CN104944943A - BNT-base lead-free electrostriction material with light-emitting characteristic and preparation method thereof - Google Patents
BNT-base lead-free electrostriction material with light-emitting characteristic and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of photoelectric functional materials, and provides a BNT-base lead-free electrostriction material with light-emitting characteristic. The chemical composition conforms to the chemical general formula (1-x)(Bi0.5Na0.5)TiO[3]-xM-yR, wherein M is selected from BaTiO3 or (Ba0.90Ca0.10)(Ti0.92Sn0.08)O3, R is selected from one of Pr, Sm, Eu, Tb, Gd, Dy, Er, Ho or Tm, 0.06<= x <=0.09, and 0.001<= y <=0.01. The invention also provides a preparation method and application of the BNT-base lead-free electrostriction material with light-emitting characteristic. The material has the photoluminescent characteristic and excellent zero-lag electrostriction property, and is hopeful to be applied to the technical fields of photoelectric integration, micro electromechanical systems, photoelectric sensing and LEDs (light-emitting diodes).
Description
Technical field
The invention belongs to photoelectric functional material field, relate to a kind of electrostriction material and preparation method, be specifically related to a kind of rear-earth-doped BNT base no-lead electrostrictive material with photoluminescence feature and preparation method.
Background technology
Electrostriction material is the ferroelectric material that a class has diffuse phase transition feature, compares with magnetostriction materials and piezoelectric, have the time of response fast, without delayed, without aging effect, do not need the features such as polarization.So-called electrostrictive effect refers to the telescopic shape change phenomenon that electric field causes, and is solid dielectric induced polarization and a kind of physical phenomenon of occurring under External Electrical Field.Square being directly proportional of Electrostrictive strain S (Δ L/L) and electrostriction coefficient Q and electric field strength E, i.e. S=QP
2=Q ε
2e
2.At present, electrostriction material extensively enters Application Areas, in micrometric displacement transverter, particularly in opticity modulation, change in optical path length be controlled the order of magnitude at wavelength, need the material that can control small size change in displacement.Most of electrostriction material of current application is plumbum-based material, such as lead magnoniobate PMN [J.Kuwata, K.Uchino, S.Nomura, Electrostrictive coefficients of Pb (Mg
1/3nb
2/3) O
3ceramics, Jpn.J.Appl.Phys.1980,19:2099-2103] etc.But traditional lead base electrostriction material contaminate environment, harm humans is healthy, and the electrostriction material therefore researching and developing novel environmental friendly has become various countries and endeavoured one of focus researched and developed.(Na
0.5bi
0.5) TiO
3(BNT) base lead-free ferroelectric material has the relaxation property similar to lead base electrostriction material, and the high electrostrictive property that therefore this material system is potential attracts attention [Adv.Mater.2009,21:4716 – 4720; J.Appl.Phys.2013,113:154102; Appl.Phys.A.2011,104:117 – 122; J.Appl.Phys.2013,114:027004].
In order to adapt to the development of new technology, meet the functionalization of Ferro-Electric Material and Element, miniaturization, intelligentized requirement, investigator is in further investigation with while constantly improving material property, and the function that active development is new with expansion, development has multi-functional ferroelectric material.The piezoelectric ceramics system BaTiO of people's early discoverys such as Wang X S Pr doping
3-CaTiO
3have opto-mechanical-electric multi-functional [CN101343180B], the Bao Dinghua teach problem group of Zhongshan University mixes Bi-stratiform leadless piezoelectric Bi altogether respectively by Eu doping and Er, Yb in the recent period
4ti
3o
12film, observes the Bi after doping
4ti
3o
12film has luminescent properties while having piezoelectric property, thus is expected to use [CN 101337772B] as multifunctional material.For paying close attention to more non-plumbum ferroelectric, piezoelectric in recent years, increasing research is being devoted to carry out the multifunction aspect of this material [such as: bismuth stratified material (CN102276248A); (Ba
0.85ca
0.15) (Zr
0.1ti
0.9) O
3material (CN103122246A); (K
0.5na
0.5) NbO
3sill (CN103265954A); (Bi
0.5na
0.5) TiO
3sill (J.Appl.Phys.2014,116:014102)].Although ferroelectric, the piezoelectric numerous with luminescence feature are developed, but at present investigator pays close attention to is more the piezoelectricity-luminous double characteristic of ferroelectric material, and for both having the characteristics of luminescence, at present also not yet someone reports the multi-functional ferroelectric material of combined with superior electrostrictive effect again.
Summary of the invention
The shortcoming of prior art in view of the above, the object of the present invention is to provide a kind of luminous electrostriction material, this material is a kind of rear-earth-doped BNT base lead-free ferroelectric material, this material is except possessing photoluminescence feature, also there is excellent electrostrictive property, be expected to be applied in the fields such as integrated at photoelectricity, micro electronmechanical, photoelectric sensing and LED technology.
For achieving the above object and other relevant objects, first aspect present invention discloses a kind of BNT base no-lead electrostrictive material with the characteristics of luminescence, and its chemical composition meets chemical general formula: (1-x) (Bi
0.5na
0.5) TiO
3-xM-yR, wherein, M is selected from BaTiO
3or (Ba
0.90ca
0.10) (Ti
0.92sn
0.08) O
3in one, R is selected from the one in Pr, Sm, Eu, Tb, Gd, Dy, Er, Ho or Tm, 0.06≤x≤0.09,0.001≤y≤0.01.
Above-mentioned chemical general formula (1-x) (Bi
0.5na
0.5) TiO
3in-xM-yR, the right index number of element and letter all represent the molar ratio relation of each corresponding element.
Preferably, 0.07≤x≤0.08,0.001≤y≤0.01.
More preferably, 0.001≤y≤0.005.
Preferably, R is selected from the one in Pr, Sm, Eu, Tb, Er or Ho.
