CN102443850A - Ferroelectric crystal lead magnesium niobate-lead stannate-lead titanate, preparation method thereof, and purpose thereof - Google Patents
Ferroelectric crystal lead magnesium niobate-lead stannate-lead titanate, preparation method thereof, and purpose thereof Download PDFInfo
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Abstract
The invention discloses a ferroelectric crystal lead magnesium niobate-lead stannate-lead titanate, a preparation method thereof, and a purpose thereof. The crystal has a perovskite structure, and exists in an MPB zone. The crystal has a chemical formula of (1-x-y)Pb(Mg1/3Nb2/3)O3-xPbSnO3-yPbTiO3, and PMN-PSn-PT for short. In the formula, x=0-0.5, and y=0.3-0.5. According to the invention, with a high-temperature solution method or a top seeded solvent growth method, the PMN-PSn-PT crystals successfully grow. Through X-ray powder diffraction, ferroelectric measuring, dielectric measuring and piezoelectric measuring, the structure, the ferroelectric property, the dielectric property and the piezoelectric property of the crystal are analyzed. A preferable component 0.52PMN-0.10PSn-0.38PT crystal is a single domain crystal. The piezoelectric property and the single domain structure have good thermal stability. The crystal has a good application prospect.
Description
Technical field
The present invention relates to a kind of novel ferroelectric crystal and preparation method thereof.Particularly, the present invention relates to ferroelectric single crystal material (1-x-y) Pb (Mg with accurate homotype phase boundary (MPB) structure
1/3Nb
2/3) O
3-xPbSnO
3-yPbTiO
3, note by abridging and be PMN-PSn-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 barium titanate (BaTiO the forties in last century
3) piezoelectric, found Pb-based lanthanumdoped zirconate titanates (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 phase boundary) 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 (relaxor ferroelectric) 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 lead titanate (PbTiO
3) sosoloid that forms shows than PZT material more excellent dielectric and piezoelectric property.Wherein more typically be exactly PMN-PT: (1-x) Pb (Mg
1/3Nb
2/3)-xPbTiO
3(PMNT) and lead zinc niobate-lead titanate: (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 an important topic in the ferroelectric material about relaxor ferroelectric monocrystal preparation, piezoelectric property and applied research.Because there is some inherent defective in the PMNT monocrystalline; Therefore in recent years; The study on the modification of PMNT ferro-electricity single crystal is become the focus of ferroelectric crystal area research, comprise two parts: the one, other an amount of ion that mixes changes the performance of PMNT monocrystalline, for example manganese, aluminium doping PMNT monocrystalline; The 2nd, on the basis of binary PMNT ferro-electricity single crystal, add ternary component, reach the purpose that improves performance, for example niobium ytterbium lead plumbate-PMN-PT: (1-x-y) Pb (Yb
1/2Nb
1/2) O
3-xPb (Mg
1/3Nb
2/3) O
3-yPbTiO
3(PYN-PMN-PT), lead niobate lead indate-lead-PMN-PT: (1-x-y) Pb (In
1/2Nb
1/2) O
3-xPb (Mg
1/3Nb
2/3) O
3-yPbTiO
3(PIN-PMN-PT), lead magnoniobate-Pb-based lanthanumdoped zirconate titanates: (1-x-y) Pb (Mg
1/3Nb
2/3) O
3-xPbZrO
3-yPbTiO
3(PMN-PZT) etc.This type three component system ferro-electricity single crystal improves a lot than Tc on the basis of two component system PMNT, and has kept the piezoelectricity and the electromechanical coupling performance of binary ferro-electricity single crystal system.Therefore, the exploitation of three component system ferro-electricity single crystal, preparation and performance study are the focuses of present ferro-electricity single crystal research field.
Lead stannate (PbSnO
3) be a kind of monocline phase calcium titanium ore structure, itself and lead titanate (PbTiO
3) the sosoloid performance character similar with PZT that forms, and PMN-PZT shows the piezoelectric property of excellence, and have high-curie temperature.Thereby can expect that lead stannate can form sosoloid with PMNT, and excellent piezoelectric property is arranged.In view of above consideration, in order to develop a kind of novel ferroelectric monocrystal material, we carry out lead magnoniobate-lead stannate-lead titanate: (1-x-y) Pb (Mg
1/3Nb
2/3) O
3-xPbSnO
3-yPbTiO
3(PMN-PSn-PT) research of system solid solution.Preparing method, structure and the electric property of near research ternary system PMN-PSn-PT monocrystalline of the component MPB zone reaches are for the piezoelectricity field provides a kind of novel ferro-electricity single crystal.
