CN105884350B - A kind of barium calcium zirconate titanate lead-free piezoceramic material and preparation method thereof - Google Patents
A kind of barium calcium zirconate titanate lead-free piezoceramic material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to technical field of inorganic nonmetallic materials, refer in particular to a kind of barium calcium zirconate titanate lead-free piezoceramic material.Formula composition includes: (Ba0.85Ca0.15)(Ti0.9Zr0.1)O391~98wt.%, BiFeO30.1~7.0wt.%, Bi2WO60.01~1wt.%, Ba (Yb1/2Nb1/2)O30.1~4wt.%, Co2O30.01~1.8wt.%；Wherein (Ba0.85Ca0.15)(Ti0.9Zr0.1)O3, it use piezoelectric ceramics general chemistry raw material, the leadless piezoelectric ceramics of high tension performance unleaded, without cadmium is prepared, moreover it is possible to which the sintering temperature for substantially reducing piezoelectric ceramics is suitable for preparing piezoceramic transducer, can substantially reduce the cost of piezoelectric ceramics.
Description
Technical field
The present invention relates to technical field of inorganic nonmetallic materials, refer in particular to a kind of barium calcium zirconate titanate lead-free piezoceramic material.
It uses piezoelectric ceramics general chemistry raw material, and the leadless piezoelectric ceramics of high tension performance unleaded, without cadmium is prepared, moreover it is possible to big
The big sintering temperature for reducing piezoelectric ceramics, the piezoelectric ceramics are suitable for preparing piezoceramic transducer, can substantially reduce piezoelectricity pottery
The cost of porcelain meets the developing direction of piezoelectric ceramics, can replace lead piezoelectric ceramics in the application of some fields, and preparing
With it is free from environmental pollution in use process.
Background technique
Piezoelectric material is a kind of new function material that can be carried out energy conversion, it can be realized between mechanical energy and electric energy
Conversion, with the fast development of electronics technology and information technology, piezoelectric material is generalized out in the every field that people live
Come, and also has critically important application being related to military and national security.With industries such as communication, electronics and health cares
Rapid development, electronic component miniaturization, functionalization, low cost and high stability etc. are required higher and higher.It was pressed in the past
In the development course of electric material, lead zirconate titanate (Pb (Zr, Ti) O3) base binary system or polynary system piezoelectric material system be in occupation of master
Status is led, but contains a large amount of lead (Pb) element in these piezoelectric materials, and lead is a kind of metal member volatile at high temperature
Element, there are huge harm for health and living environment to the mankind, are based on this, the research of leadless piezoelectric ceramics be one must
Right trend.In leadless piezoelectric ceramics, barium titanate (BaTiO3) it is the lead-free piezoceramic material found earliest, and grind at present
The lead-free piezoceramic material for studying carefully relative maturity, has broad application prospects.But in actual application, BaTiO3Ceramics
There is also some problems, such as Curie temperature are low (about 120 DEG C), piezoelectric property is not high (about 190pC/N), and operation temperature area is narrow, nothing
Method is applied to powerful energy converter etc.；The stability of the piezoelectric ceramics is not good enough simultaneously, and sintering is difficult, and sintering temperature is general
It is up to 1300 DEG C~1350 DEG C.In recent years, doping vario-property BaTiO3The research of ceramics is always domestic and international piezoelectric ceramics field
One of research emphasis, by BaTiO3The second constituent element or the available higher pressure electrical property of multicomponent mixture are added in ceramics
Unleaded piezoceramic material.There is researcher to use CaTiO3-BaZrO3-BaTiO3It is compounded to form solid solution, makes its piezoelectricity
It can be greatly improved, the CaTiO obtained using this method3-BaZrO3-BaTiO3The piezoelectric modulus of based leadless piezoelectric ceramics
(d33) it is 482PC/N, radial electromechanical coupling factor (KP) it is 0.48, still, Curie temperature is 90 DEG C or so, piezoelectric ceramics
Sintering temperature it is higher (1500~1600 DEG C), which hardly results in application.Therefore, search out a kind of high
Piezoelectric property, the effective ways that can reduce sintering temperature significantly again compared with high-curie temperature, are an important research topics.