Second aspect present invention discloses a kind of preparation method with the BNT base no-lead electrostrictive material of the characteristics of luminescence, comprises the steps:
1) weigh: according to chemical formula (1-x) (Bi
0.5na
0.5) TiO
3in-xM-yR, the stoichiometric ratio of each element takes raw material;
Preferably, step 1) described raw material is the oxide compound of doped element in the oxide compound of component in the oxide compound of matrix element in BNT, M and R.
More preferably, the oxide compound of described matrix element is Bi
2o
3, Na
2cO
3, TiO
2.
More preferably, described M is BaTiO
3time, the oxide compound of described component is TiO
2, BaCO
3; Described M is (Ba
0.90ca
0.10) (Ti
0.92sn
0.08) O
3time, the oxide compound of described component is TiO
2, BaCO
3, CaCO
3, SnO
2.
More preferably, the oxide compound of described doped element is selected from Pr
6o
11, Sm
2o
3, Eu
2o
3, Tb
2o
3, Gd
2o
3, Dy
2o
3, Er
2o
3, Ho
2o
3, Tm
2o
3in one.
2) batch mixing: by step 1) in take powder and put into ball grinder and be mixed with ball milling material, and add zirconium white (ZrO in ball milling material
2) ball and dehydrated alcohol carry out ball milling, discharging obtains mixed powder after drying;
Preferably, the material of described ball grinder is tetrafluoroethylene.
Preferably, the mass ratio of the zirconia ball added described in and ball milling material is 1.0-2.0:1.
More preferably, the mass ratio of the zirconia ball added described in and ball milling material is 1.0-1.5:1.
Preferably, the mass ratio of the dehydrated alcohol added described in and ball milling material is 1.5-3.0:1.
More preferably, the mass ratio of the dehydrated alcohol added described in and ball milling material is 1.5-2.5:1.
Preferably, described ball milling condition is: Ball-milling Time: 10-24h; Rotational speed of ball-mill: 100-200 turns/min.
More preferably, described ball milling condition is: Ball-milling Time: 22-24h; Rotational speed of ball-mill: 150-200 turns/min.
Preferably, the condition that described discharging is dried is: drying time: 4-6 hour; Bake out temperature: 80-100 DEG C.
3) pre-burning: by step 2) in dry after mixed powder briquetting, under air tight condition after pre-burning, obtain pre-fired material;
Preferably, described pre-burning condition is in 800-900 DEG C of pre-burning 2-6h under air tight condition.
More preferably, described pre-burning condition is in 850 DEG C of pre-burning 4h under air tight condition.
4) secondary ball milling: by step 3) pre-fired material again add zirconium white (ZrO
2) ball and dehydrated alcohol carry out ball milling, discharging obtains (1-x) (Bi after drying
0.5na
0.5) TiO
3-xM-yR powder;
Preferably, the zirconia ball added described in and the mass ratio of pre-fired material are 1.0-1.5:1.
Preferably, the dehydrated alcohol added described in and the mass ratio of pre-fired material are 1.5-2.5:1.
Preferably, described ball milling condition is: Ball-milling Time: 10-24h; Rotational speed of ball-mill: 100-200 turns/min.
More preferably, described ball milling condition is: Ball-milling Time: 22-24h; Rotational speed of ball-mill: 150-200 turns/min.
Preferably, the condition that described discharging is dried is: drying time: 4-6 hour; Bake out temperature: 80-100 DEG C.
5) shaping: by step 4) gained powder by the PVAC polyvinylalcohol granulation of 8-10%, obtain required green sheet through compression molding;
Preferably, described powder is 5-7:1 with the mass ratio of interpolation PVA.
Preferably, described forming pressure is 50-100MPa.
More preferably, described forming pressure is 80-100MPa.
Preferably, described green sheet is the disk of diameter 10-15mm, thickness 0.8-1.0mm.
6) sinter: by step 5) green sheet after arranging sticky process, sinter under air tight condition, namely obtain required (1-x) (Bi
0.5na
0.5) TiO
3-xM-yR material.
Preferably, described row glues the condition of process and is: temperature: 500-600 DEG C; Heat-up rate: 40-60 DEG C/h.
Preferably, the condition of described sintering is: sintering temperature: 1120-1180 DEG C; Temperature rise rate: 2-5 DEG C/min; Soaking time: 2-8h.
More preferably, the condition of described sintering is: sintering temperature: 1150 DEG C; Temperature rise rate: 3 DEG C/min; Soaking time: 2h.
Preferably, step 3) pre-burning and step 6) sintering adopts airtight Al
2o
3crucible.
More preferably, step 6) sintering time, airtight Al
2o
3crucible bottom is provided with ZrO
2as bedding and padding.ZrO
2can prevent the high temperature in sintering process from making no-lead electrostrictive material of the present invention and Al as bedding and padding
2o
3crucible adhesion.
Most preferably, step 6) sintering time, airtight Al
2o
3also step 3 is established in crucible) the pre-burning powder prepared is as filler.
There is described in third aspect present invention discloses the application of BNT base no-lead electrostrictive material at photoelectric field of the characteristics of luminescence.
Preferably, described photoelectric field be that photoelectricity is integrated, micro electronmechanical, the technical field of photoelectric sensing and LED.
As mentioned above, a kind of BNT base no-lead electrostrictive material with the characteristics of luminescence of the present invention, has perovskite structure, at matrix bismuth-sodium titanate (Bi
0.5na
0.5) TiO
3middle introducing barium titanate BaTiO
3or titanium barium stannate (Ba
0.90ca
0.10) (Ti
0.92sn
0.08) O
3constituent element, and adulterate obtained by a certain amount of rare earth element.It compared with prior art has following advantage:
(1) the luminous electrostriction material in the present invention, utilize traditional solid phase reaction method preparation, its production technique is simple, cost is low, be easy to suitability for industrialized production, not containing lead element human body and environment being had to severe contamination in prepared luminous electrostriction material, belonging to non-plumbum ferroelectric system material, is a class environmental friendliness shaped material.
