CN109957837A - A kind of neodymium doping lead magnesium niobate-lead titanate material and preparation method thereof - Google Patents
A kind of neodymium doping lead magnesium niobate-lead titanate material and preparation method thereof Download PDFInfo
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7756—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing neodynium
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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Abstract
This application discloses a kind of neodymiums to adulterate lead magnesium niobate-lead titanate material, and the ferroelectricity luminescent material including it is rare earth doped ABO3Type perovskite oxide material.The material combines the excellent ferroelectricity of ferroelectric material, piezoelectric property and the good characteristics of luminescence of rare earth element, so that the material has the electric field-tunable of luminescent properties, it is a kind of multifunctional material with ferroelectricity, piezoelectricity and luminescent properties.
Description
Technical field
This application involves a kind of neodymiums to adulterate lead magnesium niobate-lead titanate material, belongs to the luminous multifunctional material field of ferroelectricity.
Background technique
An important directions of the intellectual material as Modern High-Tech's new material development, need to realize structure function, function
It can diversification.Just include in the perceptional function that intellectual material should have be able to detect and identify extraneous or internal electricity, light,
Heat, stress and strain etc., new material proposed by the present invention are exactly the multi-functional material with ferroelectricity, piezoelectric property and luminescent properties
Material, can be realized the diversification of function, and in addition to perceptional function can also play driving function in the case where receiving environmental stimuli, response is extraneous
Variation.
Current most luminescent material is concentrated mainly in the research of optical property, is had a single function, it is difficult to realize material
Multifunction.The ferroelectric material of perovskite structure has the electric properties such as excellent ferroelectricity, piezoelectricity, dielectric, electric light, in electronics
Industry and optical field have potential application.There can be iron simultaneously by the luminescent material of matrix of ferroelectric material
Electricity, piezoelectricity and optical property, accelerate multifunction, the integration and miniaturization of device.Current ferroelectricity luminescent material focuses mostly on
In polycrystalline ceramic, application prospect is restricted, and luminescence band is concentrated mainly on visibility region.In ferroelectricity luminescent material
Luminescent properties influenced by many factors such as crystal symmetry, polarization, polarization overturnings, but the polycrystalline characteristic of ceramic material is difficult to
The influence of analyzing crystal symmetry, polarization, polarization overturning to luminescent properties.
Summary of the invention
An aspect of of the present present invention provides a kind of neodymium doping lead magnesium niobate-lead titanate material, and the neodymium adulterates lead magnesio-niobate-
Metatitanic acid lead material has perovskite type crystal structure.
Perovskite structure can use ABO3It indicates, A cations are in 12 coordination structures, positioned at what is be made of B octahedrons
In gap.
In a preferred embodiment, the chemical formula of the neodymium doping lead magnesium niobate-lead titanate material is (NdxPb1-3x/2)
[(Mg1/3Nb2/3)1-yTiy]O3;
Wherein, 0.01≤x≤0.05,0.28≤y≤0.65;
Preferably, x=0.02,0.31≤y≤0.39.
Another aspect provides a kind of preparation method of neodymium doping lead magnesium niobate-lead titanate material, the sides
Method at least includes the following steps:
A) after mixing the raw material containing neodymium source, lead source, magnesium source, niobium source, titanium source with fluxing agent, 900~1100 DEG C are placed in
Constant temperature is no less than 12 hours, obtains initial melt;
B) seed crystal is contacted with initial melt, grows to obtain the neodymium doping lead magnesio-niobate-metatitanic acid using top-seeded solution growth
Lead material.
In a preferred embodiment, neodymium source described in step a) is Nd2O3, lead source is PbO, and magnesium source is MgO, and niobium source is
Nb2O5, titanium source TiO2;
The fluxing agent is PbO and B2O3Mixture.
In a preferred embodiment, the rubbing containing neodymium source, lead source, magnesium source, niobium source, the raw material of titanium source and fluxing agent
You are than being 1:2~10.
In a preferred embodiment, the condition of step b) the top-seeded solution growth growth are as follows:
Rate of temperature fall are as follows: 1~5 DEG C/day;
The rate of seed rod rotation are as follows: 0~20/ minute.
It is yet another aspect of the present invention to provide a kind of ferroelectricity luminescent materials, adulterate lead magnesium niobate-lead titanate containing above-mentioned neodymium
Material adulterates lead magnesium niobate-lead titanate material according to the neodymium that the above method is prepared.
The material is realized by rare earth ion doped perovskite ferroelectric monocrystal material with piezoelectricity, ferroelectricity and photism
The preparation of multifunctional material and the research of performance of energy and the real-time monitoring photoluminescence intensity of electric field are that a kind of ferroelectricity is luminous more
Functional material.
