CN101928139B - Bismuth calcium titanate-based luminous piezoelectric ceramic material and preparation method - Google Patents
Bismuth calcium titanate-based luminous piezoelectric ceramic material and preparation method Download PDFInfo
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Abstract
The invention relates to the field of electronic functional material, in particular to a bismuth calcium titanate-based luminous piezoelectric ceramic material and a preparation method thereof. The chemical components of the bismuth calcium titanate-based luminous piezoelectric ceramic material accord with a chemical general formula CaxBi4-yRyTi3+xO12+3x, wherein x is more than or equal to 1 and less than or equal to 2, y is more than or equal to 0.0001 and less than or equal to 0.5, and R is selected from one or more of Pr, Gd, Er, Dy, Tm, Ho, Eu, Yb and Tb. The ceramic material has ferroelectric, piezoelectric and dielectric properties and photoluminescence property at the same time, and belongs to a novel multifunctional material. The bismuth calcium titanate-based luminous piezoelectric ceramic material has excellent photoelectric property, and has wide application prospect in the fields of photoelectric integration, micro electro-mechanics, photoelectric sensing, LED technology and the like.
Description
Technical field
The present invention relates to the electronic functional material field, be specifically related to a kind of bismuth calcium titanate-based luminous piezoelectric ceramic material and preparation method thereof.
Background technology
Along with the development of new and high technology, new material technology has become the countries in the world scholars and has fallen over each other the hot fields exploring and study.Piezoelectric is the important electronic functional material of a class, has a wide range of applications at high-technology fields such as information, laser, navigation and biologies.In order to adapt to the development of current new and high technology, satisfy functionalization, miniaturization and the intelligentized requirement of piezoelectric, existing scholar also tries to explore and expands its new function in further investigation with when constantly improving the original performance of piezoelectric both at home and abroad.Studies show that, by composition of raw materials choose and the control of experimental technique can make piezoelectric have multifunction.Group such as the applicant place takes the lead in having realized light-machine-electricity conversion multifunction in having the barium titanate calcium based leadless piezoelectric ceramics system of perovskite structure.Behind a small amount of Rare Earth Elements of Praseodymium that in the lattice of barium titanate calcium two-phase composite ceramics, mixes, not only improve this stupalith ferroelectricity, also make simultaneously this material have photoluminescence, electroluminescent and stress irradiance multifrequency nature, referring to magazine " Advanced Materials ", 2005, the 17th phase, the 1254-1258 page or leaf.The barium titanate calcium multi-functional pressure electric material that the research middle-weight rare earths praseodymium mixes has good photoelectric characteristic, has a wide range of applications at aspects such as photoelectricity, micro electronmechanical and artificial intelligence.The group at applicant place is also carrying out correlated performance research aspect the made device of this barium titanate calcium two-phase composite ceramic material system, referring to magazine " Applied Physics Express ", and 2010, the 3rd phase, article numbering: 022601.At present, domestic and international research about the rear-earth-doped multi-functional pressure electroceramics material characteristics of luminescence mainly concentrates on the barium titanate calcium system.
As an important class lead-free piezoceramic material, " bismuth stratiform " the bismuth calcium titanate base ceramic material with laminated perovskite structure has high-curie temperature, high dielectric breakdown strength, low conductivity, low-dielectric loss and the good characteristics such as antifatigue.Because these characteristics, bismuth calcium titanate-based pottery has a wide range of applications in fields such as high temperature, high frequency, piezoelectric effect device and non-volatile random access memory.And at present be only limited at present thin-film material about the report of bismuth calcium titanate-based piezoelectric optical Properties, and referring to magazine " Journal of Physics D:Applied Physics ", 2009 years, the 42nd phase, article numbering: 105411.The present invention mixes a certain amount of rare earth element for adapting to the requirement of new high-tech material technical development in the single-phase leadless piezoelectric ceramics substrate material of " bismuth stratiform " bismuth calcium titanate, by technology controlling and process to realize its photoluminescence property.This material has good photoelectric characteristic, and integrated, micro electronmechanical and fields such as photoelectric sensing, LED lighting engineering have a wide range of applications at photoelectricity.
Summary of the invention
The object of the present invention is to provide a kind of bismuth calcium titanate-based luminous piezoelectric ceramic material with ferroelectric, piezoelectricity, dielectric and photoluminescence performance and preparation method thereof, to overcome the deficiencies in the prior art.
