CN102817080A - Lead lutetioniobate-lead magnesioniobate-lead titanate ternary-system relaxation ferroelectric monocrystal and preparation method thereof - Google Patents
Lead lutetioniobate-lead magnesioniobate-lead titanate ternary-system relaxation ferroelectric monocrystal and preparation method thereof Download PDFInfo
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- CN102817080A CN102817080A CN2012103247721A CN201210324772A CN102817080A CN 102817080 A CN102817080 A CN 102817080A CN 2012103247721 A CN2012103247721 A CN 2012103247721A CN 201210324772 A CN201210324772 A CN 201210324772A CN 102817080 A CN102817080 A CN 102817080A
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Abstract
The invention discloses a lead lutetioniobate-lead magnesioniobate-lead titanate ternary-system relaxation ferroelectric monocrystal and a preparation method thereof. The chemical general formula of the monocrystal is xPb(Lu1/2Nb1/2)O3-yPb(Mg1/3Nb2/3)O3-(1-x-y)PbTiO3, wherein 0.1<=x<=0.4, 0.2<=y<=0.6, but 1-x-y is not equal to 0. The PLMNT monocrystal is prepared by a crucible descent method. The invention effectively overcomes the defect of overlow Curie temperature in the PMNT monocrystal and the defects of difficulties in crystallization and mass growth in the PLNT monocrystal in the prior art. The PLMNT monocrystal disclosed by the invention has great application potential at room temperature, is very applicable to high-temperature devices, has wide application temperature range, and can completely satisfy the application requirements in high technologies, such as ultrasonic imaging, ultrasonic motors and the like, thereby having very wide application prospects.
Description
Technical field
The present invention relates to a kind of relaxor ferroelectric monocrystal and preparation method thereof, specifically, relate to a kind of niobium lutetium lead plumbate-PMN-PT three component system relaxor ferroelectric monocrystal and preparation method thereof, belong to ferroelectric/technical field of piezoelectric materials.
Background technology
Ferroelectric/piezoelectric is widely used in various functional devices owing to possess advantages such as good dynamo-electric transition function, response speed be fast, in national economy and national defense safety, is bringing into play irreplaceable vital role.Therefore, become a focus in the ferroelectric material about relaxor ferroelectric monocrystal preparation, piezoelectric property and applied research.
With Pb (Mg
1/3Nb
2/3) O
3-PbTiO
3(PMNT) monocrystalline is the relaxor ferroelectric sosoloid monocrystal with composite perofskite type structure of representative, and a side of tripartite phase has excellent piezoelectric property, its d near three parts-cubic accurate homotype phase boundary (MPB) zone
33And k
33Can reach respectively more than 2500pC/N and 92%, the maximum strain amount has reached 1.7%, will exceed an one magnitude than piezoelectric ceramics PZT commonly used.Yet when practical application, the various physicalies of composite perofskite type solid-solution material not only and Tc (T
c) closely related, also with three parts and cubic transformation temperature (T mutually
Rt) be closely connected.The Tc of PMNT monocrystalline and three parts-cubic transformation temperature has only 140 ℃ and 65 ℃ respectively, and the TR of application has received strict restriction.When temperature surpasses transformation temperature T
RtThe time, the piezoelectric property of PMNT monocrystalline can obviously descend.In addition, the coercive electric field (E of PMNT monocrystalline
c) also lower (2-3kV/cm), limited its at some than the application in the large power supersonic transverter.Therefore, improve the Tc and the three parts-cubic transformation temperature of piezoelectric monocrystal, widen its temperature use range, have important researching value.
For solving the temperature stability problem of PMNT monocrystalline, people have studied the lead based relaxor ferro-electricity single crystal system of some high-curie temperatures in succession in recent years, like Pb (In
1/2Nb
1/2) O
3-PbTiO
3Monocrystalline (PINT), Pb (Sc
1/2Nb
1/2) O
3-PbTiO
3Monocrystalline (PSNT), Pb (Yb
1/2Nb
1/2) O
3-PbTiO
3Monocrystalline (PYNT) etc.; Its Tc and three parts-cubic transformation temperature reaches as high as 350 ℃ and 200 ℃; Near piezoceramic material commonly used; What but its crystal growth was adopted is traditional case of flux methods, smaller through the monocrystalline that sporadic nucleation is grown, and is difficult to satisfy actual application requiring.Therefore, research and develop a kind of relaxor ferroelectric monocrystal, will have research and be worth and social effect with high-curie temperature and high three parts-cubic transformation temperature.