(2) the luminous electrostriction material in the present invention, has excellent luminescent properties, can realize photoluminescence under the exciting of certain wavelength light.The color of its photoluminescence carries out tune knot by different rare earth ions, and luminous monochromaticity is good, and intensity is higher, integrated at photoelectricity, photoelectric sensing, and the fields such as LED technology have broad application prospects.
(3) the luminous electrostriction material in the present invention, also has excellent electrostrictive property, keeps the electrostriction coefficient compared favourably with lead base electrostriction material, its electrostriction coefficient Q
33=0.018-0.030m
4c
-2, and to electric field without delayed.This material has excellent antifatigue feature (circulation 10 simultaneously
6, Q
33obviously do not decline) and the feature such as temperature-stable excellent (25-180 DEG C), little to temperature dependency, anti-fatigue performance is good.
Accompanying drawing explanation
Fig. 1: 0.92 (Bi
0.5na
0.5) TiO
3-0.08 (Ba
0.90ca
0.10) (Ti
0.92sn
0.08) O
3the XRD spectrum figure of-0.002Er material.
Fig. 2: 0.92 (Bi
0.5na
0.5) TiO
3-0.08 (Ba
0.90ca
0.10) (Ti
0.92sn
0.08) O
3the utilizing emitted light spectrogram of-0.002Er material under infrared light 980nm excites.
Fig. 3: 0.92 (Bi
0.5na
0.5) TiO
3-0.08 (Ba
0.90ca
0.10) (Ti
0.92sn
0.08) O
3the S-P of-0.002Er material under room temperature 1Hz test condition
2graphic representation.
Fig. 4: 0.92 (Bi
0.5na
0.5) TiO
3-0.08 (Ba
0.90ca
0.10) (Ti
0.92sn
0.08) O
3the electrostriction coefficient Q of-0.002Er material
33with variation relation Fig. 4 a, 4b of temperature and electric field cycle index, wherein,
4a is 0.92 (Bi
0.5na
0.5) TiO
3-0.08 (Ba
0.90ca
0.10) (Ti
0.92sn
0.08) O
3the electrostriction coefficient Q of-0.002Er material
33variation with temperature graph of a relation;
4b is 0.92 (Bi
0.5na
0.5) TiO
3-0.08 (Ba
0.90ca
0.10) (Ti
0.92sn
0.08) O
3the electrostriction coefficient Q of-0.002Er material
33with the variation relation figure of electric field cycle index.
Fig. 5: 0.93 (Bi
0.5na
0.5) TiO
3emmission spectrum Fig. 5 a, 5b, 5c of-0.07BT-0.004R (R=Pr, Sm, Eu) material, wherein,
5a is 0.93 (Bi
0.5na
0.5) TiO
3the utilizing emitted light spectrogram of-0.07BT-0.004Pr material;
5b is 0.93 (Bi
0.5na
0.5) TiO
3the utilizing emitted light spectrogram of-0.07BT-0.004Sm material;
5c is 0.93 (Bi
0.5na
0.5) TiO
3the utilizing emitted light spectrogram of-0.07BT-0.004Eu material.
Fig. 6: 0.93 (Bi
0.5na
0.5) TiO
3the S-P of-0.07BT-0.004R (R=Pr, Sm, Eu) material under room temperature 1Hz test condition
2graphic representation 6a, 6b, 6c, wherein,
6a is 0.93 (Bi
0.5na
0.5) TiO
3the S-P of-0.07BT-0.004Pr material under room temperature 1Hz test condition
2graphic representation;
6b is 0.93 (Bi
0.5na
0.5) TiO
3the S-P of-0.07BT-0.004Sm material under room temperature 1Hz test condition
2graphic representation;
6c is 0.93 (Bi
0.5na
0.5) TiO
3the S-P of-0.07BT-0.004Eu material under room temperature 1Hz test condition
2graphic representation.
Embodiment
Set forth the present invention further below in conjunction with specific embodiment, should be understood that these embodiments are only not used in for illustration of the present invention and limit the scope of the invention.
Below by way of specific specific examples, embodiments of the present invention are described, those skilled in the art the content disclosed by this specification sheets can understand other advantages of the present invention and effect easily.The present invention can also be implemented or be applied by embodiments different in addition, and the every details in this specification sheets also can based on different viewpoints and application, carries out various modification or change not deviating under spirit of the present invention.
Notice, in the following example, the concrete processing unit that indicates or device all adopt conventional equipment in this area or device; All force value and scope all refer to relative pressure, and the raw material of use is also the raw material of the routine use in this area.
In addition should be understood that the one or more method stepss mentioned in the present invention do not repel and can also to there is additive method step or can also insert additive method step before and after described combination step between these steps clearly mentioned, except as otherwise noted; Will also be understood that, the relation that is connected between the one or more equipment/devices mentioned in the present invention is not repelled and can also to be there are other equipment/devices or can also insert other equipment/devices before and after described clustered aggregates/device between these two equipment/devices clearly mentioned, except as otherwise noted.And, except as otherwise noted, the numbering of various method steps is only the convenient tool differentiating various method steps, but not be ordering or the enforceable scope of restriction the present invention of restriction various method steps, the change of its relativeness or adjustment, when changing technology contents without essence, when being also considered as the enforceable category of the present invention.
Embodiment 1
Preparative chemistry general formula is (1-x) (Bi
0.5na
0.5) TiO
3the unleaded luminous electrostriction material of BNT base of-xM-yR, wherein, M=(Ba
0.90ca
0.10) (Ti
0.92sn
0.08) O
3, R=Er, x=0.08, y=0.002,0.004,0.006,0.008,0.010.
