CN103086713A - Near-zero-temperature coefficient piezoelectric ceramic for surface acoustic waves and preparation method thereof - Google Patents

Near-zero-temperature coefficient piezoelectric ceramic for surface acoustic waves and preparation method thereof Download PDF

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CN103086713A
CN103086713A CN2013100660789A CN201310066078A CN103086713A CN 103086713 A CN103086713 A CN 103086713A CN 2013100660789 A CN2013100660789 A CN 2013100660789A CN 201310066078 A CN201310066078 A CN 201310066078A CN 103086713 A CN103086713 A CN 103086713A
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piezoelectric ceramics
surface acoustic
acoustic wave
temperature coefficient
temperature
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CN103086713B (en
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黄新友
高春华
蔡尔华
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Jiangsu University
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Jiangsu University
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Abstract

The invention relates to a formula composition of near-zero-temperature coefficient piezoelectric ceramic for surface acoustic waves, which is prepared from common chemical raw materials by a conventional solid-phase process. The invention is characterized in that the formula of the piezoelectric ceramic is [(Pb(1-3/2x+y/2)Lnx][Ti(0.98-y)Mn0.02By]O3, wherein 0.01<=x<=0.5; Ln is Ce, Sm or Gd; 0.01<=y<=0.8; and B is In or Yb. The delay time temperature coefficient (T[CD]) of the prepared piezoelectric ceramic is approximate to zero, the surface acoustic wave propagation velocity (Upsilon[s]) is 2500 m/s or so, and the dielectric constant is 230 or so. The mechanical factor of merit (Q[m]) is 2000 or so, the surface acoustic wave electromechanical coupling factor (K[s]) is 0.18 or so, and the Curie temperature is 350 DEG C or so.