A kind of bismuth calcium titanate-based luminous piezoelectric ceramic material, its chemical composition meets chemical general formula Ca
xBi
4-yR
yTi
3+xO
12+3x, 1≤x≤2,0.0001≤y≤0.5 wherein, described R is selected from one or more among rare earth element Pr, Gd, Er, Dy, Tm, Ho, Eu, Yb and the Tb.
Better, the span of y is 0.005≤y≤0.02.
The preparation method of described bismuth calcium titanate-based luminous piezoelectric ceramic material is solid reaction process, in bismuth calcium titanate leadless piezoelectric ceramics substrate material, mix a certain amount of rare earth element, to realize the photoluminescence property of its powder and ceramic block material, namely excite lower and the performance of red-emitting at UV-light, blue light and green glow multiband light by technology controlling and process.
The preparation method of described bismuth calcium titanate-based luminous piezoelectric ceramic material specifically may further comprise the steps:
(1), according to chemical general formula Ca
xBi
4-yR
yTi
3+xO
12+3xThe stoichiometric ratio of middle Ca, Bi, Ti and R takes by weighing raw material: CaCO
3, Bi
2O
3, TiO
2, R oxide compound or nitrate, 1≤x≤2,0.0001≤y≤0.5 wherein.
(2), raw material that step (1) is taken by weighing mixes, add dehydrated alcohol or deionized water through grind or ball milling after, the discharging oven dry obtains powder A.
The mass ratio of described dehydrated alcohol or deionized water and raw material is 1～3: 1; The mass ratio of described ball milling material zirconia ball and raw material is 1～1.5: 1.
(3), place the alumina crucible pre-burning to obtain preburning powdered material B powder A.
Described calcined temperature is 750～950 ℃, and soaking time is 1～6h.
Preferably, described calcined temperature is 850～950 ℃, and soaking time is 2h.
(4), preburning powdered material B ground or ball milling after, adopting the quality percentage composition is that 8～10% binding agent carries out granulation to powder material B, then is pressed into ceramic green sheet C under 10～100MPa pressure.
Described binding agent is PVAC polyvinylalcohol.
The quality percentage composition of described binding agent is that binder phase is for the quality percentage composition of preburning powdered material.
(5), obtain described bismuth calcium titanate-based luminous piezoelectric ceramic material behind ceramic green sheet C row is sticking, the sintering.
The sticking temperature of described row is 550～600 ℃, and the sticking soaking time of row is 2～4h;
Described sintering temperature is 1000～1250 ℃, and the sintered heat insulating time is 2～6h;
Preferably, described sintering temperature is 1180～1200 ℃, and the sintered heat insulating time is 4h.
Rare earth doped bismuth calcium titanate-based luminous piezoelectric ceramic material of the present invention, the single-phase lead-free piezoceramic material of " bismuth stratiform " bismuth calcium titanate for laminated perovskite structure, by technology controlling and process, make the bismuth calcium titanate that itself does not have the characteristics of luminescence have photoluminescence property; And the bismuth calcium titanate-based multifunctional ceramic material of luminous piezoelectricity of the present invention can be excited and red-emitting by the wavelength of UV-light, blue light, three wave bands of green glow, and excites the most by force at blue wave band, belongs to environmentally friendly luminescent material; And praseodymium barium titanate doping calcium diphase ceramic material of the prior art is perovskite structure, and its photoluminescence can only be by ultraviolet excitation.
Bismuth calcium titanate-based luminous piezoelectric ceramic material of the present invention also has photoluminescence property when having original ferroelectric, piezoelectric and dielectric properties, belong to novel multifunctional material.This stupalith has good photoelectric properties, and the field such as, photoelectric sensing integrated, micro electronmechanical at photoelectricity, LED technology has a wide range of applications.
Description of drawings
Fig. 1 CaBi
4-yR
yTi
4O
15, x=1, the XRD figure spectrum of y=0.005,0.01,0.015,0.02 sample.
Fig. 2 CaBi
4-yR
yTi
4O
15, x=1, the exciting light collection of illustrative plates of y=0.005,0.01,0.015,0.02 sample.
Fig. 3 CaBi
4-yR
yTi
4O
15, x=1, the utilizing emitted light collection of illustrative plates of y=0.005,0.01,0.015,0.02 sample.