With Bi
2o
3, Na
2cO
3, TiO
2, BaCO
3, CaCO
3, SnO
2and Er
2o
3(analytical pure) is raw material, by 0.92 (Bi
0.5na
0.5) TiO
3-0.08 (Ba
0.90ca
0.10) (Ti
0.92sn
0.08) O
3in-yEr (y=0.002,0.004,0.006,0.008,0.010), the stoichiometric ratio (mol ratio) of Bi, Na, Ti, Ba, Ca, Sn and Er takes raw material, uses dehydrated alcohol for medium and uses ZrO
2ball ball milling 24 hours in ball grinder, wherein, rotational speed of ball-mill: 150-200 turns/min, and the mass ratio of the zirconia ball added and ball milling material is 1.5:1, and the mass ratio of the dehydrated alcohol added and ball milling material is 2.0:1.Then, dry, after briquetting, be placed on airtight Al
2o
3in crucible, at 850 DEG C of pre-burning 4h, then the powder after pre-burning is placed in ball grinder again, uses dehydrated alcohol for medium and use ZrO
2ball ball milling 24 hours, wherein, rotational speed of ball-mill: 150-200 turns/min, and the mass ratio of the zirconia ball added and ball milling material is 1.5:1, and the mass ratio of the dehydrated alcohol added and ball milling material is 2.0:1.Add 8%PVA after drying and carry out granulation, powder is 5:1 with the mass ratio of interpolation PVA, then 80MPa obtains the disk of diameter 10mm, thickness 1mm through compression molding, at 550 DEG C of binder removals, finally within 2 hours, namely forms the no-lead electrostrictive material of as above filling a prescription at 1150 DEG C of sintering.
By 0.92 (Bi in above-mentioned gained sample
0.5na
0.5) TiO
3-0.08 (Ba
0.90ca
0.10) (Ti
0.92sn
0.08) O
3-0.002Er no-lead electrostrictive material sample carries out phase structure test, obtains sample XRD figure as shown in Figure 1 spectrum.Be single perovskite structure by thing phase show sample in Fig. 1, not containing Er
2o
3dephasign, this shows that Er element successfully enters 0.92 (Bi
0.5na
0.5) TiO
3-0.08 (Ba
0.90ca
0.10) (Ti
0.92sn
0.08) O
3in parent lattice.
By 0.92 (Bi in above-mentioned gained sample
0.5na
0.5) TiO
3-0.08 (Ba
0.90ca
0.10) (Ti
0.92sn
0.08) O
3-0.002Er no-lead electrostrictive material sample carries out luminescent properties test, obtains the transmitting collection of illustrative plates of sample as shown in Figure 2 under infrared light 980nm excites.There is as shown this sample in Fig. 2 the Up-conversion emission of high strength under infrared light 980nm excites, and launch predominant wavelength at green glow and red spectral band.
By 0.92 (Bi in above-mentioned gained sample
0.5na
0.5) TiO
3-0.08 (Ba
0.90ca
0.10) (Ti
0.92sn
0.08) O
3it is 0.5mm thin slice that the sample disk of-0.002Er no-lead electrostrictive material is polished into thickness through fine sand, is coated to Ag electrode, carries out electrostrictive property test, obtain the S-P of the sample shown in Fig. 3 under room temperature 1Hz test condition in the upper and lower surface of thin slice
2curve.As can be seen from Figure 3 material has the electrostrictive property without electric hysteresis compared favourably with lead base electrostriction material, its electrostriction coefficient Q
33for 0.027m
4/ C
2.Meanwhile, fatigue resistance and temperature stability test are carried out to this no-lead electrostrictive material sample, obtains the Q shown in Fig. 4 a, 4b
33with temperature and electric field cycle index graph of a relation.Q
33to temperature and electric field cycle index insensitive, as shown in Figure 4 b, in circulation 10
6after, Q
33obviously do not decline, anti-fatigue performance is good; Meanwhile, as shown in fig. 4 a, Q
33keep stable 25-180 DEG C of temperature range, little to temperature dependency.
Embodiment 2
Preparative chemistry general formula is (1-x) (Bi
0.5na
0.5) TiO
3the unleaded luminous electrostriction material of BNT base of-xM-yR, wherein, M=(Ba
0.90ca
0.10) (Ti
0.92sn
0.08) O
3, R=Pr, x=0.08, y=0.002,0.004,0.006,0.008,0.010.
With Bi
2o
3, Na
2cO
3, TiO
2, BaCO
3, CaCO
3, SnO
2and Pr
6o
11(analytical pure) is raw material, by 0.92 (Bi
0.5na
0.5) TiO
3-0.08 (Ba
0.90ca
0.10) (Ti
0.92sn
0.08) O
3in-yPr (y=0.002,0.004,0.006,0.008,0.010), the stoichiometric ratio (mol ratio) of Bi, Na, Ti, Ba, Ca, Sn and Pr takes raw material, uses dehydrated alcohol for medium and uses ZrO
2ball ball milling 24 hours in ball grinder, wherein, rotational speed of ball-mill: 150-200 turns/min, and the mass ratio of the zirconia ball added and ball milling material is 1.5:1, and the mass ratio of the dehydrated alcohol added and ball milling material is 2.0:1.Then, dry, after briquetting, be placed on airtight Al
2o
3in crucible, at 850 DEG C of pre-burning 4h, then the powder after pre-burning is placed in ball grinder again, uses dehydrated alcohol for medium and use ZrO
2ball ball milling 24 hours, wherein, rotational speed of ball-mill: 150-200 turns/min, and the mass ratio of the zirconia ball added and ball milling material is 1.5:1, and the mass ratio of the dehydrated alcohol added and ball milling material is 2.0:1.Add 8%PVA after drying and carry out granulation, powder is 5:1 with the mass ratio of interpolation PVA, then 80MPa obtains the disk of diameter 10mm, thickness 1mm through compression molding, at 550 DEG C of binder removals, finally within 2 hours, namely forms the no-lead electrostrictive material of as above filling a prescription at 1150 DEG C of sintering.It is 0.5mm thin slice that the disk of no-lead electrostrictive material is polished into thickness through fine sand, is coated to Ag electrode, tests its electrostrictive property in the upper and lower surface of thin slice.