Summary of the invention
To the problems referred to above that prior art exists, the purpose of this invention is to provide a kind of niobium lutetium lead plumbate-PMN-PT three component system relaxor ferroelectric monocrystal and preparation method thereof with high-curie temperature and high three parts-cubic transformation temperature.
For realizing the foregoing invention purpose, the technical scheme that the present invention adopts is following:
A kind of niobium lutetium lead plumbate-PMN-PT three component system relaxor ferroelectric monocrystal has following chemical general formula: xPb (Lu
1/2Nb
1/2) O
3-yPb (Mg
1/3Nb
2/3) O
3-(1-x-y) PbTiO
3Be abbreviated as: xPLN-yPMN-(1-x-y) PT or PLMNT, wherein PLN represents Pb (Lu
1/2Nb
1/2) O
3, PMN represents Pb (Mg
1/3Nb
2/3) O
3, PT represents PbTiO
3Wherein: 0.1≤x≤0.4,0.2≤y≤0.6, but 1-x-y ≠ 0.
As a kind of preferred version, said x=0.1～0.3, said y=0.4～0.6, and 1-x-y=0.2～0.3.
A kind of method for preparing above-mentioned niobium lutetium lead plumbate-PMN-PT three component system relaxor ferroelectric monocrystal is falling crucible method, comprises following concrete steps:
A) according to general formula xPb (Lu
1/2Nb
1/2) O
3-yPb (Mg
1/3Nb
2/3) O
3-(1-x-y) PbTiO
3Accurately take by weighing the Lu of stoichiometric ratio
2O
3, MgO, Nb
2O
5, PbO and TiO
2Each raw material, ball milling make and mix; Wherein: 0.1≤x≤0.4,0.2≤y≤0.6, but 1-x-y ≠ 0;
B) material of above-mentioned mixing is expected as rising of crystal growth after 4～8 hours 1000～1100 ℃ of following presintering;
C) rising of crystal growth expected pack in the crucible; Add seed crystal; Adopt falling crucible method to carry out crystal growth: control crystal growth furnace temperature is 1400～1550 ℃; The melt soaking time is 5～7 hours, and the crucible fall off rate is 0.1～2.0mm/h, and the maximum temperature gradient of crucible descending direction is 5～7 ℃/mm;
D) growth ending, furnace cooling is to room temperature.
Ball milling described in the step a) is dry ball milling or wet ball grinding, and the ball milling time was recommended as more than 12 hours, is preferably 24 hours.
The Lu of raw material described in the step a)
2O
3, MgO, Nb
2O
5, PbO and TiO
2Purity all be preferably greater than 99.99%.
Crucible is preferably platinum crucible described in the step c).
Seed crystal described in the step c) is the niobic magnesium acid lead-lead titanate single-crystal (PMNT) of PLMNT monocrystalline or heterogeneous isomorphism.
As further preferred version, said seed crystal be oriented to < 111 >, < 110>or < 100 >.
As further preferred version, the crucible fall off rate in the step c) is 0.1～0.8mm/h.
Compared with prior art; A kind of niobium lutetium lead plumbate provided by the invention-PMN-PT three component system relaxor ferroelectric monocrystal (PLMNT monocrystalline) has high-curie temperature and high three parts-cubic transformation temperature, shows excellent piezoelectric property and good electric field stability; Experimental result shows: the d of the optimum cut type of prepared PLMNT monocrystalline
33And k
33Respectively up to 2300pC/N and 92%; The d of 31 patterns
31And k
31Respectively up to-2100pC/N and 90%; Its three parts-cubic transformation temperature Trt and Tc Tc have reached 100 ℃ and 180 ℃ respectively, and be higher more than 30 ℃ than the relevant temperature of existing P MN-0.30PT monocrystalline; And said PLMNT crystal still has good piezoelectricity and electromechanical coupling performance before being warmed up to its three parts-cubic transformation temperature.In addition, adopt falling crucible method not only to have the advantage that can grow in batches, can also grow diameter greater than 20mm, length is greater than the large size PLMNT monocrystalline of 50mm.