Summary of the invention
The objective of the invention is to develop a kind of novel ferro-electricity single crystal and study its preparation technology, for ferroelectric single crystal material increases a kind of product innovation.This crystalline material can be widely used in fields such as piezoelectricity, pyroelectric electric device.
A kind of novel ferroelectric single crystal material provided by the invention, it is characterized in that: the crystal name is called: lead magnoniobate-lead stannate-lead titanate.The crystalline chemical constitution is: (1-x-y) Pb (Mg
1/3Nb
2/3) O
3-xPbSnO
3-yPbTiO
3, be abbreviated as: PMN-PSn-PT belongs to calcium titanium ore structure.Wherein, x=0～0.5, y=0.3～0.5.There is accurate homotype phase boundary (MPB) district in this sosoloid.
Described chemical constitution, the chemical constitution of the ferroelectric single crystal material of ternary system is preferably: 0.52PMN-0.10PSn-0.38PT.
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, MgO, TiO
2, SnO
2, 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, MgO, RiO
2, SnO
2, 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.
Ferroelectric crystal preparation methods of the present invention, be based on can growing large-size top-seeded solution growth, it is characterized in that comprising following concrete steps:
A) with initial feed PbO or Pb
3O
4, MgO, TiO
2, SnO
2, 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, constant temperature certain hour.Seed crystal with the o growth finds supersolubility temperature (between 950 ℃-1100 ℃) then.Introduce seeded growth at supersolubility temperature, 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.
Used raw material PbO or Pb
3O
4, MgO, TiO
2, SnO
2, Nb
2O
5Be oxide powder.
The platinum crucible that is adopted is the cylinder shape crucible.
The seeded growth direction is (001) or (110) or (111) direction.
The crystal growing furnace that is adopted is a resistance heating element, and heating unit is wire spiral or globars or Si-Mo rod.
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 PMN-PSn-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 PMN, PSn and PT, grow the MPB district and near PMN-PSn-PT crystalline Tc Tc can be between 140～300 ℃, piezoelectric coefficient d
33(500-2500pC/N).The PMN-PSn-PT system structure is stable, shows good thermostability.
The X-ray powder diffraction of the prepared ferroelectric single crystal material 0.52PMN-0.10PSn-0.38PT 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
CBe 155 ℃ (1kHz), three parts-cubic transformation temperature T
RtBe 45 ℃, 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 1900, and dielectric loss is 0.05, and high-k is higher than 8500 (1kHz); (001) the ferroelectric hysteresis loop research of direction crystal cut shows coercive field 2E
cBe 9.5kV/cm, residual polarization 2P
rBe 50 μ C/cm
2(001) piezoelectric coefficient d of direction crystal cut
33Reach 1350pC/N; 0.52PMN-0.10PSn-0.38PT crystal shows poling; The crystal that promptly grows need not polarize and just show higher piezo-electric modulus (1350pC/N); And lower the temperature after four hours and still do not have the umpolarization phenomenon being higher than Tc (200 ℃) insulation; This thermal treatment number of times is not observed umpolarization greater than ten times yet and is occurred, and shows that the 0.52PMN-0.10PSn-0.38PT crystal has stable single domain.
Figure of description
Fig. 1: the PMN-PSn-PT crystal of preparing method's growth of the present invention.
Fig. 2: 0.52PMN-0.10PSn-0.38PT crystalline X-ray powder diffraction spectrum, the crystal that shows growth is pure tripartite uhligite phase.
Fig. 3: 0.52PMN-0.10PSn-0.38PT crystalline specific inductivity, the temperature variant relation curve of dielectric loss.
Fig. 4: 0.52PMN-0.10PSn-0.38PT crystalline ferroelectric hysteresis loop.
Fig. 5: 0.52PMN-0.10PSn-0.38PT crystalline piezoelectric coefficient d
33Variation with the thermal treatment number of times.Heat treatment process: be warmed up to 200 degrees centigrade from room temperature, be incubated 4 hours, drop to room temperature then naturally.
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.
Embodiment 1:
Adopt o growth PMN-PSn-PT ferroelectric single crystal material.
With initial feed PbO or Pb
3O
4, MgO, TiO
2, SnO
2, 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 PMN-PSn-PT ferro-electricity single crystal.
With initial feed PbO or Pb
3O
4, MgO, TiO
2, SnO
2, 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:
PMN-PSn-PT among embodiment one and two growth ferroelectric crystal material (shown in Figure 1) is carried out structure and performance test, and preferred ingredient 0.52PMN-0.10PSn-0.38PT 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 0.52PMN-0.10PSn-0.38PT ferroelectric crystal is tripartite calcium titanium ore structure (shown in Figure 2).