Embodiment
Further set forth the present invention below in conjunction with specific embodiment, should be understood that these embodiment only are used for explanation the present invention and are not used in restriction protection scope of the present invention.
Embodiment 1
With preparation CaBi
4-0.005Pr
0.005Ti
4O
15, CaBi
4-0.01Pr
0.01Ti
4O
15, CaBi
4-0.015Pr
0.015Ti
4O
15, CaBi
4-0.02Pr
0.02Ti
4O
15Be example, raw material is chosen CaCO
3, Bi
2O
3, TiO
2, Pr
6O
11, press chemical general formula CaBi
4-0.005Pr
0.005Ti
4O
15, CaBi
4-0.01Pr
0.01Ti
4O
15, CaBi
4-0.015Pr
0.015Ti
4O
15, CaBi
4-0.02Pr
0.02Ti
4O
15In the stoichiometric ratio of Ca, Bi, Ti and R take by weighing raw material, take by weighing add that dehydrated alcohol or deionized water grind and mixes behind the raw material in mortar must powder A after abundant
1, A
2, A
3, A
4, the mass ratio of wherein said dehydrated alcohol or deionized water and raw mix is 1～3: 1; The mass ratio of described ball milling material zirconia ball and raw mix is 1～1.5: 1.With powder A
1, A
2, A
3, A
4Place respectively the alumina crucible pre-burning, described calcined temperature is 850 ℃, and temperature rise rate is 3 ℃/min, is incubated after 2 hours, and naturally cooling obtains preburning powdered material B
1, B
2, B
3, B
4With preburning powdered material B
1, B
2, B
3, B
4After grinding respectively, adopt again 10% PVAC polyvinylalcohol as binding agent preburning powdered material B to be carried out granulation, under 100MPa pressure, be pressed into ceramic green sheet C
1, C
2, C
3, C
4With ceramic green sheet C
1, C
2, C
3, C
4After 550 ℃ of lower insulations sticking processing of row in 2 hours, obtained described luminous piezoelectric ceramic material CaBi in 4 hours at 1180 ℃ of lower sintered heat insulatings more respectively
4-0.005Pr
0.005Ti
4O
15, CaBi
4-0.01Pr
0.01Ti
4O
15, CaBi
4-0.015Pr
0.015Ti
4O
15And CaBi
4-0.02Pr
0.02Ti
4O
15
Luminous piezoelectric ceramic material CaBi with gained among the embodiment 1
4-0.005Pr
0.005Ti
4O
15, CaBi
4-0.01Pr
0.01Ti
4O
15, CaBi
4-0.015Pr
0.015Ti
4O
15And CaBi
4-0.02Pr
0.02Ti
4O
15Detect, obtain following Fig. 1, Fig. 2 and Fig. 3:
Fig. 1 is CaBi
4-yR
yTi
4O
15, x=1, the XRD figure spectrum of y=0.005,0.01,0.015,0.02 sample.
Fig. 2 is CaBi
4-yR
yTi
4O
15, x=1, the exciting light collection of illustrative plates of y=0.005,0.01,0.015,0.02 sample.
Fig. 3 is CaBi
4-yR
yTi
4O
15, x=1, the utilizing emitted light collection of illustrative plates of y=0.005,0.01,0.015,0.02 sample.
The luminous piezoelectric ceramic material of composing the embodiment 1 as can be known from the XRD figure of Fig. 1 is single pure phase " bismuth stratiform " bismuth calcium titanate structure, and shows without other dephasign in the XRD figure spectrum; The exciting light collection of illustrative plates of Fig. 2 sample can find out, the luminous piezoelectric ceramic material in the present embodiment all can be excited by the ripple of UV-light (300nm-430nm), blue light (440nm-510nm) or three wave bands of green glow (550nm-570nm); The utilizing emitted light collection of illustrative plates of Fig. 3 sample can be found out, the equal red-emitting of the luminous piezoelectric ceramic material in the present embodiment, and the emission peak position is 614nm.
With preparation Ca
1.5Bi
4-0.01Pr
0.01Ti
4.5O
16.5Be example, raw material is chosen CaCO
3, Bi
2O
3, TiO
2, Pr
6O
11, by prescription Ca
1.5Bi
4-0.01Pr
0.01Ti
4O
16.5The element proportioning takes by weighing selected raw material, and calcined temperature is 900 ℃, and the sticking holding temperature of processing rear ceramic green sheet of row is 1200 ℃, and all the other experiment conditions are consistent with embodiment 1.