In a word; The present invention not only effectively overcome the crystallization that Tc is too low and the PLNT monocrystalline exists that PMNT monocrystalline of the prior art exists relatively difficulty, be difficult to the defective of growth in batches; And the PLMNT monocrystalline that provides not only has huge application potential at normal temperatures, also is fit to very much be applied in the high-temperature device, has wide use temperature scope; Can satisfy high-tech application requirements such as ultra sonic imaging, ultrasonic motor fully, application prospect is very wide.
Description of drawings
Fig. 1 is niobium lutetium lead plumbate-PMN-PT three component system relaxor ferroelectric monocrystal XRD figure spectrum at room temperature that embodiment 1 makes;
Fig. 2 be the niobium lutetium lead plumbate that makes of embodiment 1-PMN-PT three component system relaxor ferroelectric monocrystal behind < 001>direction polarization at room temperature ferroelectric hysteresis loop;
Fig. 3 is the niobium lutetium lead plumbate that makes of embodiment 1-PMN-PT three component system relaxor ferroelectric monocrystal behind < 001>direction polarization, and at room temperature unidirectional field causes strain curve figure;
Fig. 4 is niobium lutetium lead plumbate-PMN-PT three component system relaxor ferroelectric monocrystal edge that embodiment 1 makes<001>Dielectric properties ε under 100Hz, 1kHz and 10kHz frequency respectively behind the direction polarization
rGraph of relation with tan δ and temperature;
Fig. 5 is the piezoelectric constant (d of the thickness vibration mode vibration shape sample of niobium lutetium lead plumbate-PMN-PT three component system relaxor ferroelectric monocrystal of making of embodiment 1
33) from 30 ℃ to 150 ℃ change curves;
Fig. 6 is the piezoelectric constant (d of the length vibration modes vibration shape sample of niobium lutetium lead plumbate-PMN-PT three component system relaxor ferroelectric monocrystal of making of embodiment 1
31) and electromechanical coupling factor (k
31) change curve respectively from 30 ℃ to 110 ℃.
Embodiment
Below in conjunction with accompanying drawing and embodiment to the present invention do further in detail, intactly explanation.
The specific inductivity that relates among the present invention is to record sample electric capacity through Agilent 4294A type electric impedance analyzer, and proximate calculation obtains according to plate condenser; Electromechanical coupling factor is according to the IEEE176-1987 standard, adopts Agilent 4294A type electric impedance analyzer to measure the impedance spectrum of different mode cut type, according to resonant frequency f
sWith anti-resonance frequency f
pCalculate; Room temperature piezoelectric constant d
33Be the ZJ-3A type d that adopts Acoustical Inst., Chinese Academy of Sciences to make
33Tester is directly measured, and other piezoelectric constant is to be calculated by specific inductivity and electromechanical coupling factor according to the IEEE176-1987 standard; In the measurement of high-temperature piezoelectric performance, variation of temperature is to realize through the ZJW-1 type temperature controller of Xi'an Communications University's electronics Research Institute; The ferroelectric hysteresis loop of PLMNT monocrystalline causes strain with the field and records through Aixxact TF-1000 type ferroelectric analyser.
