CN102534788A - Ferroelectric single crystal containing Pb(Ga1/2Nb1/2)O3, Pb(Mg1/3Nb2/3)O3 and PbTiO3, as well as preparation method and application of ferroelectric single crystal - Google Patents
Ferroelectric single crystal containing Pb(Ga1/2Nb1/2)O3, Pb(Mg1/3Nb2/3)O3 and PbTiO3, as well as preparation method and application of ferroelectric single crystal Download PDFInfo
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- CN102534788A CN102534788A CN2012100563036A CN201210056303A CN102534788A CN 102534788 A CN102534788 A CN 102534788A CN 2012100563036 A CN2012100563036 A CN 2012100563036A CN 201210056303 A CN201210056303 A CN 201210056303A CN 102534788 A CN102534788 A CN 102534788A
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Abstract
The invention discloses a ferroelectric crystal containing Pb(Ga1/2Nb1/2)O3, Pb(Mg1/3Nb2/3)O3 and PbTiO3, as well as a preparation method and the application of the ferroelectric crystal. The material of the crystal adopts perovskite structures, exists in an MPB zone, and adopts the chemical formula (1-x-y)Pb(Ga1/2Nb1/2)O3-xPb(Mg1/3Nb2/3)O3-yPbTiO3. The crystal grows according to a high-temperature solution method or a top crystallon method and is a square crystal of which the exposing surface (001) is a natural growth surface. The crystal has better piezo-electricity and electromechanical performance, as well as higher Curie temperature and better heat resistance, thereby having a broad application prospect.
Description
Technical field
The present invention relates to a kind of novel ferroelectric monocrystalline and preparation method thereof.Particularly, the present invention relates to and have accurate homotype phase boundary (MPB) structure and higher relatively ferroelectric single crystal material (1-x-y) Pb (Ga of Tc
1/2Nb
1/2) O
3-xPb (Mg
1/3Nb
2/3) O
3-yPbTiO
3, note by abridging and be PGN-PMN-PT, and crystalline preparation method, structure and electric property, belong to crystal technology and functional materials and learn the field.
Background technology
Ferroelectric/piezoelectric is owing to possess advantages such as good dynamo-electric conversion performance, response speed be fast; Be widely used in various functional devices; Like transmitter, transverter, sonar, driving mechanism, wave filter, little speaker etc., in national economy and national defense safety, bringing into play irreplaceable vital role.Find BaTiO the forties in last century
3Piezoelectric has been found Pb (Zr the fifties
1-xTi
x) O
3, be called for short PZT.The PZT stupalith is a kind of conventional piezoelectric materials that is widely used in transverter (transducer) and performer (actuator), dominate in the piezoelectricity Application Areas always.There is accurate homotype phase boundary (morphotropic phaseboundary) in this material, notes by abridging to be MPB.PZT is the performance piezoelectric property at the MPB place, the piezoelectric coefficient d of PZT piezoelectric ceramics
33～700pC/N, electromechanical coupling factor k
33～70%.Along with the research to MPB, relaxation ferroelectric (relaxorferroelectric) comes to light.In recent years, having calcium titanium ore structure is widely used on performer and the sonac owing to having high piezoelectricity near the relaxation ferroelectric the MPB.Relaxation ferroelectric has complex perovskite structure, and general structure is: Pb (B
1, B
2) O
3(B
1=Mg
2+, Zn
2+, Sc
3+, In
3+, B
2=Nb
5+, Ta
5+, W
6+).Relaxation ferroelectric and PbTiO
3The sosoloid that forms shows than PZT material more excellent dielectric and piezoelectric property.Wherein more typically be exactly (1-x) Pb (Mg
1/3Nb
2/3)-xPbTiO
3(PMNT) and (1-x) Pb (Zn
1/3Nb
2/3)-xPbTiO
3(PZNT) system.Such monocrystal material component shows high electromechanical coupling factor (k near MPB
33＞90%) extra-high voltage coefficient (d,
33＞2000pC/N) become the core piezoelectric of ultrasonic transducer, transmitter and driving mechanism of a new generation with big strain (＞1%).Therefore, become a focus in the ferroelectric material about relaxor ferroelectric monocrystal preparation, piezoelectric property and applied research.Though PMNT and PZNT Stability Analysis of Structures, excellent performance, this type of material has several types of defectives.The PMNT monocrystalline of MPB component shows low Tc T