After testing as can be known, the gained final sample is luminous piezoelectric ceramic material Ca among the present invention among this embodiment
1.5Bi
4-0.01Pr
0.01Ti
4.5O
16.5
Luminous piezoelectric ceramic material in the present embodiment all can be excited by the ripple of UV-light (300nm-430nm), blue light (440nm-510nm) or three wave bands of green glow (550nm-570nm).
Embodiment 3
With preparation Ca
2Bi
4-0.02Pr
0.02Ti
5O
18Be example, raw material is chosen CaCO
3, Bi
2O
3, TiO
2, Pr
6O
11, by prescription Ca
2Bi
4-0.02Pr
0.02Ti
5O
18The element proportioning takes by weighing selected raw material, and calcined temperature is 950 ℃, and the sticking holding temperature of processing rear ceramic green sheet of row is 1200 ℃, and all the other experiment conditions are consistent with embodiment 1.
After testing as can be known, after testing as can be known, the gained final sample is the luminous piezoelectric ceramic material Ca among the present invention among this embodiment
2Bi
4-0.02Pr
0.02Ti
5O
18
Luminous piezoelectric ceramic material in the present embodiment all can be excited by the ripple of UV-light (300nm-430nm), blue light (440nm-510nm) or three wave bands of green glow (550nm-570nm).
With preparation CaBi
4-0.01Eu
0.01Ti
4O
15Be example, raw material is chosen CaCO
3, Bi
2O
3, TiO
2, Eu
2O
3, by prescription Ca
2Bi
4-0.01Eu
0.01Ti
5O
18The element proportioning takes by weighing selected raw material, and calcined temperature is 850 ℃, and soaking time is 2h, and the sticking holding temperature of processing rear ceramic green sheet of row is 1150 ℃, and soaking time is 6h, and all the other experiment conditions are consistent with embodiment 1.
After testing as can be known, the gained final sample is luminous piezoelectric ceramic material CaBi among the present invention among this embodiment
4-0.01Eu
0.01Ti
4O
15
Luminous piezoelectric ceramic material in the present embodiment all can be excited by the ripple of UV-light (300nm-430nm), blue light (440nm-510nm) or three wave bands of green glow (550nm-570nm).
Embodiment 5
With preparation Ca
2Bi
4-0.02Eu
0.02Ti
5O
18Be example, raw material is chosen CaCO
3, Bi
2O
3, TiO
2, Eu
2O
3, by prescription Ca
2Bi
4-0.02Pr
0.02Ti
5O
18The element proportioning takes by weighing selected raw material, and calcined temperature is 950 ℃, and the sticking holding temperature of processing rear ceramic green sheet of row is 1200 ℃, and all the other experiment conditions are consistent with embodiment 1.
After testing as can be known, the gained final sample is luminous piezoelectric ceramic material Ca among the present invention among this embodiment
2Bi
4-0.02Eu
0.02Ti
5O
18
Luminous piezoelectric ceramic material in the present embodiment all can be excited by the ripple of UV-light (300nm-430nm), blue light (440nm-510nm) or three wave bands of green glow (550nm-570nm).
Embodiment 6
With preparation CaBi
4-0.01Eu
0.01Gd
0.01Ti
4O
15, raw material is chosen CaCO
3, Bi
2O
3, TiO
2, Eu
2O
3, Gd
2O
3, by prescription CaBi
4-0.01Eu
0.01Gd
0.01Ti
4O
15The element proportioning takes by weighing selected raw material, and calcined temperature is 850 ℃, and the sticking holding temperature of processing rear ceramic green sheet of row is 1220 ℃ ℃, and all the other experiment conditions are consistent with embodiment 1.
After testing as can be known, the gained final sample is luminous piezoelectric ceramic material CaBi among the present invention among this embodiment
4-0.01Eu
0.01Gd
0.01Ti
4O
15
Luminous piezoelectric ceramic material in the present embodiment all can be excited by the ripple of UV-light (300nm-430nm), blue light (440nm-510nm) or three wave bands of green glow (550nm-570nm).
