompressed granulation; Through the 300MP extrusion forming, make disk; In 750 ℃ of binder removals; Burying material in 1200 ℃～1280 ℃ sealings burns till; After goods burnt till, grinding thickness was to 1mm, and the silver electrode that is covered after the ultrasonic cleaning in 850 ℃ of silver ink firings, polarizes in 150 ℃ of silicone oil again, and the polarization time is 30 minutes, and field intensity is 2500V/mm, makes the piezoelectric ceramics of praseodymium doping lead zirconate titanate.
The prescription that embodiment 1～6 selects is Pb 0.955Pr 0.03(Zr yTi 1-y) O 3Series, y=0.51,0.52,0.54,0.56,0.58,0.60, raw material consists of mass percent, and concrete prescription sees table 1 for details.
Table 1
Embodiment Pb 3O 4 Pr 6O 11 ZrO 2 TiO 2 Add up to Firing temperature (/ ℃)
1 67.0845 1.5698 19.3162 12.0295 100 1220
2 66.9952 1.5676 19.6687 11.7684 100 1220
3 66.8174 1.5635 20.3710 11.2481 100 1220
4 66.6405 1.5594 21.0695 10.7305 100 1220
5 66.4646 1.5548 21.7644 10.2157 100 1220
6 66.2878 1.5512 22.4560 9.7050 100 1220
The prescription that embodiment 7～11 selects is Pb 1-1.5xPr x(Zr 0.54Ti 0.46) O 3Series, x=0.02,0.03,0.04,0.06,0.08, raw material consists of mass percent, and concrete prescription sees table 2 for details.
Table 2
Embodiment Pb 3O 4 Pr 6O 11 ZrO 2 TiO 2 Add up to Firing temperature (/ ℃)
7 67.5084 1.0367 20.2644 11.1890 100 1220
8 66.8163 1.5635 20.3719 11.2483 100 1220
9 66.1119 2.0957 20.4796 11.3078 100 1220
10 64.6941 3.1773 20.6994 11.4292 100 1220
11 63.2303 4.2825 20.9240 11.5532 100 1220
The Pr-PZT piezoelectric ceramics characteristic of different zirconium content sees table 3 and table 4 for details.
Table 3
Embodiment ε 33 T/ε 0 tanδ d 33 K p Q m T c(/℃) Resistivity (/ 10 12Ω·cm) Density p (g/cm 3)
1 950 0.015 190 0.290 135 334 6.6 7.457
2 1020 0.016 208 0.314 117 330 2.8 7.547
3 2000 0.020 420 0.540 75 315 0.98 7.911
4 1480 0.024 400 0.460 76 302 1.1 7.860
5 870 0.031 281 0.388 104 293 4.4 7.645
6 790 0.034 242 0.360 119 280 7.5 7.520
Table 4
Embodiment ε 33 T/ε 0 Tanδ d 33 K p Q m T c(℃) Density p (g/cm 3)
7 1704 0.019 285 0.482 65 332 7.553
8 2000 0.020 420 0.540 75 315 7.911
9 1882 0.020 298 0.453 68 273 7.821
10 1914 0.021 258 0.422 63 238 7.650
11 1939 0.023 240 0.415 62 165 7.540
From table 3, can obviously find out embodiment 3 (zirconium content is 54mol%), DIELECTRIC CONSTANT 33 T/ ε 0, piezoelectric constant d 33, electromechanical coupling factor K p, density p all reaches maximum value, mechanical quality factor Q mWith the resistivity minimum.
From table 4, can obviously find out embodiment 8 (praseodymium content is 3mol%), ε 33 T/ ε 0, d 33, K p, Q mReach maximum value with ρ.
Embodiment 8 compares with the adulterated ceramic performance of no praseodymium and the results are shown in Table 5, mixes the lead titanate piezoelectric ceramics d of praseodymium as can be seen 33, K p, ε 33 T/ ε 0Increase Q mReduce.
Table 5
Performance Pb 0.955Pr 0.03(Zr 0.54Ti 0.46)O 3 Pb(Zr 0.48Ti 0.52)O 3
T c(/℃) 315 386
d 33(pC/N) 420 223
K p 0.54 0.53
Q m 75 500
Tanδ 0.02 0.4
ε 33 T/ε 0 2000 730
Praseodymium doping lead zirconate titanate piezoelectric ceramics of the present invention makes the specific inductivity of lead titanate piezoelectric ceramics bring up to original 2.73 times, piezoelectric constant is brought up to 1.89 times of lead titanate piezoelectric ceramics, electromechanical coupling factor has increased 2% than originally, the over-all properties of lead titanate piezoelectric ceramics all is improved.And praseodymium is as the rare-earth mineral low price, and reserves are abundant, its preferably piezoelectric and dielectric properties also will play promoter action for the expansion in piezoelectric ceramics market, can be widely used in stopper, the long compensation of laser gyro laser cavity, shaking laser gyroscope wheel etc.