CLow (＜150 ℃) and low umpolarization temperature (T
Rt＜70 ℃), reduced the stability of dielectric and piezoelectric property, cause easy umpolarization, the TR of practical application is narrow.Particularly prepare in the process at transverter, temperature variation can reduce dielectric, the piezoelectric property of material, even the umpolarization phenomenon occurs, directly has influence on performance, stability and the consistence of device.Be exactly PMNT coercive field little (2-3kV/cm) in addition, make it be not suitable for being applied to high electric field.The more important thing is the mechanical quality factor of PMNT and PZNT little (Q～50).More than these shortcomings all make PMNT and PZNT not be suitable for high-power and comparatively high temps.Therefore, we hope to explore a kind of novel high curie point, high performance relaxor ferroelectric monocrystal is used for high power device, to be suitable for the demand for development of current ferroelectric material.In recent years, (1-x) Pb (Yb
1/2Nb
1/2) O
3-xPbTiO
3(PYN-PT), (1-x) Pb (In
1/2Nb
1/2) O
3-xPbTiO
3(PIN-PT), (1-x) Pb (Sc
1/2Nb
1/2) O
3-xPbTiO
3(PSN-PT) relaxor ferroelectric monocrystal of high-curie temperature is reported that but this type relaxor ferroelectric monocrystal difficult growth, is difficult to obtain high-quality bulky single crystal.So we hope to find, and a kind of Curie temperature is high, performance is good and can grow the novel relaxor ferroelectric monocrystal of high quality bulk.
In view of above consideration, a kind ofly can be used for high-power and to have the ferroelectric single crystal material of high-curie temperature in order to seek, we carry out (the Ga to (1-x-y) Pb
1/2Nb
1/2) O
3-xPb (Mg
1/3Nb
2/3)-yPbTiO
3(PGN-PMN-PT) research of system solid solution.Research ternary system PGN-PMN-PT the MPB zone and near preparation method, structure and the electric property of monocrystalline of component, for the piezoelectricity field provides a kind of novel and can be used for the ferroelectric monocrystalline of high-curie temperature high-performance of high power device.
Summary of the invention
The objective of the invention is to seek a kind of novel ferro-electricity single crystal and study its preparation technology to the problem of above-mentioned proposition; To solve the difficult ferro-electricity single crystal of growing and not being applicable to high power device preferably of existing high-curie temperature ferro-electricity single crystal, for ferroelectric single crystal material increases a kind of product innovation.This crystalline material can be widely used in the piezoelectric device field.
A kind of novel ferroelectric single crystal material provided by the invention, it is characterized in that: the crystalline chemical constitution is: (1-x-y) Pb (Ga
1/2Nb
1/2) O
3-xPb (Mg
1/3Nb
2/3)-yPbTiO
3, be abbreviated as: PGN-PMN-PT belongs to calcium titanium ore structure and has accurate homotype phase boundary (MPB) district.
Described chemical constitution, the chemical constitution of the ferroelectric single crystal material of ternary system is elected as: 0.01PGN-0.54PMN-0.45PT.
Ferroelectric crystal preparation methods of the present invention is based on the o that this system is fit to growth, it is characterized in that comprising following concrete steps:
A) with initial feed PbO or Pb
3O
4, Ga
2O
3, TiO
2, MgO, Nb
2O
5Carry out proportioning by the crystalline chemical constitution;
B) solubility promoter adopts PbO or Pb
3O
4And H
3BO
3Or B
2O
3Composite auxiliary solvent;
C) with crystal raw material and solubility promoter mixed grinding in container;
D) powder that mixes is packed in the platinum crucible, and place the crystal growing furnace material to platinum crucible;
E) in crystal growing process, raw material is heated to (between 950-1200 ℃) more than the supersolubility temperature, the constant temperature certain hour is then with 1-20 ℃ speed cooling every day.Growth ending, with the 5-30 ℃/h annealing of lowering the temperature, crystal is taken out in the back.