Claims (6)
1. bismuth calcium titanate-based luminous piezoelectric ceramic material, its chemical composition meets chemical general formula Ca
xBi
4-yR
yTi
3+xO
12+3x, 1≤x≤2,0.0001≤y≤0.5 wherein, described R is selected from one or more among Pr, Gd, Er, Dy, Tm, Ho, Eu, Yb and the Tb; Described bismuth calcium titanate-based luminous piezoelectric ceramic material is the single-phase lead-free piezoceramic material of laminated perovskite structure " bismuth stratiform " bismuth calcium titanate, and has photoluminescence performance, can be excited and red-emitting by the wavelength of UV-light, blue light, three wave bands of green glow.
2. bismuth calcium titanate-based luminous piezoelectric ceramic material as claimed in claim 1 is characterized in that, the span of y is 0.005≤y≤0.02.
3. bismuth calcium titanate-based luminous piezoelectric ceramic material as claimed in claim 1 or 2 is characterized in that, described bismuth calcium titanate-based luminous piezoelectric ceramic material is for adopting solid reaction process to make.
4. such as the preparation method of the arbitrary described bismuth calcium titanate-based luminous piezoelectric ceramic material of claim 1-3, it is characterized in that, comprise the steps:
(1), according to chemical general formula Ca
xBi
4-yR
yTi
3+xO
12+3xThe stoichiometric ratio of middle Ca, Bi, Ti and R takes by weighing raw material: CaCO
3, Bi
2O
3And TiO
2, and the oxide compound of R or nitrate, wherein 1≤x≤2,0.0001≤y≤0.5;
(2), raw material that step (1) is taken by weighing mixes, add dehydrated alcohol or deionized water through grind or ball milling after, the discharging oven dry obtains powder A;
(3), place the alumina crucible pre-burning to obtain preburning powdered material B powder A, wherein, described calcined temperature is 750～950 ℃, and soaking time is 1～6h;
(4), preburning powdered material B ground or ball milling after, adopting the quality percentage composition is that 8～10% binding agent polyvinyl alcohol carries out granulation to preburning powdered material B, then is pressed into ceramic green sheet C under 10～100MPa pressure;
(5), obtain described bismuth calcium titanate-based luminous piezoelectric ceramic material behind ceramic green sheet C row is sticking, the sintering, wherein, the sticking temperature of described row is 550～600 ℃, and the sticking soaking time of row is 2～4h; Described sintering temperature is 1000～1250 ℃, and the sintered heat insulating time is 2～6h.
5. preparation method as claimed in claim 4 is characterized in that, the mass ratio of described dehydrated alcohol or deionized water and raw material is 1～3:1; The mass ratio of ball milling material zirconia ball and raw material is 1～1.5:1 in the described ball milling.
6. the application in, photoelectric sensing integrated, micro electronmechanical at photoelectricity such as the arbitrary described bismuth calcium titanate-based luminous piezoelectric ceramic material of claim 1-3 and the LED field.
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| CN102276248B (en) * | 2011-04-22 | 2014-07-16 | 同济大学 | Oxide up-conversion luminescence piezoelectric material of bismuth lamellar perovskite structure and preparation method thereof |
| CN103214241A (en) * | 2013-05-03 | 2013-07-24 | 聊城大学 | Barium titanate-based lead-free piezoelectric luminous material and preparation method thereof |
| CN104710173B (en) * | 2015-03-10 | 2017-03-08 | 宁波大学 | Non-plumbum ferroelectric up-conversion fluorescence ceramic material and its preparation method and application |
| CN106910838B (en) * | 2017-03-31 | 2018-10-09 | 华南理工大学 | A kind of perovskite luminescent device and preparation method thereof based on piezoelectric film |
| CN110066173B (en) * | 2019-04-08 | 2021-09-21 | 昆明理工大学 | BaMgSiO4Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material, preparation method and application thereof |
| CN116120054B (en) * | 2023-02-10 | 2024-03-12 | 厦门乃尔电子有限公司 | Bismuth calcium titanate-based piezoelectric ceramic material and preparation method thereof |
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| JP3788198B2 (en) * | 1999-08-26 | 2006-06-21 | 株式会社村田製作所 | Piezoelectric ceramic composition and piezoelectric ceramic element using the same |
| US20080152530A1 (en) * | 2006-12-20 | 2008-06-26 | The Hong Kong Polytechnic University | Method of preparing ferroelectric powders and ceramics |
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