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 PDFInfo
- 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
- Authority
- CN
- China
- Prior art keywords
- lead zirconate
- zirconate titanate
- piezoelectric ceramics
- piezoelectric ceramic
- praseodymium
- Prior art date
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- 239000000919 ceramic Substances 0.000 title claims abstract description 37
- 229910052451 lead zirconate titanate Inorganic materials 0.000 title claims abstract description 20
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 229910052777 Praseodymium Inorganic materials 0.000 title claims description 20
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 title claims description 20
- 238000002360 preparation method Methods 0.000 title claims description 5
- 239000000463 material Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052709 silver Inorganic materials 0.000 claims abstract description 7
- 239000004332 silver Substances 0.000 claims abstract description 7
- 238000005469 granulation Methods 0.000 claims abstract description 6
- 230000003179 granulation Effects 0.000 claims abstract description 6
- 230000010287 polarization Effects 0.000 claims abstract description 4
- 238000000465 moulding Methods 0.000 claims abstract description 3
- 238000000227 grinding Methods 0.000 claims description 8
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 7
- 238000010304 firing Methods 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000001125 extrusion Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 229920002545 silicone oil Polymers 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract 2
- 229910002637 Pr6O11 Inorganic materials 0.000 abstract 1
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 238000013329 compounding Methods 0.000 abstract 1
- XMFOQHDPRMAJNU-UHFFFAOYSA-N lead(II,IV) oxide Inorganic materials O1[Pb]O[Pb]11O[Pb]O1 XMFOQHDPRMAJNU-UHFFFAOYSA-N 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 abstract 1
- 238000005245 sintering Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 5
- NKZSPGSOXYXWQA-UHFFFAOYSA-N dioxido(oxo)titanium;lead(2+) Chemical compound [Pb+2].[O-][Ti]([O-])=O NKZSPGSOXYXWQA-UHFFFAOYSA-N 0.000 description 4
- 150000002910 rare earth metals Chemical class 0.000 description 4
- 230000008878 coupling Effects 0.000 description 3
- 238000010168 coupling process Methods 0.000 description 3
- 238000005859 coupling reaction Methods 0.000 description 3
- 229910052746 lanthanum Inorganic materials 0.000 description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
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
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.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100528267A CN101265091A (en) | 2008-04-21 | 2008-04-21 | Praseodymium doping lead zirconate titanate piezoelectric ceramic and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100528267A CN101265091A (en) | 2008-04-21 | 2008-04-21 | Praseodymium doping lead zirconate titanate piezoelectric ceramic and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101265091A true CN101265091A (en) | 2008-09-17 |
Family
ID=39987814
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|---|---|---|---|
| CNA2008100528267A Pending CN101265091A (en) | 2008-04-21 | 2008-04-21 | Praseodymium doping lead zirconate titanate piezoelectric ceramic and preparation method thereof |
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Cited By (5)
| 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 |
-
2008
- 2008-04-21 CN CNA2008100528267A patent/CN101265091A/en active Pending
Cited By (6)
| 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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