Used raw material PbO or Pb
3O
4, Ga
2O
3, TiO
2, MgO, Nb
2O
5Be oxide powder.
The platinum crucible that is adopted is the cylinder shape crucible.
The crystal growing furnace that is adopted is a resistance heating element, and heating unit is wire spiral or globars or Si-Mo rod.
The crystal boundary of being grown is for appearing the square crystal of (001) self-sow face.
Crystalline preparation method according to the invention all adopts solubility promoter, and solubility promoter is with PbO or Pb
3O
4And H
3BO
3Or B
2O
3Composite auxiliary solvent.It is good to grow crystal mass, does not have the solubility promoter inclusion, and uniform component property is good.This crystal can be used for being used for the device of sonar probe, underwater acoustic transducer, driving mechanism, the isobaric electrical domain of ultrasonic motor.
Ferroelectric single crystal material PGN-PMN-PT according to the invention has the MPB structure.At PbTiO
3(PT) content is tripartite calcium titanium ore structure more after a little while, at PbTiO
3Content carries out the transition to cubic calcium titanium ore structure more for a long time.Different according to the ratio of PGN, PMN and PT, grow the MPB district and near PGN-PMN-PT crystalline Tc Tc can be between 150～320 ℃, three parts-cubic transformation temperature T
RtBetween 50～200 ℃, coercive field E
c(＞3kV/cm), piezoelectric coefficient d
33(500-2500pC/N), electromechanical coupling factor (＞80%).The PGN-PMN-PT system structure is stable, shows good thermostability.
The X-ray powder diffraction of the prepared ferroelectric single crystal material 0.01PGN-0.54PMN-0.45PT that goes out shows that crystal at room temperature has pure tripartite calcium titanium ore structure; (001) the dielectric temperature of the crystal cut of direction spectrum shows Tc T
CReach 160 ℃ (1kHz), the bright three parts of the dielectric temperature stave-cubic transformation temperature T of the sample after the polarization
RtBe 90 ℃, three parts-cubic transformation temperature occur and show that component is positioned at the MPB district; When frequency was 1kHz, the specific inductivity under the room temperature reached 2000, and dielectric loss is 0.01, and high-k is higher than 17000 (1kHz); Electromechanical coupling factor at room temperature reaches 90%, and temperature stability is preferably arranged; (001) the ferroelectric hysteresis loop research of direction crystal cut shows coercive field E
cBe 4.04kV/cm, residual polarization P
rBe 30 μ C/cm
2(001) piezoelectric coefficient d of direction crystal cut
33Reach 1100pC/N.
Description of drawings
Fig. 1 is the 0.1PGN-0.54PMN-0.45PT monocrystalline with the top-seeded solution growth growth;
Fig. 2 is the powder diagram under the 0.1PGN-0.54PMN-0.45PT monocrystalline normal temperature of growth;
Fig. 3 ' composes with the temperature variant dielectric temperature of loss tan δ for the DIELECTRIC CONSTANTS of the 0.1PGN-0.54PMN-0.45PT monocrystalline of growth.
Fig. 4 is the electromechanical coupling factor K of the 0.1PGN-0.54PMN-0.45PT monocrystalline of growth
33With the variation of temperature curve.
Fig. 5 is the electric current I-electric field E and the polarizability P-electric field E ferroelectric hysteresis loop of the 0.1PGN-0.54PMN-0.45PT monocrystalline of growth.
Embodiment
Below in conjunction with concrete embodiment the present invention is done further detailed, complete explanation, but do not limit content of the present invention.
The crystal growing furnace that the present invention adopted is Design and Machining voluntarily; The powder diffractometer that is used for structural analysis adopt Rigaku diffractometer (Rigaku, Japan); Dielectric temperature spectrum is with the Alpha-A wideband dielectric/electric impedance analyzer of German Novocontrol company; Ferroelectric hysteresis loop is to record (frequency is 2Hz) by the ferroelectric analyser of aix-ACCT TF2000 that German Aixacct company produces, and alternating temperature equipment adopts the self-control tube furnace, and voltage is provided by the Trek 610D that U.S. Trek company produces.Electromechanical coupling factor is according to the IEEE176-1987 standard, records impedance spectrum by Alpha-A wideband dielectric/electric impedance analyzer, then according to resonant frequency f
rWith antiresonant frequency f
aCalculate.