Description

A kind of nearly zero-temperature coefficient surface acoustic wave piezoelectric ceramics and preparation method thereof
Technical field
The present invention relates to technical field of inorganic nonmetallic materials, refer in particular to a kind of nearly zero-temperature coefficient surface acoustic wave and use the formula of piezoelectric ceramics to form; It adopts the preparation method of conventional solid phase method pottery, utilizes the general chemistry raw material, prepares nearly zero-temperature coefficient surface acoustic wave piezoelectric ceramics, and this piezoelectric ceramics is suitable for preparing surface acoustic wave device.
Technical background
Piezoelectric ceramics has good piezoelectric effect, to use a class very widely in function ceramics, as sensor, transverter, wave filter etc., play an important role in national economy and national defense industry, piezoelectric ceramics is mainly Pb-based lanthanumdoped zirconate titanates base and ternary and four-component-system piezoelectric ceramics; At present, making surface acoustic wave device is mainly Pb-based lanthanumdoped zirconate titanates base piezoelectric ceramic and crystalline material, but crystalline material is difficult to satisfy the requirement of high electromechanical coupling factor and low-temperature coefficient, the monocrystal material price general charged is expensive, and generally they are anisotropic materials, so high-precision directional cutting technology need to be arranged, this is also its shortcoming; The Pb-based lanthanumdoped zirconate titanates base piezoelectric ceramic only has application report in all-bottom sound surface-duided wave (SAW) devices field, but its temperature factor is too large, is difficult to the making of high-frequency sound surface wave (SAW) device; Lead titanate ceramics have good piezoelectric property, and by the mode of various replacements and doping, people have overcome the sintering difficulty, have obtained some and have been widely used in the formula of different field, especially in the high frequency field; We are by research, and we obtain nearly zero-temperature coefficient high-frequency sound surface wave (SAW) and use lead titanate piezoelectric ceramics.
Summary of the invention
The object of the present invention is achieved like this: a kind of nearly zero-temperature coefficient surface acoustic wave piezoelectric ceramics, its formula is: [(Pb (1-(3/2) x+y/2)Ln x] [Ti (0.98-y)Mn 0.02B y] O 3, 0.01≤x≤0.5, Ln=Ce, Sm or Gd; 0.01≤y≤0.8, B=In or Yb.
The present invention adopts conventional solid phase method pottery preparation technology, namely at first by the formula batching, the admixtion ball mill pulverizing is mixed, after drying, add the tackiness agent granulation, be pressed into again green sheet, then carry out binder removal and sintering in air, after insulation and naturally cooling, obtain lead titanate piezoelectric ceramics, on pottery by electrode, then polarization, aging, surveys performance.
Above-mentioned nearly zero-temperature coefficient surface acoustic wave preferably adopts following two kinds of schemes with the formula of piezoelectric ceramics:
[(Pb (1-(3/2) x+y/2)Ln x] [Ti (0.98-y)Mn 0.02B y] O 3, 0.05≤x≤0.4, Ln=Ce, Sm or Gd; 0.03≤y≤0.6, B=In or Yb;
[(Pb (1-(3/2) x+y/2)Ln x] [Ti (0.98-y)Mn 0.02B y] O 3, 0.08≤x≤0.3, Ln=Ce, Sm or Gd; 0.1≤y≤0.5, B=In or Yb.
The present invention compared with prior art has following advantage:
1, the piezoelectric ceramics of this patent time of lag temperature factor close to zero; Curie temperature is high, is 350 ℃ of left and right.
2, the piezoelectric ceramics performance of this patent is easy to regulate, to satisfy the requirement of serial high-frequency sound surface wave (SAW) device.
3, this pottery adopts conventional solid phase method piezoelectric ceramics preparation technology to be prepared, and the raw material that uses is conventional chemical feedstocks, and cost of manufacture is low.
Embodiment
The invention will be further described in conjunction with the embodiments now.Table 1 provides the embodiments of the invention formula ([(Pb of totally 4 samples (1-3/2x+y/2)Ln x] [Ti (0.98-y)Mn 0.02B y] O 3).
Embodiments of the invention are the formula of totally 4 samples:
Formula 1 is: [(Pb 0.995S M0.03] [Ti 0.9Mn 0.02In 0.08] O 3
Formula 2 is: [(Pb 0.96S M0.06] [Ti 0.88Mn 0.02In 0.1] O 3
Formula 3 is: [(Pb 0.95Gd 0.1] [Ti 0.78Mn 0.02Yb 0.2] O 3
Formula 4 is: [(Pb 0.825Gd 0.2] [Ti 0.73Mn 0.02Yb 0.25] O 3).
Main raw material adopts conventional chemical feedstocks, is specially: tri-lead tetroxide (Pb 3O 4), titanium dioxide (TiO 2), manganous carbonate (MnCO 3), samarium sesquioxide (Sm 2O 3), three Indium sesquioxide (In 2O 3), yttria (Yb 2O 3), Gadolinium trioxide (Gd 2O 3); By above-mentioned formula batching, adopt the planetary ball mill ball milling to mix with distilled water or deionized water in the material for preparing, material: ball: water=1:3:(0.6 ~ 1.0), after ball milling 4 ~ 8 hours, dry to get dry mash, adding the concentration that accounts for its weight 5 ~ 8% in dry mash is the polyvinyl alcohol solution of 10% (weight percent), carry out granulation, mixed rear mistake 40 mesh sieves, carry out again dry-pressing and become green sheet under 20 ~ 30Mpa pressure, then be to be incubated 1 ~ 4 hour under 750 ~ 850 ℃ to carry out binder removal in temperature, temperature rise rate is 50-100 ℃/hour; Then sample is placed in alumina crucible, airtight sintering, sintering temperature is 1200-1260 ℃, soaking time is 1-3 hour, namely obtains ceramic plate; Ceramic plate is two sides coating silver electrode after grinding and polishing, and polarization under 120-160 ℃ in silicone oil, and polarized electric field is 6000-8000 volt/mm, and the polarization time is 45-60 minute; Through overaging 48 hours, test its performance; Above-mentioned performance of respectively filling a prescription sample is listed in table 1; Temperature factor (T time of lag of prepared piezoelectric ceramics as can be seen from Table 1 CD) close to zero, acoustic surface wave propagation speed (υ s) be the 2530m/s left and right, specific inductivity (ε) is about 230 left and right; Qm (Q m) be 2000 left and right, surface acoustic wave electromechanical coupling factor (K s) be 0.18 left and right, Curie temperature (T c) be 350 ℃ of left and right.
Table 1 embodiments of the invention are formula and the performance of totally 4 samples
Figure 467800DEST_PATH_IMAGE001
The above is only preferred embodiment of the present invention, not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, is equal to and replaces and improvement etc., within all should being included in protection scope of the present invention.