Summary of the invention
The object of the present invention is to provide a kind of high-performance barium calcium zirconate titanate lead-free piezoceramic materials.
The object of the present invention is achieved like this:
The high-performance barium calcium zirconate titanate leadless piezoelectric ceramics formula composition includes: (Ba0.85Ca0.15)(Ti0.9Zr0.1)O3
91~98wt.%, BiFeO30.1~7.0wt.%, Bi2WO60.01~1wt.%, Ba (Yb1/2Nb1/2)O30.1~
4wt.%, Co2O30.01~1.8wt.%；Wherein (Ba0.85Ca0.15)(Ti0.9Zr0.1)O3、BiFeO3、Bi2WO6、Ba(Yb1/ 2Nb1/2)O3Conventional chemical raw material is respectively adopted with Solid phase synthesis.
(Ba used in medium of the invention0.85Ca0.15)(Ti0.9Zr0.1)O3It is to be prepared using following technique: will be normal
The chemical raw material BaCO of rule3、CaCO3、TiO2、ZrO2By 0.85:0.15:0.9:0.1 molar ratio ingredient, after ground and mixed is uniform
It is put into alumina crucible and keeps the temperature 120 minutes in 1350-1390 DEG C, solid state reaction kinetics (Ba0.85Ca0.15)(Ti0.9Zr0.1)O3,
Ground 200 mesh, spare after cooling.
Bi used in medium of the invention2WO6It is to be prepared using following technique: by conventional chemical raw material Bi2O3With
WO3It by 1:1 molar ratio ingredient, is put into after ground and mixed is uniform in alumina crucible and keeps the temperature 120 minutes in 850 DEG C, obtained after cooling
To Bi2WO6, ground 200 mesh is spare.
BiFeO used in medium of the invention3It is to be prepared using following technique: by conventional chemical raw material Bi2O3、
Fe2O3By 1/2:1/2 molar ratio ingredient, it is put into after ground and mixed is uniform in alumina crucible and keeps the temperature 120 minutes in 800-900 DEG C,
Solid state reaction kinetics BiFeO3, ground 200 mesh, spare after cooling.
Ba (Yb used in medium of the invention1/2Nb1/2)O3Preparation process include: by conventional chemical raw material
BaCO3、Yb2O3、Nb2O5By 1:1/4:1/4 molar ratio ingredient, it is put into after ground and mixed is uniform in alumina crucible in 1250-
1280 DEG C heat preservation 120-180 minutes, solid state reaction kinetics Ba (Yb1/2Nb1/2)O3, ground 200 mesh, spare after cooling.
The present invention uses following ceramic dielectric preparation process: being closed respectively using conventional chemical raw material with solid phase method first
At (Ba0.85Ca0.15)(Ti0.9Zr0.1)O3、BiFeO3、Bi2WO6、Ba(Yb1/2Nb1/2)O3, formula ingredient is then pressed by batch
Ball mill grinding mixing, after being dried, be added adhesive be granulated, it is re-compacted at green sheet, then in air carry out dumping and
Sintering, obtains high performance piezoelectric ceramics, and by silver electrode, then performance is surveyed in polarization.
The formula of above-mentioned leadless piezoelectric ceramics is preferably with following two kinds of schemes:
(Ba0.85Ca0.15)(Ti0.9Zr0.1)O392~96wt.%, BiFeO30.1~5.0wt.%, Bi2WO60.01~
0.8wt.%, Ba (Yb1/2Nb1/2)O30.1~3.8wt.%, Co2O30.03~1.6wt.%.
(Ba0.85Ca0.15)(Ti0.9Zr0.1)O392~95wt.%, BiFeO30.1~5.5wt.%, Bi2WO30.01~
0.8wt.%, Ba (Yb1/2Nb1/2)O30.1~3.5wt.%, Co2O30.03~1.5wt.%.