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 need not polarization.The sample for preparing is used for piezoelectric property d
33Test with dielectric temperature spectrum.Measured unpolarized 0.52PMN-0.10PSn-0.38PT crystalline piezo-electric modulus is 1350pC/N (shown in Figure 5), is indicated as the single domain ferroelectrics.Carry out the test of dielectric temperature spectrum after having surveyed piezo-electric modulus.Measure the dielectric temperature spectrum of 0.52PMN-0.10PSn-0.38PT ferroelectric crystal, temperature is from-50 ℃ to 300 ℃.The dielectric thermogram shows the Tc T of the ferroelectric crystal material that obtains
CIt is 155 ℃; Obtain three parts-cubic transformation temperature T on the dielectric thermogram
RtIt is 45 ℃.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 1900 and 0.05 (shown in Figure 3).
C) resulting 0.52PMN-0.10PSn-0.38PT 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 15kV/cm be issued to saturated, this moment coercive field 2E
cBe 9.5kV/cm, residual polarization 2P
rBe 50 μ C/cm
2(shown in Figure 4).
D) the above-mentioned 0.52PMN-0.10PSn-0.38PT crystal that is used for the piezoelectricity test is connected to tube furnace; Carry out the stability test of crystalline piezoelectricity and single domain; Temperature is from room temperature to 200 ℃, and keeps 4 hours at 200 ℃, drops to room temperature then and carries out the piezoelectric property test.This heat treatment process is carried out ten times, the piezoelectric coefficient d that obtains
33Be 1200-1440pC/N (shown in Figure 5), show that 0.52PMN-0.10PSn-0.38PT crystalline piezoelectricity and single domain have good temperature stability.
Can be known that by the foregoing description that PMN-PSn-PT ferroelectric crystal material has is ferroelectric preferably, piezoelectric property and temperature stability, and is a kind of single domain crystal, piezoelectricity and single domain all have good temperature stability, and therefore 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 (7)
1. ferroelectric crystal material lead magnoniobate-lead stannate-lead titanate is characterized in that: this materials chemistry formula is (1-x-y) Pb (Mg
1/3Nb
2/3) O
3-xPbSnO
3-yPbTiO
3, belong to typical calcium titanium ore structure, wherein, x=0～0.5, y=0.3～0.5, there is accurate homotype phase battery limit (BL) in this sosoloid.
2. ferroelectric single crystal material according to claim 1 is characterised in that: the chemical constitution of this material is 0.52PMN-0.10PSn-0.38PT.
3. ferroelectric single crystal material according to claim 1 is characterised in that: this material part component is a kind of single domain ferroelectric crystal.
4. 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, MgO, TiO
2, SnO
2, 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.
5. 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, MgO, TiO
2, SnO
2, 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.
6. the preparation method of ferroelectric single crystal material according to claim 5, it is characterized in that: described seeded growth direction is (001) or (110) or (111) direction.
7. the purposes of the described ferroelectric single crystal material of claim 1, it is characterized in that: this material is used to prepare the device in piezoelectricity, pyroelectricity field.
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| CN107611251A (en) * | 2016-07-11 | 2018-01-19 | 中国科学院福建物质结构研究所 | A kind of piezoelectric and preparation method thereof |
| CN112142466A (en) * | 2019-06-26 | 2020-12-29 | 中国科学院上海硅酸盐研究所 | Lead niobate ytterbium acid based antiferroelectric ceramic material and preparation method thereof |
| CN114436652A (en) * | 2022-01-28 | 2022-05-06 | 厦门乃尔电子有限公司 | Lead zirconate titanate-lead tantalite-lead niobate piezoelectric ceramic material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105369357A (en) * | 2014-07-08 | 2016-03-02 | 中国科学院福建物质结构研究所 | Crystal material, preparation method and applications thereof |
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| CN107611251A (en) * | 2016-07-11 | 2018-01-19 | 中国科学院福建物质结构研究所 | A kind of piezoelectric and preparation method thereof |
| CN112142466A (en) * | 2019-06-26 | 2020-12-29 | 中国科学院上海硅酸盐研究所 | Lead niobate ytterbium acid based antiferroelectric ceramic material and preparation method thereof |
| CN112142466B (en) * | 2019-06-26 | 2021-05-25 | 中国科学院上海硅酸盐研究所 | Lead niobate ytterbium acid based antiferroelectric ceramic material and preparation method thereof |
| CN114436652A (en) * | 2022-01-28 | 2022-05-06 | 厦门乃尔电子有限公司 | Lead zirconate titanate-lead tantalite-lead niobate piezoelectric ceramic material and preparation method thereof |
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