Embodiment 1:
Adopt o growth PGN-PMN-PT ferroelectric single crystal material.
With initial feed PbO or Pb
3O
4, Ga
2O
3, TiO
2, MgO, Nb
2O
5, solubility promoter adopts PbO or Pb
3O
4And H
3BO
3Or B
2O
3Composite auxiliary solvent, proportionally weighing, mixed grinding.The powder that mixes is packed in the platinum crucible, and place the crystal growing furnace material to platinum crucible.Be heated to more than the supersolubility temperature constant temperature certain hour, slowly cooling growth then with changing good material; Bubble material temperature is between 950-1200 ℃, with 1-20 ℃ speed cooling every day; Available platinum wire is suspended in liquid level central authorities in process of growth, to form nucleation centre, is reduced to nuclear volume and promotes nucleating growth; Growth ending, with the 10-30 ℃/h annealing of lowering the temperature, crystal is taken out in the back.Through crystalline X-ray powder diffraction, dielectric, ferroelectric, piezoelectric property test analysis, confirm its structure and performance to growth.
Embodiment 2:
Adopt top-seeded solution growth growth PGN-PMN-PT ferro-electricity single crystal.
With initial feed PbO or Pb
3O
4, Ga
2O
3, TiO
2, MgO, Nb
2O
5, solubility promoter adopts PbO or Pb
3O
4And H
3BO
3Or B
2O
3Composite auxiliary solvent, proportionally weighing, mixed grinding.The powder that mixes is packed in the platinum crucible, and place the crystal growing furnace material to platinum crucible.Be heated to more than the supersolubility temperature changing good material, the constant temperature certain hour finds vegetative point to grow with seed crystal; Growth about 950-1100 ℃, brilliant rotational speed rate is 5-30rpm, rate of temperature fall is 0.2-5 ℃ of every day; Growth ending, crystal propose liquid level, with the 10-30 ℃/h annealing of lowering the temperature.The monocrystalline that grows is for appearing the square crystal of (001) self-sow face, and crystal mass is good, does not have the solubility promoter inclusion, and uniform component property is good.Through crystalline X-ray powder diffraction, dielectric, ferroelectric, piezoelectric property test analysis, confirm its structure and performance to growth.
Embodiment 3:
PGN-PMN-PT ferroelectric crystal material among embodiment one and two is carried out structure and performance test, and preferred ingredient 0.01PGN-0.54PMN-0.45PT carries out structure and performance test.
A) crystal being cut small pieces grinds and to be finely ground to powder and to be used for powdery diffractometry and to use.Powdery diffractometry spectrogram according to the gained ferroelectric crystal shows that room temperature 0.01PGN-0.54PMN-0.45PT ferroelectric crystal is tripartite calcium titanium ore structure.
B) resulting ferroelectric crystal material is cut small pieces by (001) direction, polish smooth with the different sand paper two sides of will cutting into slices then.Silver electrode on the two sides quilt that polishes smooth, and under the DC electric field of 120 ℃ of 15kV/cm, polarized 15 minutes, keep electric field to drop to room temperature then, and discharged 24 hours.The sample for preparing is used for piezoelectric property d
33Test with dielectric temperature spectrum.Measured piezo-electric modulus is 1100pC/N.Surveyed and carried out the test of dielectric temperature spectrum behind the piezo-electric modulus, the sample of first polarimetry is surveyed the sample of umpolarization then.Measure the dielectric temperature spectrum of 0.01PGN-0.54PMN-0.45PT ferroelectric crystal, temperature is from-50 ℃ to 300 ℃.The dielectric thermogram shows the Tc T of the ferroelectric crystal material that obtains
CIt is 160 ℃; Obtain three parts-cubic transformation temperature T from the dielectric thermogram of polar sample
RtIt is 90 ℃.Crystal exists three parts-cubic transformation temperature to show that crystal composition is positioned at the MPB district.Specific inductivity under the room temperature and dielectric loss are respectively 2000 and 0.01.