Compared with the prior art, the invention has the following advantages:
1, the medium of this patent uses following preparation process: being respectively synthesized (Ba first0.85Ca0.15)(Ti0.9Zr0.1)O3、
BiFeO3、Bi2WO3、Ba(Yb1/2Nb1/2)O3, then according to formula ingredient, ball milling mixing is dry, and it is molten that a certain amount of PVA is added
Liquid is granulated, dry-pressing formed, sintering, by silver electrode, polarization, test performance.
2, the piezoelectric strain constant (d of prepared piezoelectric ceramics33) higher, it can achieve 320pC/N or more；It is radial electromechanical
The coefficient of coup (Kp) is higher, can achieve 35% or more；Dielectric constant (ε) is higher, can achieve 2500 or more；Curie temperature
(Tc) higher, it can achieve 135 DEG C or more；Dielectric loss (tan δ) is less than 0.02；Sintering temperature is lower, and sintering temperature is not more than
1360℃；Stability is good in use process, highly-safe, no pollution to the environment.
3, primary raw material can produce high performance leadless piezoelectric ceramics of the invention using piezoelectric ceramics raw material.
Specific embodiment
Presently in connection with embodiment, the invention will be further described.Table 1 provides the embodiment of the present invention totally 4 samples
Formula.
The embodiment of the present invention the formula of totally 4 samples primary raw material use piezoelectric ceramics raw material, in the preparation first
(Ba is respectively synthesized with solid phase method using conventional chemical raw material0.85Ca0.15)(Ti0.9Zr0.1)O3、BiFeO3、Bi2WO3、Ba
(Yb1/2Nb1/2)O3, above-mentioned formula ingredient is then pressed, the material prepared dehydrated alcohol is used into planetary ball mill ball milling mixing,
Material: ball: dehydrated alcohol=1:3:(0.6~1.0) (mass ratio) dry to obtain dry mash, in dry mash after ball milling 4~8 hours
The poly-vinyl alcohol solution for accounting for the concentration of its weight 8~10% as 10% (weight percent) is added, is granulated, crosses 40 after mixed
Mesh, then dry-pressing is carried out into green sheet under 20~30Mpa pressure, heat preservation 2~3 is small at being then 1330~1360 DEG C in temperature
Shi Jinhang dumping and sintering, then 15 minutes progress silver ink firings are kept the temperature at 780~800 DEG C, silver electrode is formed, and 100 in silicone oil
DEG C polarization, polarized electric field be 3000~4000 volts/mm, the polarization time be 15~20 minutes；Polarization finishes, small by aging 48
When, test its performance.
The performance of above-mentioned each formula sample is listed in table 2.The piezoelectric strain of prepared piezoelectric ceramics is normal as can be seen from Table 2
Number (d33) higher, it can achieve 320pC/N or more；Radial electromechanical coupling factor (Kp) is higher, can achieve 35% or more；Dielectric
Constant (ε) is higher, can achieve 2500 or more；Curie temperature (Tc) is higher, can achieve 135 DEG C or more；Dielectric loss (tan
δ) less than 0.02；Sintering temperature is lower, and sintering temperature is 1360 DEG C or less.
The formula of 1 the embodiment of the present invention of table totally 4 samples
Note: BCTZ is (Ba0.85Ca0.15)(Ti0.9Zr0.1)O3Abbreviation
Table 2 is respectively formulated the performance of sample
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of barium calcium zirconate titanate lead-free piezoceramic material, it is characterised in that the barium calcium zirconate titanate lead-free piezoceramic material
Formula composition are as follows: (Ba0.85Ca0.15)(Ti0.9Zr0.1)O391~98wt.%, BiFeO30.1~7.0wt.%, Bi2WO60.01
~1wt.%, Ba (Yb1/2Nb1/2)O30.1~4wt.%, Co2O30.01~1.8wt.%.
2. a kind of barium calcium zirconate titanate lead-free piezoceramic material as described in claim 1, it is characterised in that: described
(Ba0.85Ca0.15)(Ti0.9Zr0.1)O3、BiFeO3、Bi2WO6、Ba(Yb1/2Nb1/2)O3Conventional chemical raw material is respectively adopted with solid
The synthesis of phase method.