Claims (4)

1. the piezoelectric ceramics of a praseodymium doping lead zirconate titanate, its composition and molar content are Pb 1-1.5xPr x(Zr yTi 1-y) O 3, x=0.02～0.08 wherein, y=0.51～0.60.
2. the piezoelectric ceramics of praseodymium doping lead zirconate titanate according to claim 1, the raw material of described composition is Pb 3O 4, ZrO 2, TiO 2, Pr 6O 11
3. the preparation method of the piezoelectric ceramics of the praseodymium doping lead zirconate titanate of claim 1, step is as follows:
(1) batching: with Pb 3O 4, ZrO 2, TiO 2, Pr 6O 11Be raw material, press Pb 1-1.5xPr x(Zr yTi 1-y) O 3, x=0.02～0.08 wherein, the stoichiometric ratio of y=0.51～0.60 is mixed, and wet ball grinding 4 hours sieves after the drying;
(2) granulation: at Al 2O 3Seal pre-burning in the crucible and be incubated 2 hours, ball milling 4 hours adds 7% polyvinyl alcohol after oven dry is sieved, after the 100MPa precompressed granulation;
(3) moulding:, make disk through the 300MP extrusion forming;
(4) in 750 ℃ of binder removals;
(5) burn till: bury material in 1200 ℃～1280 ℃ sealings and burn till;
(6) after goods burnt till, the silver electrode that is covered after grinding, ultrasonic cleaning in 850 ℃ of silver ink firings, polarized in 150 ℃ of silicone oil again, makes the piezoelectric ceramics of praseodymium doping lead zirconate titanate.
4. according to the preparation method of the piezoelectric ceramics of the praseodymium doping lead zirconate titanate of claim 3, it is characterized in that the goods grinding thickness of described step (6) is 1mm, the polarization time is 30 minutes, and field intensity is 2500V/mm.
CNA2008100528267A 2008-04-21 2008-04-21 Praseodymium doping lead zirconate titanate piezoelectric ceramic and preparation method thereof Pending CN101265091A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101717251B (en) * 2009-12-04 2012-05-23 北京工业大学 Modified lead titanate piezoelectric ceramic material and preparation method thereof
CN107746257A (en) * 2017-09-27 2018-03-02 无锡市惠丰电子有限公司 A kind of preparation method of piezoceramic material
CN108585852A (en) * 2018-05-10 2018-09-28 哈尔滨工业大学 A kind of praseodymium doped niobium indium magnesium titanate-zirconate luminous piezoelectric ceramic, preparation method and applications
CN112341196A (en) * 2020-10-27 2021-02-09 海鹰企业集团有限责任公司 Novel piezoelectric ceramic powder refining method and piezoelectric ceramic
CN113321507A (en) * 2021-05-26 2021-08-31 中南大学 Doped modified lead-based piezoelectric ceramic with excellent and stable piezoelectric performance

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101717251B (en) * 2009-12-04 2012-05-23 北京工业大学 Modified lead titanate piezoelectric ceramic material and preparation method thereof
CN107746257A (en) * 2017-09-27 2018-03-02 无锡市惠丰电子有限公司 A kind of preparation method of piezoceramic material
CN108585852A (en) * 2018-05-10 2018-09-28 哈尔滨工业大学 A kind of praseodymium doped niobium indium magnesium titanate-zirconate luminous piezoelectric ceramic, preparation method and applications
CN108585852B (en) * 2018-05-10 2021-04-20 哈尔滨工业大学 Praseodymium-doped lead indium niobate magnesio-titanate luminescent piezoelectric ceramic, and preparation method and application thereof
CN112341196A (en) * 2020-10-27 2021-02-09 海鹰企业集团有限责任公司 Novel piezoelectric ceramic powder refining method and piezoelectric ceramic
CN113321507A (en) * 2021-05-26 2021-08-31 中南大学 Doped modified lead-based piezoelectric ceramic with excellent and stable piezoelectric performance

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