C) resulting ferroelectric crystal material is cut small pieces by (001) direction, polish smooth with the different sand paper two sides of will cutting into slices then.Silver electrode is used for the test of ferroelectric hysteresis loop on the two sides quilt that polishes smooth.Measure different electric ferroelectric hysteresis loop after the match.+/-alternating-electric field of 25kV/cm be issued to saturated, this moment coercive field E
cBe 4.04kV/cm, residual polarization P
rBe 30 μ C/cm
2
D) resulting ferroelectric crystal material is cut cylindrical sample by (001) direction.Six faces of cylindrical sample all need polish smooth, silver electrode on the quilt of two ends.Be used for testing impedance after sample is warmed up to 160 ℃ of direct current polarizations, and calculate its electromechanical coupling factor.Thereby obtain the dielectric coupling coefficient k of 0.01PGN-0.54PMN-0.45PT ferroelectric crystal
33Concern with variation of temperature.Under the room temperature, k
33Be 90%, and shown good temperature stability.
Can know that by the foregoing description that PGN-PMN-PT ferroelectric crystal material has is dynamo-electric, ferroelectric preferably, piezoelectric property and temperature stability, and application prospect is arranged.In addition, more than detailed embodiment do not limit content of the present invention, as long as in technology of the present invention and knowledge scheme, do corresponding modification or replacement, all because of in claim of the present invention.
Claims (6)
1. niobium gallic acid lead-PMN-PT ferro-electricity single crystal is characterized in that: this materials chemistry formula is (1-x-y) Pb (Ga
1/2Nb
1/2) O
3-xPb (Mg
1/3Nb
2/3) O
3-yPbTiO
3, belong to typical calcium titanium ore structure and this sosoloid and have accurate homotype phase battery limit (BL).
2. ferro-electricity single crystal according to claim 1 is characterised in that: the chemical constitution of this material is 0.01PGN-0.54PMN-0.45PT.
3. the preparation method of the described ferroelectric single crystal material of claim 1 comprises following growth step:
A) with initial feed PbO or Pb
3O
4, Ga
2O
3, TiO
2, MgO, Nb
2O
5Carry out proportioning by the crystalline chemical constitution;
B) solubility promoter adopts PbO or Pb
3O
4And H
3BO
3Or B
2O
3Composite auxiliary solvent;
C) with crystal raw material and solubility promoter mixed grinding in container;
D) powder that mixes is packed in the platinum crucible, and place the crystal growing furnace material to platinum crucible;
E) in crystal growing process, raw material is heated between 950-1200 ℃, the constant temperature certain hour is then with 1-20 ℃ speed cooling every day; Growth ending, with the 5-30 ℃/h annealing of lowering the temperature, crystal is taken out in the back.
4. the preparation method of the described ferro-electricity single crystal of claim 1 comprises following growth step:
A) with initial feed PbO or Pb
3O
4, Ga
2O
3, TiO
2, MgO, Nb
2O
5Carry out proportioning by the crystalline chemical constitution;
B) solubility promoter adopts PbO or Pb
3O
4And H
3BO
3Or B
2O
3Composite auxiliary solvent;
C) with crystal raw material and solubility promoter mixed grinding in container;
D) powder that mixes is packed in the platinum crucible, and place the crystal growing furnace material to platinum crucible;
E) in crystal growing process, raw material is heated between 950-1200 ℃ the constant temperature certain hour; Seed crystal with the o growth finds supersolubility temperature then, introduces seeded growth at supersolubility temperature, and brilliant rotational speed rate is 5-30rpm in the process of growth, and rate of temperature fall is 0.2-5 ℃ of every day; Growth ending, with the 5-30 ℃/h annealing of lowering the temperature, crystal is taken out in the back.
5. the preparation method of ferro-electricity single crystal according to claim 4, it is characterized in that: described seeded growth direction is (001) or (110) or (111) direction.
6. the purposes of the described ferro-electricity single crystal of claim 1, it is characterized in that: this material is used for the device in piezoelectricity field.
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Cited By (1)
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| CN106637405A (en) * | 2015-10-30 | 2017-05-10 | 中国科学院福建物质结构研究所 | An infinitely mixable and meltable ferroelectric solid solution monocrystalline lead scandium niobate-lead magnesium niobate-lead titanate and a preparing method thereof |
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