3. a kind of barium calcium zirconate titanate lead-free piezoceramic material as claimed in claim 1 or 2, which is characterized in that described
(Ba0.85Ca0.15)(Ti0.9Zr0.1)O3It is to be prepared using following technique: by conventional chemical raw material BaCO3、CaCO3、TiO2、
ZrO2By 0.85:0.15:0.9:0.1 molar ratio ingredient, it is put into after ground and mixed is uniform in alumina crucible in 1350-1390 DEG C
Heat preservation 120 minutes, solid state reaction kinetics (Ba0.85Ca0.15)(Ti0.9Zr0.1)O3, ground 200 mesh, spare after cooling.
4. a kind of barium calcium zirconate titanate lead-free piezoceramic material as claimed in claim 1 or 2, it is characterised in that described
Bi2WO6It is to be prepared using following technique: by conventional chemical raw material Bi2O3And WO3By 1:1 molar ratio ingredient, ground and mixed is equal
It is put into after even in alumina crucible and keeps the temperature 120 minutes in 850 DEG C, obtain Bi after cooling2WO6, ground 200 mesh is spare.
5. a kind of barium calcium zirconate titanate lead-free piezoceramic material as claimed in claim 1 or 2, it is characterised in that described
BiFeO3It is to be prepared using following technique: by conventional chemical raw material Bi2O3、Fe2O3By 1/2:1/2 molar ratio ingredient, grinding
It is put into alumina crucible after mixing and keeps the temperature 120 minutes in 800-900 DEG C, solid state reaction kinetics BiFeO3, ground after cooling
Honed 200 mesh, it is spare.
6. a kind of barium calcium zirconate titanate lead-free piezoceramic material as claimed in claim 1 or 2, it is characterised in that the Ba
(Yb1/2Nb1/2)O3Preparation process include: by conventional chemical raw material BaCO3、Yb2O3、Nb2O5Match by 1:1/4:1/4 molar ratio
Material, be put into after ground and mixed is uniform in alumina crucible in 1250-1280 DEG C heat preservation 120-180 minutes, solid state reaction kinetics Ba
(Yb1/2Nb1/2)O3, ground 200 mesh, spare after cooling.
7. a kind of barium calcium zirconate titanate lead-free piezoceramic material as described in claim 1, it is characterised in that the barium zirconium phthalate
Calcium lead-free piezoceramic material formula composition are as follows: (Ba0.85Ca0.15)(Ti0.9Zr0.1)O392~96wt.%, BiFeO30.1~
5.0wt.%, Bi2WO60.01~0.8wt.%, Ba (Yb1/2Nb1/2)O30.1~3.8wt.%, Co2O30.03~1.6wt.%.
8. a kind of barium calcium zirconate titanate lead-free piezoceramic material as described in claim 1, it is characterised in that the barium zirconium phthalate
Calcium lead-free piezoceramic material formula composition are as follows: (Ba0.85Ca0.15)(Ti0.9Zr0.1)O392~95wt.%, BiFeO30.1~
5.5wt.%, Bi2WO60.01~0.8wt.%, Ba (Yb1/2Nb1/2)O30.1~3.5wt.%, Co2O30.03~
1.5wt.%.
9. a kind of barium calcium zirconate titanate lead-free piezoceramic material as described in claim 1, it is characterised in that: the barium zirconium phthalate
Calcium lead-free piezoceramic material piezoelectric constant (d33) higher, it can achieve 320pC/N or more；Radial electromechanical coupling factor is higher,
It can achieve 35% or more；Dielectric constant (ε) is higher, can achieve 2500 or more；Curie temperature (Tc) is higher, can achieve