The purity that accurately takes by weighing stoichiometric ratio according to chemical formula 0.13PLN-0.57PMN-0.30PT is all greater than 99.99% Lu
2O
3, MgO, Nb
2O
5, PbO and TiO
2Each powder raw material, ball milling made and mixes in 24 hours; Then 1050 ℃ of sintering 6 hours, make single crystal growing and rise and expect; Said single crystal growing is worked the platinum crucible that places sealing of expecting, and (thickness of crucible and shape do not have strict restriction; For reducing cost a plurality of crucibles of a preferred stove, particularly special-shaped crucible; Can be with reference to a plurality of disclosed patents of Shanghai Silicate Inst., Chinese Academy of Sciences, for example CN1113970A); Crucible is inserted in the crystal growing furnace; Select the heterogeneous isomorphism of no bulk defects for use<111>The niobic magnesium acid lead-lead titanate single-crystal of direction (PMNT) is as seed crystal; Adopt falling crucible method to carry out crystal growth: control crystal growth furnace temperature is 1450～1550 ℃, and the melt soaking time is 5 hours, and the crucible fall off rate is 0.1～0.8mm/h, and the maximum temperature gradient of crucible descending direction is 5～7 ℃/mm; Growth ending naturally cools to room temperature with furnace temperature; Can obtain and seed crystal direction unanimity and the shape complete PLMNT monocrystalline identical,, confirm that its real composition is 0.13PLN-0.59PMN-0.28PT through the XRF quantitative analysis with crucible.Originally execute routine gained monocrystalline and remove the seed crystal part, the crystal ingot portion size is Φ 20mm * 45mm, and < 001>direction chip area can reach more than 10mm * 10mm.
Learn through measuring and calculating: near the PLMNT monocrystalline the accurate homotype phase boundary at room temperature shows excellent piezoelectric property, edge<001>Behind the direction polarization, piezoelectric constant d
33Up to 2300pC/N, the electromechanical coupling constant k
33Reach 92%; The edge<110>Behind the direction polarization, the piezoelectric constant d of 31 patterns
31Reach-2000pC/N the electromechanical coupling constant k
31Reach 90%.
Fig. 1 is niobium lutetium lead plumbate-PMN-PT three component system relaxor ferroelectric monocrystal XRD figure spectrum at room temperature that present embodiment makes, and can be known by Fig. 1: this PLMNT monocrystalline at room temperature presents pure tripartite phase calcium titanium ore structure, and does not have burnt green stone to generate mutually.
Fig. 2 is niobium lutetium lead plumbate-PMN-PT three component system relaxor ferroelectric monocrystal edge that present embodiment makes<001>At room temperature ferroelectric hysteresis loop behind the direction polarization can be known by Fig. 2: the coercive electric field (E of this PLMNT monocrystalline
c) reaching 6kV/cm, spontaneous polarization is 30 μ C/cm
2
Fig. 3 is the niobium lutetium lead plumbate that makes of present embodiment-PMN-PT three component system relaxor ferroelectric monocrystal behind < 001>direction polarization, and at room temperature unidirectional field causes strain curve figure; Can be known by Fig. 3: the maximum strain of this PLMNT monocrystalline reaches 0.7%; And when electric field adds to 30kV/cm; The piezoelectric property of this PLMNT monocrystalline does not have considerable change, further specifies this PLMNT crystal and has good electric field stability.
Fig. 4 is niobium lutetium lead plumbate-PMN-PT three component system relaxor ferroelectric monocrystal edge that present embodiment makes<001>Dielectric properties ε under 100Hz, 1kHz and 10kHz frequency respectively behind the direction polarization
rWith the graph of relation of tan δ and temperature, can know: the three parts of this PLMNT monocrystalline-cubic transformation temperature T by Fig. 4
RtWith Tc T
cReached 100 ℃ and 180 ℃ respectively, all the relevant temperature than PMN-0.30PT monocrystalline has exceeded more than 30 ℃.