Prepared no-lead electrostrictive material sample is single perovskite structure, not containing Pr
6o
11dephasign.Sample excitation position is in blue light position, and utilizing emitted light is gold-tinted, it comprises green glow and red light portion.Material has the electrostrictive property without electric hysteresis compared favourably with lead base electrostriction material, this performance to temperature and electric field cycle index insensitive, circulation 10
6, Q
33obviously do not decline, keep stable at 25-180 DEG C, therefore, little to temperature dependency, anti-fatigue performance is good.
Embodiment 3
Preparative chemistry general formula is (1-x) (Bi
0.5na
0.5) TiO
3the unleaded luminous electrostriction material of BNT base of-xM-yR, wherein, M=BaTiO
3, R=Er, x=0.07, y=0.002,0.004,0.006,0.008,0.010.
With Bi
2o
3, Na
2cO
3, TiO
2, BaCO
3and Er
2o
3(analytical pure) is raw material, by 0.92 (Bi
0.5na
0.5) TiO
3-0.07BaTiO
3in-yEr (y=0.002,0.004,0.006,0.008,0.010), the stoichiometric ratio (mol ratio) of Bi, Na, Ti, Ba and Er takes raw material, uses dehydrated alcohol for medium and uses ZrO
2ball ball milling 24 hours in ball grinder, wherein, rotational speed of ball-mill: 150-200 turns/min, and the mass ratio of the zirconia ball added and ball milling material is 1.5:1, and the mass ratio of the dehydrated alcohol added and ball milling material is 2.0:1.Then, dry, after briquetting, be placed on airtight Al
2o
3in crucible, at 850 DEG C of pre-burning 4h, then the powder after pre-burning is placed in ball grinder again, uses dehydrated alcohol for medium and use ZrO
2ball ball milling 24 hours, wherein, rotational speed of ball-mill: 150-200 turns/min, and the mass ratio of the zirconia ball added and ball milling material is 1.5:1, and the mass ratio of the dehydrated alcohol added and ball milling material is 2.0:1.Add 8%PVA after drying and carry out granulation, powder is 5:1 with the mass ratio of interpolation PVA, then 80MPa obtains the disk of diameter 10mm, thickness 1mm through compression molding, at 550 DEG C of binder removals, finally within 2 hours, namely forms the no-lead electrostrictive material of as above filling a prescription at 1150 DEG C of sintering.It is 0.5mm thin slice that the disk of no-lead electrostrictive material is polished into thickness through fine sand, is coated to Ag electrode, tests its electrostrictive property in the upper and lower surface of thin slice.
Prepared no-lead electrostrictive material sample is single perovskite structure, not containing Er
2o
3dephasign.This sample has the Up-conversion emission of high strength under blue light 980nm excites, and launches predominant wavelength at green glow and red spectral band.Material has the electrostrictive property without electric hysteresis compared favourably with lead base electrostriction material, this performance to temperature and electric field cycle index insensitive, circulation 10
6, Q
33obviously do not decline, keep stable at 25-180 DEG C, therefore, little to temperature dependency, anti-fatigue performance is good.
Embodiment 4
Preparative chemistry general formula is (1-x) (Bi
0.5na
0.5) TiO
3the unleaded luminous electrostriction material of BNT base of-xM-yR, wherein, M=BaTiO
3, R=Pr, x=0.07, y=0.002,0.004,0.006,0.008,0.010.
With Bi
2o
3, Na
2cO
3, TiO
2, BaCO
3and Pr
6o
11(analytical pure) is raw material, by 0.93 (Bi
0.5na
0.5) TiO
3-0.07BaTiO
3in-yPr (y=0.002,0.004,0.006,0.008,0.010), the stoichiometric ratio (mol ratio) of Bi, Na, Ti, Ba and Pr takes raw material, uses dehydrated alcohol for medium and uses ZrO
2ball ball milling 24 hours in ball grinder, wherein, rotational speed of ball-mill: 150-200 turns/min, and the mass ratio of the zirconia ball added and ball milling material is 1.5:1, and the mass ratio of the dehydrated alcohol added and ball milling material is 2.0:1.Then, dry, after briquetting, be placed on airtight Al
2o
3in crucible, at 850 DEG C of pre-burning 4h, then the powder after pre-burning is placed in ball grinder again, uses dehydrated alcohol for medium and use ZrO
2ball ball milling 24 hours, wherein, rotational speed of ball-mill: 150-200 turns/min, and the mass ratio of the zirconia ball added and ball milling material is 1.5:1, and the mass ratio of the dehydrated alcohol added and ball milling material is 2.0:1.Add 8%PVA after drying and carry out granulation, powder is 5:1 with the mass ratio of interpolation PVA, then 80MPa obtains the disk of diameter 10mm, thickness 1mm through compression molding, at 550 DEG C of binder removals, finally within 2 hours, namely forms the no-lead electrostrictive material of as above filling a prescription at 1150 DEG C of sintering.
By 0.93 (Bi in above-mentioned gained sample
0.5na
0.5) TiO
3-0.07BaTiO
3-0.004Pr no-lead electrostrictive material sample carries out phase structure test, and sample is single perovskite structure, not containing Pr
6o
11dephasign, shows that Pr element successfully enters 0.93 (Bi
0.5na
0.5) TiO
3-0.07BaTiO
3in parent lattice.