In a preferred embodiment, the neodymium doping lead magnesium niobate-lead titanate material has ferroelectric hysteresis loop, coercive field model
It is trapped among 1.5~18kV/cm, residual polarization range is in 14~36.7 μ C/cm2。
In a preferred embodiment, luminescence generated by light central wavelength applied by the ferroelectricity luminescent material is located at least in
Near 879nm and 1061nm.
In a preferred embodiment, the photoluminescence intensity of the ferroelectricity luminescent material can by modulation electric field strength into
Row real-time monitoring.
The beneficial effect that the application can generate includes:
1) ferroelectricity luminescent material provided herein combines the excellent ferroelectricity of ferroelectric material, piezoelectric property and rare earth
The good characteristics of luminescence of element, so that the material has the electric field-tunable of luminescent properties, it is a kind of with ferroelectricity, piezoelectricity and hair
The multifunctional material of optical property;
2) ferroelectricity luminescent material provided herein, coercive field EcFor 1.5~18kV/cm, remanent polarization PrIt is 14
~36.7 μ C/cm2;
3) ferroelectricity luminescent material provided herein increases to about 3 times of coercive fields, the material by 0kV/cm in extra electric field
Expect that concussion variation occurs under electric regulation degree in the fluorescence intensity of 879nm and 1061nm wave band.
4) preparation method of neodymium provided herein doping lead magnesium niobate-lead titanate material, can get centimetres
Large single crystal sample.
Detailed description of the invention
Fig. 1 is the sample 1 in embodiment 1#(NdxPb1-3x/2)[(Mg1/3Nb2/3)1-yTiy]O3(x=0.02, y=0.39)
Ferroelectricity shines the monocrystalline figure of monocrystal material X-ray powder diffraction figure at room temperature and growth.
Fig. 2 is the sample 1 in embodiment 1#(NdxPb1-3x/2)[(Mg1/3Nb2/3)1-yTiy]O3(x=0.02, y=0.39)
Ferroelectricity shines the dielectric thermogram of monocrystal material at different frequencies.
Fig. 3 is the sample 1 in embodiment 1#(NdxPb1-3x/2)[(Mg1/3Nb2/3)1-yTiy]O3(x=0.02, y=0.39)
Ferroelectric hysteresis loop of the monocrystal material under not same electric field.
Fig. 4 is the sample 1 in embodiment 1#(NdxPb1-3x/2)[(Mg1/3Nb2/3)1-yTiy]O3(x=0.02, y=0.39)
Monocrystal material is in the real-time emission spectrum applied under not same electric field.
Specific embodiment
The application is described in detail below with reference to embodiment, but the application is not limited to these embodiments.
Unless otherwise instructed, the raw material in embodiments herein is bought by commercial sources.
In embodiment, unless otherwise instructed, analytical test strip part is as follows:
X-ray powder diffraction uses Rigaku X-ray diffractometer (Rigaku diffractometer
MiniFlex600 the powder sample of crystal) is measured;
The testing impedance system for the concept40 impedance analyzer that measurement is produced using Novocontrol company, Germany
It unites (Novocontrol Alpha-A);
The TF2000 ferroelectric properties test macro that ferroelectricity test is produced using aixACCT company, Germany;
Fluorescence spectral measuring using Britain Edinburgh Instruments company production FLS980 it is ultraviolet-near-infrared
Steady transient state Fluorescence Spectrometer.
1 sample 1 of embodiment#Preparation
1) since there are the effects of segregation, first according to general formula (NdxPb1-3x/2)[(Mg1/3Nb2/3)1-yTiy]O3, wherein x=
0.02, y=0.42, stoichiometric ratio weighs Nd2O3、PbO、MgO、Nb2O5、TiO2, as solute;
2) select fluxing agent for PbO and B2O3Mixture, molar ratio 10:1, choose solute and solvent molar ratio
Example meets 1:9, and solute and solvent are sufficiently mixed, and uses for crystal growth;
3) it is put into the mixture of solute and solvent as the initial feed of crystal growth in platinum crucible, in 1100 DEG C of perseverances
Temperature melts the initial feed in crucible sufficiently uniformly, is made using lead magnesium niobate-lead titanate (PMNT) monocrystalline of required component
For seed crystal, seed crystal is slowly drop down to ullage at 960 DEG C, the saturated solution after seed crystal preheating, in decline seed crystal and crucible
Liquid level contact.Then Slow cooling is carried out according still further to daily 3~4 DEG C of rate to grow monocrystalline, the speed of rotation of seed rod is
5/ minute.