Claims (4)

1. a nearly zero-temperature coefficient surface acoustic wave piezoelectric ceramics, is characterized in that described piezoelectric ceramics chemical formula is: [(Pb (1-(3/2) x+y/2)Ln x] [Ti (0.98-y)Mn 0.02B y] O 3, 0.01≤x≤0.5, Ln=Ce, Sm or Gd; 0.01≤y≤0.8, B=In or Yb; Temperature factor (T time of lag of described piezoelectric ceramics CD) be 0.01-0.08 ppm/ ℃, acoustic surface wave propagation speed (υ s) be 2530 ~ 2550m/s, specific inductivity (ε) is 228 ~ 238; Qm (Q m) be 1936-2020, surface acoustic wave electromechanical coupling factor (K s) be 0.18-0.24, Curie temperature (T c) be 348-362 ℃.
2. a kind of nearly zero-temperature coefficient surface acoustic wave piezoelectric ceramics as claimed in claim 1, is characterized in that described piezoelectric ceramics chemical formula is: [(Pb (1-(3/2) x+y/2)Ln x] [Ti (0.98-y)Mn 0.02B y] O 3, 0.05≤x≤0.4, Ln=Ce, Sm or Gd; 0.03≤y≤0.6, B=In or Yb;
A kind of nearly zero-temperature coefficient surface acoustic wave piezoelectric ceramics as claimed in claim 1 is characterized in that described piezoelectric ceramics chemical formula is: [(Pb (1-(3/2) x+y/2)Ln x] [Ti (0.98-y)Mn 0.02B y] O 3, 0.08≤x≤0.3, Ln=Ce, Sm or Gd; 0.1≤y≤0.5, B=In or Yb.
3. a kind of nearly zero-temperature coefficient surface acoustic wave as claimed in claim 1 with the preparation method of piezoelectric ceramics, is characterized in that comprising the steps: with tri-lead tetroxide (Pb 3O 4), titanium dioxide (TiO 2), manganous carbonate (MnCO 3), samarium sesquioxide (Sm 2O 3), three Indium sesquioxide (In 2O 3), yttria (Yb 2O 3) and Gadolinium trioxide (Gd 2O 3) be raw material; By above-mentioned formula batching, adopt the planetary ball mill ball milling to mix with distilled water or deionized water in the material for preparing, material: ball: water=1:3:(0.6 ~ 1.0), ball milling was dried to get dry mash after 4 ~ 8 hours, add polyvinyl alcohol solution in dry mash, carry out granulation, mixed rear mistake 40 mesh sieves, then carry out dry-pressing become green sheet under 20 ~ 30Mpa pressure, then be to be incubated 1 ~ 4 hour under 750 ~ 850 ℃ to carry out binder removal in temperature, temperature rise rate is 50-100 ℃/hour; Then sample is placed in alumina crucible, airtight sintering, sintering temperature is 1200-1260 ℃, soaking time is 1-3 hour, namely obtains ceramic plate.
4. a kind of nearly zero-temperature coefficient surface acoustic wave as claimed in claim 4 is with the preparation method of piezoelectric ceramics, and it is characterized in that: the mass percentage concentration of described polyvinyl alcohol solution is 10%, accounts for 5 ~ 8% of dry mash weight.
CN201310066078.9A 2013-03-04 2013-03-04 Near-zero-temperature coefficient piezoelectric ceramic for surface acoustic waves and preparation method thereof Expired - Fee Related CN103086713B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103420671A (en) * 2013-08-13 2013-12-04 江苏大学 Piezoceramic material for low-medium-frequency broadband ceramic filter
CN113651615A (en) * 2021-09-23 2021-11-16 无锡邦能超声科技有限公司 Piezoceramic material and high-stability ultrasonic transducer

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JPS5499000A (en) * 1978-01-20 1979-08-04 Hitachi Ltd Piezo-electric ceramic composition
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CN101475372A (en) * 2008-12-31 2009-07-08 山东沂光电子股份有限公司 Piezoelectric ceramic material for high performance surface acoustic wave transducer

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JPS5768091A (en) * 1980-10-15 1982-04-26 Hitachi Ltd Piezoelectric porcelain composition and surface acoustic wave element utilizing it
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103420671A (en) * 2013-08-13 2013-12-04 江苏大学 Piezoceramic material for low-medium-frequency broadband ceramic filter
CN103420671B (en) * 2013-08-13 2015-06-10 江苏大学 Piezoceramic material for low-medium-frequency broadband ceramic filter
CN113651615A (en) * 2021-09-23 2021-11-16 无锡邦能超声科技有限公司 Piezoceramic material and high-stability ultrasonic transducer
CN113651615B (en) * 2021-09-23 2022-10-14 大连世达科技有限公司 Piezoceramic material and high-stability ultrasonic transducer

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