By 0.93 (Bi in above-mentioned gained sample
0.5na
0.5) TiO
3-0.07BaTiO
3-0.004Pr no-lead electrostrictive material sample carries out luminescent properties test, obtains the utilizing emitted light spectrogram of sample as shown in Figure 5 a.Excite predominant wavelength at the blue wave band of 430-500nm as what show this sample in Fig. 5 a, excite main peak at 473nm, this phosphor emission peak wavelength 565-670nm wave band is green glow and red spectral band.
By 0.93 (Bi in above-mentioned gained sample
0.5na
0.5) TiO
3-0.07BaTiO
3it is 0.5mm thin slice that the sample disk of-0.004Pr no-lead electrostrictive material is polished into thickness through fine sand, is coated to Ag electrode, carries out electrostrictive property test in the upper and lower surface of thin slice, obtains the S-P of sample under room temperature 1Hz test condition as shown in Figure 6 a
2curve.Can find out that from Fig. 6 a material has the electrostrictive property without electric hysteresis compared favourably with lead base electrostriction material, its electrostriction coefficient Q
33for 0.029m
4/ C
2, Q simultaneously
33to temperature and electric field cycle index insensitive, circulation 10
6, Q
33obviously do not decline, keep stable at 25-180 DEG C, therefore, little to temperature dependency, anti-fatigue performance is good.
Embodiment 5
Preparative chemistry general formula is (1-x) (Bi
0.5na
0.5) TiO
3the unleaded luminous electrostriction material of BNT base of-xM-yR, wherein, M=BaTiO
3, R=Sm, x=0.07, y=0.002,0.004,0.006,0.008,0.010.
With Bi
2o
3, Na
2cO
3, TiO
2, BaCO
3and Sm
2o
3(analytical pure) is raw material, by 0.93 (Bi
0.5na
0.5) TiO
3-0.07BaTiO
3in-ySm (y=0.002,0.004,0.006,0.008,0.010), the stoichiometric ratio (mol ratio) of Bi, Na, Ti, Ba and Sm takes raw material, uses dehydrated alcohol for medium and uses ZrO
2ball ball milling 24 hours in ball grinder, wherein, rotational speed of ball-mill: 150-200 turns/min, and the mass ratio of the zirconia ball added and ball milling material is 1.5:1, and the mass ratio of the dehydrated alcohol added and ball milling material is 2.0:1.Then, dry, after briquetting, be placed on airtight Al
2o
3in crucible, at 850 DEG C of pre-burning 4h, then the powder after pre-burning is placed in ball grinder again, uses dehydrated alcohol for medium and use ZrO
2ball ball milling 24 hours, wherein, rotational speed of ball-mill: 150-200 turns/min, and the mass ratio of the zirconia ball added and ball milling material is 1.5:1, and the mass ratio of the dehydrated alcohol added and ball milling material is 2.0:1.Add 8%PVA after drying and carry out granulation, powder is 5:1 with the mass ratio of interpolation PVA, then 80MPa obtains the disk of diameter 10mm, thickness 1mm through compression molding, at 550 DEG C of binder removals, finally within 2 hours, namely forms the no-lead electrostrictive material of as above filling a prescription at 1150 DEG C of sintering.
By 0.93 (Bi in above-mentioned gained sample
0.5na
0.5) TiO
3-0.07BaTiO
3-0.004Sm no-lead electrostrictive material sample carries out phase structure test, and sample is single perovskite structure, not containing Sm
2o
3dephasign, shows that Sm element successfully enters 0.93 (Bi
0.5na
0.5) TiO
3-0.07BaTiO
3in parent lattice.
By 0.93 (Bi in above-mentioned gained sample
0.5na
0.5) TiO
3-0.07BaTiO
3-0.004Sm no-lead electrostrictive material sample carries out luminescent properties test, obtains the utilizing emitted light spectrogram of result sample as shown in Figure 5 b.Excitation wavelength as shown this sample in Fig. 5 b is positioned at the scope of 400-500nm, matches with the luminescent spectrum of the LED blue chip of commercialization.The main peak of its emission spectrum is positioned at the red emission of 600nm, and affiliated emission band is 550-720nm, is gold-tinted and red spectral band.
By 0.93 (Bi in above-mentioned gained sample
0.5na
0.5) TiO
3-0.07BaTiO
3it is 0.5mm thin slice that the sample disk of-0.004Sm no-lead electrostrictive material is polished into thickness through fine sand, is coated to Ag electrode, carries out electrostrictive property test in the upper and lower surface of thin slice, obtains the S-P of sample under room temperature 1Hz test condition as shown in Figure 6 b
2curve.Can find out that from Fig. 6 b material has the electrostrictive property without electric hysteresis compared favourably with lead base electrostriction material, its electrostriction coefficient Q
33for 0.020m
4/ C
2, Q simultaneously
33to temperature and electric field cycle index insensitive, circulation 10
6, Q
33obviously do not decline, keep stable at 25-180 DEG C, therefore, little to temperature dependency, anti-fatigue performance is good.
Embodiment 6
Preparative chemistry general formula is (1-x) (Bi
0.5na
0.5) TiO
3the unleaded luminous electrostriction material of BNT base of-xM-yR, wherein, M=BaTiO
3, R=Eu, x=0.07, y=0.002,0.004,0.006,0.008,0.010.