4) since there are the component effects of segregation in the crystal growing process, the monocrystalline component that said components obtain is:
(NdxPb1-3x/2)[(Mg1/3Nb2/3)1-yTiy]O3, x=0.02, y=0.39.Therefore the segregation coefficient of Ti is in above-mentioned crystal
0.9, the monocrystal material of target proportion can be obtained according to the proportion of segregation coefficient adjustment solute material.
Gained neodymium adulterates lead magnesium niobate-lead titanate large single crystal sample, is denoted as sample 1#.Sample 1#For 22mm × 23mm × 8mm
Cuboid-type monocrystalline.
Embodiment 2: sample 2#Preparation
1) since there are the effects of segregation, first according to general formula (NdxPb1-3x/2)[(Mg1/3Nb2/3)1-yTiy]O3, wherein x=
0.02, y=0.34, stoichiometric ratio weighs Nd2O3、PbO、MgO、Nb2O5、TiO2, as solute;
2) select fluxing agent for PbO and B2O3Mixture, molar ratio 10:1, choose solute and solvent molar ratio
Meet 1:9, solute and solvent are sufficiently mixed, for crystal growth use;
3) it is put into the mixture of solute and solvent as the initial feed of crystal growth in platinum crucible, in 1000 DEG C of perseverances
Temperature melts the initial feed in crucible sufficiently uniformly, will at 940 DEG C using the PMNT monocrystalline of required component as seed crystal
Seed crystal is slowly drop down to ullage, and after seed crystal preheating, decline seed crystal is contacted with the saturated solution liquid level in crucible.Then it presses again
Slow cooling next life long crystal is carried out according to daily 3 DEG C of rate, the speed of rotation of seed rod is 10/ minute.
4) since there are the component effects of segregation in the crystal growing process, the monocrystalline component that said components obtain is:
(NdxPb1-3x/2)[(Mg1/3Nb2/3)1-yTiy]O3, x=0.02, y=0.31.Therefore the segregation coefficient of Ti is in above-mentioned crystal
0.9, the monocrystal material of target proportion can be obtained according to the proportion of segregation coefficient adjustment solute material.
Gained neodymium adulterates lead magnesium niobate-lead titanate large single crystal sample, is denoted as sample 2#.Sample 2#For 20mm × 20mm × 8mm
Cuboid-type monocrystalline.
3 sample 3 of embodiment#With sample 4#Preparation
Sample 3#With sample 4#Used raw material, method and the specific steps are the same as those in embodiment 1, the difference is that, adjustment
Raw material proportioning and the condition of top-seeded solution growth growth, specific as shown in table 1:
Table 1
4 sample 1 of embodiment#~sample 4#Object mutually characterize
Sample 1 is cut respectively#~sample 4#Fraction crystal grind into powder, using XRD diffractometer carry out object mutually really
It is fixed, the results show that sample 1#~sample 4#It is high-purity perovskite crystal material, with sample 1#For Typical Representative, sample shines
Piece and X-ray powder diffraction figure are as shown in Figure 1.
5 sample 1 of embodiment#~sample 4#Dielectric temperature compose measurement
According to the crystallographic direction of<001>, respectively by sample 1#~sample 4#It is parallel up and down that cutting is polished into having for regular shape
The sample in face is composed test using Jie's temperature under 1 hertz of impedance analyzer progress, 10 hertz, 100 hertz, 1000 hertz frequencies, is obtained
Obtain the Curie temperature information and dielectric constant of crystalline material.
The results show that sample 1#~sample 4#Room temperature dielectric of Curie temperature in the range of 93~253 DEG C, when 1kHz
Constant is in the range of 424~5648.
With sample 1#For Typical Representative, dielectric thermogram is as shown in Figure 2.As seen from Figure 2, sample 1#Curie's temperature
Degree is 142 DEG C, and the dielectric constant under room temperature when 1kHz is 2611.
6 sample 1 of embodiment#~sample 4#Ferroelectric hysteresis loop measurement
Using ferroelectricity instrument respectively by sample 1#~sample 4#Ferroelectric hysteresis loop measurement is carried out, determines the ferroelectric properties of crystalline material.