135 DEG C or more；Dielectric loss (tan δ) is less than 0.02；Sintering temperature is lower, is not more than 1360 DEG C.
10. a kind of preparation method of barium calcium zirconate titanate lead-free piezoceramic material as described in claim 1, it is characterised in that:
(Ba is respectively synthesized with solid phase method using conventional chemical raw material first0.85Ca0.15)(Ti0.9Zr0.1)O3、BiFeO3、Bi2WO6、Ba
(Yb1/2Nb1/2)O3, then by formula ingredient, the material prepared dehydrated alcohol is used into planetary ball mill ball milling mixing, by quality
Than material: ball: dehydrated alcohol=1:3:(0.6~1.0), after ball milling 4~8 hours, dry mash is dried to obtain, is added and accounts in dry mash
The poly-vinyl alcohol solution that the mass percentage concentration of dry mash weight 8~10% is 10%, is granulated, and crosses 40 meshes after mixed,
Again under 20~30MPa pressure carry out dry-pressing at green sheet, then temperature be 1330~1360 DEG C at keep the temperature 2~3 hours into
Row dumping and sintering, then 15 minutes progress silver ink firings are kept the temperature at 780~800 DEG C, form silver electrode, and 100 DEG C of pole in silicone oil
Change, polarized electric field is 3000~4000 volts/mm, and the polarization time is 15~20 minutes；Polarization finishes, and by aging 48 hours, surveys
Try its performance.
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| CN106518121A (en) * | 2016-11-10 | 2017-03-22 | 佛山蓝途科技有限公司 | High-Curie-temperature leadless piezoelectric ceramic and preparation method thereof |
| CN107151138B (en) * | 2017-05-02 | 2020-07-10 | 桂林电子科技大学 | Low-loss ultrahigh-voltage-performance lead-free piezoelectric ceramic material and preparation method thereof |
| CN107032785B (en) * | 2017-05-11 | 2020-04-17 | 桂林电子科技大学 | Lead-free ferroelectric ceramic with narrow band gap and high polarity and preparation method thereof |
| CN107177144B (en) * | 2017-06-27 | 2019-08-16 | 哈尔滨理工大学 | A kind of sandwich structure nanofiber/Kynoar complex media and preparation method thereof |
| CN107602114B (en) * | 2017-10-26 | 2022-05-20 | 贵州大学 | Barium calcium zirconate titanate BCZT piezoelectric ceramic and texturing preparation method thereof |
| CN108546124B (en) * | 2018-05-03 | 2021-07-30 | 景德镇市鑫惠康电子有限责任公司 | Preparation method of BCZT-based lead-free piezoelectric ceramic |
| CN109097841B (en) * | 2018-07-24 | 2021-10-22 | 哈尔滨理工大学 | Anisotropic nanofiber polyvinylidene fluoride-based composite medium and preparation method thereof |
| CN110128137B (en) * | 2019-05-27 | 2022-01-25 | 太原师范学院 | Photosensitive ceramic dielectric material and preparation method thereof |
| CN112723877B (en) * | 2020-12-29 | 2022-06-17 | 北京工业大学 | Ceramic-metal lead-free piezoelectric composite material with micron inner crystal structure and preparation method thereof |
| CN113200744B (en) * | 2021-04-25 | 2021-11-30 | 湖南省美程陶瓷科技有限公司 | Lead-free piezoelectric ceramic sensor material and preparation method thereof |
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| CN1287988A (en) * | 1999-08-16 | 2001-03-21 | 株式会社村田制作所 | Method for mfg. piezoelectric ceramics |
| CN103373849A (en) * | 2013-07-09 | 2013-10-30 | 贵州大学 | Niobium oxide doped barium calcium zirconate titanate leadless piezoelectric ceramic powder material |
| CN105418067A (en) * | 2015-12-08 | 2016-03-23 | 天津大学 | Preparation method of barium calcium zirconate titanate lead-free piezoelectric textured ceramic |
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| CN1287988A (en) * | 1999-08-16 | 2001-03-21 | 株式会社村田制作所 | Method for mfg. piezoelectric ceramics |
| CN103373849A (en) * | 2013-07-09 | 2013-10-30 | 贵州大学 | Niobium oxide doped barium calcium zirconate titanate leadless piezoelectric ceramic powder material |
| CN105418067A (en) * | 2015-12-08 | 2016-03-23 | 天津大学 | Preparation method of barium calcium zirconate titanate lead-free piezoelectric textured ceramic |
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