With Bi
2o
3, Na
2cO
3, TiO
2, BaCO
3and Eu
2o
3(analytical pure) is raw material, by 0.93 (Bi
0.5na
0.5) TiO
3-0.07BaTiO
3in-yEu (y=0.002,0.004,0.006,0.008,0.010), the stoichiometric ratio (mol ratio) of Bi, Na, Ti, Ba and Eu takes raw material, uses dehydrated alcohol for medium and uses ZrO
2ball ball milling 24 hours in ball grinder, wherein, rotational speed of ball-mill: 150-200 turns/min, and the mass ratio of the zirconia ball added and ball milling material is 1.5:1, and the mass ratio of the dehydrated alcohol added and ball milling material is 2.0:1.Then, dry, after briquetting, be placed on airtight Al
2o
3in crucible, at 850 DEG C of pre-burning 4h, then the powder after pre-burning is placed in ball grinder ball milling 24 hours again, wherein, rotational speed of ball-mill: 150-200 turns/min, and the mass ratio of the zirconia ball added and ball milling material is 1.5:1, and the mass ratio of the dehydrated alcohol added and ball milling material is 2.0:1.Add 8%PVA after drying and carry out granulation, powder is 5:1 with the mass ratio of interpolation PVA, then 80MPa obtains the disk of diameter 10mm, thickness 1mm through compression molding, at 550 DEG C of binder removals, finally within 2 hours, namely forms the no-lead electrostrictive material of as above filling a prescription at 1150 DEG C of sintering.
By 0.93 (Bi in above-mentioned gained sample
0.5na
0.5) TiO
3-0.07BaTiO
3-0.004Eu no-lead electrostrictive material sample carries out phase structure test, and sample is single perovskite structure, not containing Eu
2o
3dephasign, shows that Eu element successfully enters 0.93 (Bi
0.5na
0.5) TiO
3-0.07BaTiO
3in parent lattice.
By 0.93 (Bi in above-mentioned gained sample
0.5na
0.5) TiO
3-0.07BaTiO
3-0.004Eu no-lead electrostrictive material sample carries out luminescent properties test, obtains the utilizing emitted light spectrogram of result sample as shown in Figure 5 c.As shown the blue wave band of transmitting predominant wavelength at 450-550nm of this sample in Fig. 5 c, excite main peak at 526nm, this phosphor emission peak wavelength 550-720nm wave band is gold-tinted and red spectral band.
By 0.93 (Bi in above-mentioned gained sample
0.5na
0.5) TiO
3-0.07BaTiO
3it is 0.5mm thin slice that the sample disk of-0.004Eu no-lead electrostrictive material is polished into thickness through fine sand, is coated to Ag electrode, carries out electrostrictive property test in the upper and lower surface of thin slice, obtains the S-P of sample under room temperature 1Hz test condition as fig. 6 c
2curve.Can find out that from Fig. 6 c material has the electrostrictive property without electric hysteresis compared favourably with lead base electrostriction material, its electrostriction coefficient Q
33for 0.019m
4/ C
2, Q simultaneously
33to temperature and electric field cycle index insensitive, circulation 10
6, Q
33obviously do not decline, keep stable at 25-180 DEG C, therefore, little to temperature dependency, anti-fatigue performance is good.
Embodiment 7
Preparative chemistry general formula is (1-x) (Bi
0.5na
0.5) TiO
3the unleaded luminous electrostriction material of BNT base of-xM-yR, wherein, M=(Ba
0.90ca
0.10) (Ti
0.92sn
0.08) O
3, R=Tb, x=0.08, y=0.002,0.004,0.006,0.008,0.010.
With Bi
2o
3, Na
2cO
3, TiO
2, BaCO
3, CaCO
3, SnO
2and Tb
2o
3(analytical pure) is raw material, by 0.92 (Bi
0.5na
0.5) TiO
3-0.08 (Ba
0.90ca
0.10) (Ti
0.92sn
0.08) O
3in-y Tb (y=0.002,0.004,0.006,0.008,0.010), the stoichiometric ratio (mol ratio) of Bi, Na, Ti, Ba, Ca, Sn and Tb takes raw material, uses dehydrated alcohol for medium and uses ZrO
2ball ball milling 22 hours in ball grinder, wherein, rotational speed of ball-mill: 100 turns/min, the mass ratio of the zirconia ball added and ball milling material is 2.0:1, and the mass ratio of the dehydrated alcohol added and ball milling material is 3.0:1.Then, dry, after briquetting, be placed on airtight Al
2o
3in crucible, at 800 DEG C of pre-burning 6h, then the powder after pre-burning is placed in ball grinder again, uses dehydrated alcohol for medium and use ZrO
2ball ball milling 22 hours, wherein, rotational speed of ball-mill: 100 turns/min, the mass ratio of the zirconia ball added and ball milling material is 1.5:1, and the mass ratio of the dehydrated alcohol added and ball milling material is 2.5:1.Add 10%PVA after drying and carry out granulation, powder is 7:1 with the mass ratio of interpolation PVA, then 100MPa obtains the disk of diameter 15mm, thickness 0.8mm through compression molding, at 500 DEG C of binder removals, finally within 4 hours, namely forms the lead-free ferroelectric material of as above filling a prescription at 1120 DEG C of sintering.It is 0.5mm thin slice that the disk of lead-free ferroelectric material is polished into thickness through fine sand, is coated to Ag electrode, tests its electrostrictive property in the upper and lower surface of thin slice.
Prepared sample is single perovskite structure, not containing Tb
2o
3dephasign.Sample has excellent luminescent properties, and material has the electrostrictive property without electric hysteresis compared favourably with lead base electrostriction material simultaneously, this performance to temperature and electric field cycle index insensitive, circulate 10
6, Q
33obviously do not decline, keep stable at 25 ~ 180 DEG C, therefore, little to temperature dependency, anti-fatigue performance is good.
Embodiment 8
Preparative chemistry general formula is (1-x) (Bi
0.5na
0.5) TiO
3the unleaded luminous electrostriction material of BNT base of-xM-yR, wherein, M=BaTiO
3, R=Ho, x=0.07, y=0.002,0.004,0.006,0.008,0.010.