In order further to confirm PLMNT monocrystalline temperature stability at high temperature, the crystal that grows has been carried out the high-temperature behavior sign.Fig. 5 is the piezoelectric constant (d of the thickness vibration mode vibration shape sample of niobium lutetium lead plumbate-PMN-PT three component system relaxor ferroelectric monocrystal of making of present embodiment
33) from 30 ℃ to 150 ℃ change curves, can know by Fig. 5: shown in the piezoelectric constant d of thickness vibration mode vibration shape sample
33Very little 30～80 ℃ of variations, significantly raise at 80～100 ℃, locate to reach peak 5800pC/N to 100 ℃, after temperature is higher than 100 ℃ with temperature rising d
33Significantly reduce, explain that three parts-cubic phase transformation has taken place this crystal near 100 ℃.Fig. 6 is the piezoelectric constant (d of the length vibration modes vibration shape sample of niobium lutetium lead plumbate-PMN-PT three component system relaxor ferroelectric monocrystal of making of present embodiment
31) and electromechanical coupling factor (k
31) change curve respectively from 30 ℃ to 110 ℃, can know by Fig. 6: the electromechanical coupling factor k of the length vibration modes vibration shape sample of this PLMNT monocrystalline
31Little from 30 ℃ to 90 ℃ variation, after surpassing 90 ℃, temperature sharply descends; And piezoelectric constant d
31Before 90 ℃, raise and rise, d after 90 ℃ with temperature
31Descend.Can know in conjunction with Fig. 5 and Fig. 6: this PLMNT crystal is less than three parts-cubic transformation temperature; Promptly; In the time of 100 ℃; Still have good piezoelectricity and electromechanical coupling performance, the 0.13PLN-0.59PMN-0.28PT monocrystalline that further specifies accurate homotype phase boundary component not only has huge application potential at normal temperatures, also is highly suitable for to be able in some high-temperature devices use.
Embodiment 2
The purity that accurately takes by weighing stoichiometric ratio according to chemical formula 0.30PLN-0.40PMN-0.30PT is all greater than 99.99% Lu
2O
3, MgO, Nb
2O
5, PbO and TiO
2Each powder raw material, ball milling made and mixes in 24 hours; Then 1100 ℃ of sintering 4 hours, make single crystal growing and rise and expect; Said single crystal growing worked to expect placing 1 said identical platinum crucible, then crucible is inserted in the crystal growing furnace with embodiment; Select the heterogeneous isomorphism of no bulk defects for use<111>The niobic magnesium acid lead-lead titanate single-crystal of direction (PMNT) is as seed crystal; Adopt falling crucible method to carry out crystal growth: control crystal growth furnace temperature is 1400～1450 ℃, and the melt soaking time is 7 hours, and the crucible fall off rate is 0.1～0.8mm/h, and the maximum temperature gradient of crucible descending direction is 5～7 ℃/mm; Growth ending naturally cools to room temperature with furnace temperature; Can obtain and seed crystal direction unanimity and the shape complete PLMNT monocrystalline identical,, confirm that its real composition is 0.30PLN-0.40PMN-0.30PT through the XRF quantitative analysis with crucible.Originally execute routine gained monocrystalline and remove the seed crystal part, the crystal ingot portion size is Φ 20mm * 50mm, and < 001>direction chip area can reach more than 10mm * 10mm.
Learn through analyzing: the d of the optimum cut type of the PLMNT monocrystalline that present embodiment is prepared
33And k
33Respectively up to 2000pC/N and 92%; The d of 31 patterns
31And k
31Respectively up to-2100pC/N and 90%; Its three parts-cubic transformation temperature T
RtWith Tc T
c95 ℃ and 170 ℃ have been reached respectively; And said PLMNT crystal still has good piezoelectricity and electromechanical coupling performance before being warmed up to its three parts-cubic transformation temperature.
Be necessary at last in this explanation to be: above embodiment only is used for technical scheme of the present invention is done explanation in further detail; Can not be interpreted as the restriction to protection domain of the present invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.
Claims (10)
1. niobium lutetium lead plumbate-PMN-PT three component system relaxor ferroelectric monocrystal is characterized in that having following chemical general formula: xPb (Lu
1/2Nb
1/2) O
3-yPb (Mg
1/3Nb
2/3) O
3-(1-x-y) PbTiO
3Wherein: 0.1≤x≤0.4,0.2≤y≤0.6, but 1-x-y ≠ 0.
2. niobium lutetium lead plumbate according to claim 1-PMN-PT three component system relaxor ferroelectric monocrystal is characterized in that: said x=0.1～0.3, said y=0.4～0.6, and 1-x-y=0.2～0.3.