The results show that sample 1#~sample 4#Coercive field range in 1.5~18kV/cm, residual polarization range 14~
36.7μC/cm2。
With sample 1#For Typical Representative, ferroelectric hysteresis loop is as shown in figure 3, as seen from Figure 3, sample 1#Coercive field be
4.9kV/cm, residual polarization are 36.7 μ C/cm2。
7 sample 1 of embodiment#~sample 4#Photoluminescence performance
Using Fluorescence Spectrometer respectively by sample 1#~sample 4#The test of photoluminescence performance is carried out, is finally being applied directly
While galvanic electricity field, crystallo-luminescence intensity is measured with the situation of change of electric field (times coercive field from 0kV/cm to about 3).
The results show that sample 1#~sample 4#Luminous intensity as electric field changes, real-time electric field tune may be implemented
Control luminous intensity.
With sample 1#Transmitting for Typical Representative, at not same electric field (0kV/cm, 4.91kV/cm, 15.08kV/cm)
Spectral results as shown in figure 4, as seen from Figure 4, the luminous intensity of sample with the increase of the real-time electric field of application occur it is bright
Aobvious downward trend, when applying the electric field of 4.91kV/cm, the luminous intensity near 1061nm declines near 28%, 879nm
Luminous intensity decline 27%;When application electric field is 15.08kV/cm, it is attached that the luminous intensity near 1061nm declines 35%, 879nm
Close luminous intensity decline 33%;Show that electric field effectively can carry out real-time monitoring to luminous intensity.
The above is only several embodiments of the application, not does any type of limitation to the application, although this Shen
Please disclosed as above with preferred embodiment, however not to limit the application, any person skilled in the art is not taking off
In the range of technical scheme, a little variation or modification are made using the technology contents of the disclosure above and is equal to
Case study on implementation is imitated, is belonged in technical proposal scope.
Claims (10)
1. a kind of neodymium adulterates lead magnesium niobate-lead titanate material, which is characterized in that the neodymium adulterates lead magnesium niobate-lead titanate material
With perovskite type crystal structure.
2. neodymium according to claim 1 adulterates lead magnesium niobate-lead titanate material, which is characterized in that the neodymium adulterates niobium magnesium
The chemical formula of titanate-zirconate material is (NdxPb1-3x/2)[(Mg1/3Nb2/3)1-yTiy]O3;
Wherein, 0.01≤x≤0.05,0.28≤y≤0.65;
Preferably, x=0.02,0.31≤y≤0.39.
3. the preparation method of neodymium doping lead magnesium niobate-lead titanate material as claimed in claim 1 or 2, which is characterized in that the method
It at least includes the following steps:
A) after mixing the raw material containing neodymium source, lead source, magnesium source, niobium source, titanium source with fluxing agent, 900~1100 DEG C of constant temperature are placed in
No less than 12 hours, obtain initial melt;
B) seed crystal is contacted with initial melt, grows to obtain the neodymium doping lead magnesium niobate-lead titanate material using top-seeded solution growth
Material.
4. according to the method described in claim 3, it is characterized in that, neodymium source described in step a) is Nd2O3, lead source is PbO, magnesium
Source is MgO, and niobium source is Nb2O5, titanium source TiO2;
The fluxing agent is PbO and B2O3Mixture.
5. according to the method described in claim 3, it is characterized in that, it is described containing neodymium source, lead source, magnesium source, niobium source, titanium source original
The molar ratio of material and fluxing agent is 1:2~10.
6. according to the method described in claim 3, it is characterized in that, the condition of step b) the top-seeded solution growth growth are as follows:
Rate of temperature fall are as follows: 1~5 DEG C/day;
The rate of seed rod rotation are as follows: 0~20 rev/min.
7. a kind of ferroelectricity luminescent material, which is characterized in that adulterate lead magnesium niobate-lead titanate containing neodymium of any of claims 1 or 2
Material adulterates lead magnesium niobate-lead titanate material according to the neodymium that any one of claim 3 to 6 the method is prepared.
8. ferroelectricity luminescent material according to claim 7, which is characterized in that the neodymium adulterates lead magnesium niobate-lead titanate material
Material has ferroelectric hysteresis loop, and coercive field range is in 1.5~18kV/cm, and residual polarization range is in 14~36.7 μ C/cm2。
9. ferroelectricity luminescent material according to claim 7, which is characterized in that photic applied by the ferroelectricity luminescent material
Centre of luminescence wavelength is located at least near 879nm and 1061nm.
10. ferroelectricity luminescent material according to claim 7, which is characterized in that the luminescence generated by light of the ferroelectricity luminescent material
Intensity can carry out real-time monitoring by modulation electric field strength.
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CN113956040B (en) * | 2020-07-20 | 2022-07-12 | 中国科学院上海硅酸盐研究所 | Transparent photoelectric ceramic material with ultrahigh voltage coefficient and ultrahigh photoluminescence performance and preparation method thereof |
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