With Bi
2o
3, Na
2cO
3, TiO
2, BaCO
3and Ho
2o
3(analytical pure) is raw material, by 0.92 (Bi
0.5na
0.5) TiO
3-0.07BaTiO
3in-yHo (y=0.002,0.004,0.006,0.008,0.010), the stoichiometric ratio (mol ratio) of Bi, Na, Ti, Ba and Ho takes raw material, uses dehydrated alcohol for medium and uses ZrO
2ball ball milling 23 hours in ball grinder, wherein, rotational speed of ball-mill: 200 turns/min, the mass ratio of the zirconia ball added and ball milling material is 1.0:1, and the mass ratio of the dehydrated alcohol added and ball milling material is 1.0:1.Then, dry, after briquetting, be placed on airtight Al
2o
3in crucible, at 900 DEG C of pre-burning 2h, then the powder after pre-burning is placed in ball grinder again, uses dehydrated alcohol for medium and use ZrO
2ball ball milling 23 hours, wherein, rotational speed of ball-mill: 200 turns/min, the mass ratio of the zirconia ball added and ball milling material is 1.0:1, and the mass ratio of the dehydrated alcohol added and ball milling material is 1.5:1.Add 9%PVA after drying and carry out granulation, powder is 6:1 with the mass ratio of interpolation PVA, then 90MPa obtains the disk of diameter 10mm, thickness 1mm through compression molding, at 600 DEG C of binder removals, finally within 2 hours, namely forms the lead-free ferroelectric material of as above filling a prescription at 1180 DEG C of sintering.It is 0.5mm thin slice that the disk of lead-free ferroelectric material is polished into thickness through fine sand, is coated to Ag electrode, tests its electrostrictive property in the upper and lower surface of thin slice.
Prepared sample is single perovskite structure, not containing Ho
2o
3dephasign.Sample has excellent luminescent properties, and material has the electrostrictive property without electric hysteresis compared favourably with lead base electrostriction material simultaneously, this performance to temperature and electric field cycle index insensitive, circulate 10
6, Q
33obviously do not decline, keep stable at 25 ~ 180 DEG C, therefore, little to temperature dependency, anti-fatigue performance is good.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (10)
1. have a BNT base no-lead electrostrictive material for the characteristics of luminescence, its chemical composition meets chemical general formula: (1-x) (Bi
0.5na
0.5) TiO
3-xM-yR, wherein, M is selected from BaTiO
3or (Ba
0.90ca
0.10) (Ti
0.92sn
0.08) O
3in one, R is selected from the one in Pr, Sm, Eu, Tb, Gd, Dy, Er, Ho or Tm, 0.06≤x≤0.09,0.001≤y≤0.01.
2. there is a preparation method for the BNT base no-lead electrostrictive material of the characteristics of luminescence, comprise the steps:
1) weigh: according to chemical formula (1-x) (Bi
0.5na
0.5) TiO
3in-xM-yR, the stoichiometric ratio of each element takes raw material;
2) batch mixing: by step 1) in take powder and put into ball grinder and be mixed with ball milling material, and in ball milling material, add zirconia ball and dehydrated alcohol carries out ball milling, discharging obtains mixed powder after drying;
3) pre-burning: by step 2) in dry after mixed powder briquetting, under air tight condition after pre-burning, obtain pre-fired material;
4) secondary ball milling: by step 3) pre-fired material again add zirconia ball and dehydrated alcohol carries out ball milling, discharging obtains (1-x) (Bi after drying
0.5na
0.5) TiO
3-xM-yR powder;
5) shaping: by step 4) gained powder by the PVAC polyvinylalcohol granulation of 8-10%, obtain required green sheet through compression molding;
6) sinter: by step 5) green sheet after arranging sticky process, sinter under air tight condition, namely obtain required (1-x) (Bi
0.5na
0.5) TiO
3-xM-yR material.
3. there is the preparation method of the BNT base no-lead electrostrictive material of the characteristics of luminescence according to claim 2, it is characterized in that, step 1) in, described raw material is the oxide compound of doped element in the oxide compound of component in the oxide compound of matrix element in BNT, M and R.
4. there is the preparation method of the BNT base no-lead electrostrictive material of the characteristics of luminescence according to claim 2, it is characterized in that, step 2) in, described in the mass ratio of the zirconia ball that adds and ball milling material be 1.0-2.0:1; The mass ratio of the described dehydrated alcohol that adds and ball milling material is 1.5-3.0:1.
5. there is the preparation method of the BNT base no-lead electrostrictive material of the characteristics of luminescence according to claim 2, it is characterized in that, step 3) in, described pre-burning condition is in 800-900 DEG C of pre-burning 2-6h under air tight condition.
6. there is the preparation method of the BNT base no-lead electrostrictive material of the characteristics of luminescence according to claim 2, it is characterized in that, step 4) in, described in the mass ratio of the zirconia ball that adds and pre-fired material be 1.0-1.5:1; The mass ratio of the described dehydrated alcohol that adds and pre-fired material is 1.5-2.5:1.
7. there is the preparation method of the BNT base no-lead electrostrictive material of the characteristics of luminescence according to claim 2, it is characterized in that, step 5) in, described powder is 5-7:1 with the mass ratio of interpolation PVA.
8. there is the preparation method of the BNT base no-lead electrostrictive material of the characteristics of luminescence according to claim 2, it is characterized in that, step 6) in, the condition that described row glues process is: temperature: 500-600 DEG C, heat-up rate: 40-60 DEG C/h; The condition of described sintering is: sintering temperature: 1120-1180 DEG C, temperature rise rate: 2-5 DEG C/min, soaking time: 2-8h.
9. there is the application of BNT base no-lead electrostrictive material at photoelectric field of the characteristics of luminescence according to claim 1.
10. application according to claim 9, is characterized in that, described photoelectric field is that photoelectricity is integrated, micro electronmechanical, the technical field of photoelectric sensing and LED.
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