3. method for preparing the described niobium lutetium lead plumbate of claim 1-PMN-PT three component system relaxor ferroelectric monocrystal is characterized in that: be falling crucible method, comprise following concrete steps:
A) according to general formula xPb (Lu
1/2Nb
1/2) O
3-yPb (Mg
1/3Nb
2/3) O
3-(1-x-y) PbTiO
3Accurately take by weighing the Lu of stoichiometric ratio
2O
3, MgO, Nb
2O
5, PbO and TiO
2Each raw material, ball milling make and mix; Wherein: 0.1≤x≤0.4,0.2≤y≤0.6, but 1-x-y ≠ 0;
B) material of above-mentioned mixing is expected as rising of crystal growth after 4～8 hours 1000～1100 ℃ of following presintering;
C) rising of crystal growth expected pack in the crucible; Add seed crystal; Adopt falling crucible method to carry out crystal growth: control crystal growth furnace temperature is 1400～1550 ℃; The melt soaking time is 5～7 hours, and the crucible fall off rate is 0.1～2.0mm/h, and the maximum temperature gradient of crucible descending direction is 5～7 ℃/mm;
D) growth ending, furnace cooling is to room temperature.
4. the method for preparing niobium lutetium lead plumbate-PMN-PT three component system relaxor ferroelectric monocrystal according to claim 3, it is characterized in that: ball milling described in the step a) is dry ball milling or wet ball grinding, and the ball milling time was greater than 12 hours.
5. the method for preparing niobium lutetium lead plumbate-PMN-PT three component system relaxor ferroelectric monocrystal according to claim 3 is characterized in that: the Lu of raw material described in the step a)
2O
3, MgO, Nb
2O
5, PbO and TiO
2Purity all greater than 99.99%.
6. the method for preparing niobium lutetium lead plumbate-PMN-PT three component system relaxor ferroelectric monocrystal according to claim 3, it is characterized in that: said crucible is a platinum crucible.
7. the method for preparing niobium lutetium lead plumbate-PMN-PT three component system relaxor ferroelectric monocrystal according to claim 3, it is characterized in that: seed crystal described in the step c) is the niobic magnesium acid lead-lead titanate single-crystal of PLMNT monocrystalline or heterogeneous isomorphism.
8. the method for preparing niobium lutetium lead plumbate-PMN-PT three component system relaxor ferroelectric monocrystal according to claim 7 is characterized in that: said seed crystal is the niobic magnesium acid lead-lead titanate single-crystal of the heterogeneous isomorphism of no bulk defects.
9. the method for preparing niobium lutetium lead plumbate-PMN-PT three component system relaxor ferroelectric monocrystal according to claim 7 is characterized in that: said seed crystal be oriented to < 111 >, < 110>or < 100 >.
10. the method for preparing niobium lutetium lead plumbate-PMN-PT three component system relaxor ferroelectric monocrystal according to claim 7, it is characterized in that: the crucible fall off rate in the step c) is 0.1～0.8mm/h.
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| CN103603042A (en) * | 2013-11-18 | 2014-02-26 | 中国科学院福建物质结构研究所 | Ferroelectric monocrystal yttrium lead niobate-magnesium lead niobate-lead titanate as well as preparation and application thereof |
| CN103710754A (en) * | 2014-01-09 | 2014-04-09 | 中国科学院福建物质结构研究所 | Ferroelectric piezoelectric single crystal lead holmium niobate-lead magnesium niobate-lead titanate as well as preparation and application thereof |
| CN103710756A (en) * | 2013-12-16 | 2014-04-09 | 中国科学院福建物质结构研究所 | Antiferroelectric crystal lead lutecium niobate-lead titanate and preparation method thereof |
| CN104153000A (en) * | 2013-05-14 | 2014-11-19 | 中国科学院上海硅酸盐研究所 | Ternary relaxation piezoelectric single crystal material and growing method thereof |
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| CN105154976A (en) * | 2015-09-28 | 2015-12-16 | 西安工业大学 | PSN-PMN-PT-PZ ferroelectric single-crystal material |
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