CN106637405A - An infinitely mixable and meltable ferroelectric solid solution monocrystalline lead scandium niobate-lead magnesium niobate-lead titanate and a preparing method thereof - Google Patents
An infinitely mixable and meltable ferroelectric solid solution monocrystalline lead scandium niobate-lead magnesium niobate-lead titanate and a preparing method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- 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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
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- C—CHEMISTRY; METALLURGY
- 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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
Abstract
The invention relates to ferroelectric solid solution monocrystalline lead scandium niobate-lead magnesium niobate-lead titanate and a preparing method thereof. A top seed crystal growth process is adopted to perform growth. The process is simple, and the prepared crystal has excellent performance. The ferroelectric solid solution monocrystalline lead scandium niobate-lead magnesium niobate-lead titanate has excellent piezoelectric performance and a high Curie temperature, can meet requirements of medicine and military application having very high requirements on material stability, and has good research and application value.
Description
Technical field
The present invention relates to a kind of crystalline material, more particularly to a kind of ternary ferroelectric solid solution crystals material.Tool
For body, the present invention relates to have the ferroelectric sosoloid monocrystalline of B positions composite construction
(1-x-y)Pb(Sc1/2Nb1/2)O3-yPb(Mg1/3Nb2/3)O3-xPbTiO3(0<x<1,0<y<1,0<1-x-y<1),
And its growth technique, structure and electric property, belong to crystal technology and functional crystal field.
Background technology
Lead-based perovskite structure solid solution, especially with lead titanates as a kind of solid-solution material of end-member composition,
Due to its excellent piezoelectric property mechanical-electric coupling field for example habitata, seabed identification, ultrasonic imaging,
Especially national defense construction aspect has extensive and important application for sensing and micro mechanical system.New relaxor ferroelectric
Monocrystalline (1-x) Pb (Mg1/3Nb2/3)O3-xPbTiO3And (1-x) Pb (Zn (PMN-PT)1/3Nb2/3)O3-xPbTiO3
(PZN-PT) successful growth, has greatly accelerated the development of acoustic transducer device of new generation, becomes ferroelectricity field
Milestone in development history, is referred to as ferroelectricity field 50 years in history " once exciting by doctor L.C.Cross
The breakthrough of the popular feeling ".This kind of relaxor ferroelectric monocrystal or becomes high performance underwater sound transducing of new generation
The core piezoelectric of device, medical supersonic transducer, sensor and driver, it causes ultrasonic transducer
The performance such as bandwidth and high-energy-density is greatly improved, and in novel high-performance acoustic transducer field, is subject to
The extensive attention of people.But, such material Curie temperature (<170 DEG C) and phase transition temperature (60-80 DEG C)
It is relatively low so as to which that application is restricted.Therefore, new high-curie temperature, high-performance ferroelectric piezoelectric is explored
Monocrystal material just becomes the trend and focus of ferroelectric piezoelectric Materials of future generation.
Lead scandate columbate [Pb (Sc1/2Nb1/2)O3] (PSN) belong to A (B'1/2B”1/2)O3One compounds of group, tool
There are complex perovskite structure, room temperature subordinate tripartite's phase (counterfeit cubic symmetry), with PbTiO3(PT) (under room temperature
Tetragonal) form complete solid solution system (PSN-PT).But PSN-PT crystal growths face at present greatly
A difficult problem, the higher (T of the material melting pointm>1425 DEG C), there is higher requirement to crystal growing apparatus and crucible,
And difficulty is crystallized, it is difficult to grow large-sized monocrystalline.Therefore, also rarely have at present by PSN with it is above-mentioned
The technology report of PMN-PT or PZN-PT combinations.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, there is provided a kind of brand-new lead scandate columbate-magnoniobate
The growth technique of lead-lead titanates (PSN-PMN-PT) crystal, using the technique different compositions can be prepared,
The especially PSN-PMN-PT crystal of quasi- homotype phase boundary regions (MPB areas), the crystal has high
Curie temperature and phase transition temperature, while having excellent piezoelectric property concurrently.
To realize the object of the invention, the present invention is adopted the following technical scheme that：
A kind of ferroelectric sosoloid monocrystalline lead scandate columbate-PMN-PT, the crystal-chemical formula is
(1-x-y)Pb(Sc1/2Nb1/2)O3-yPb(Mg1/3Nb2/3)O3-xPbTiO3, wherein, 0<x<1,0<y<1,
0<1-x-y<1, it is the unlimited miscible perovskite type ferroelectric sosoloid monocrystal of a class ternary, the crystal has one
Quasi- homotype phase boundary regions.
Preferably, wherein, 0.2≤x≤0.7；It is furthermore preferred that 0.4≤x≤0.6.Preferably, wherein, y=0.1～0.4.
The invention provides the preparation method of above-mentioned ferroelectric sosoloid monocrystalline lead scandate columbate-PMN-PT,
It adopts top seed crystal growth technique, comprises the steps：
1) raw material is weighed according to the stoichiometric proportion of the PSN-PMN-PT chemical formulas；Prepare flux；
The raw material is mixed with flux, loads platinum crucible；
2) crucible is put in molten salt furnace, seed crystal is fixed in seed rod；Be warming up to 1050～1070 DEG C it is (excellent
Select 1060 DEG C), 1～4d of constant temperature (preferably 2～3d), lower seed crystal determines saturation point for 1030-1040 DEG C,
Then crystal growth is carried out with the speed cooling of 0.5～2 DEG C/d (preferably 1～1.5 DEG C/d), is down to 900～1000 DEG C
Lift crystal when (preferably 950 DEG C), anneal, obtain the ferroelectric sosoloid monocrystalline lead scandate columbate-niobium of the present invention
Magnesium titanate-zirconate (PSN-PMN-PT).
Preferably, the seed crystal is adopted and is obtained with the following method：
A) raw material is weighed according to the stoichiometric proportion of the PSN-PMN-PT chemical formulas；Prepare flux；
The raw material is mixed with flux, loads platinum crucible；
B) crucible is put in molten salt furnace, platinum wire is fixed in seed rod；Be warming up to 1050～1070 DEG C it is (excellent
Select 1060 DEG C), 1～4d of constant temperature (preferably 2～3d), lower platinum wire, with 2～10 DEG C/d (preferably 4～6 DEG C/d,
More preferably 5 DEG C/d) speed cooling carry out crystal growth, when being down to 900～1000 DEG C (preferably 950 DEG C)
Lift crystal, anneal, take out crystal, cutting and grinding prepares the seed crystal.
Wherein, the step 1 in said method) or step A) in flux include PbO and B2O3, it is excellent
Choosing is by PbO and B2O3Composition.Wherein, PbO and B2O3Mol ratio be 4～8:1, preferably 6:1.
Wherein, the step 1 in said method) or step A) in raw material include PbO, Sc2O3、MgO、
Nb2O5And TiO2。
Wherein, the step 1 in said method) or step A) in raw material be with the mol ratio of flux
1:5～10, preferably 1:6～8, more preferably 1:7.
Wherein, the step 1 in said method) or step A) be specially：
By initial feed PbO, Sc2O3、MgO、Nb2O5And TiO2According to the lead scandate columbate-magnoniobate
The stoichiometric proportion of the chemical formula of lead-lead titanates is weighed, and including PbO and B2O3(the two mole
Compare PbO:B2O3For 4～8:1, preferably 6:1) flux is with 1:5～10 (preferably 1:6～8, more preferably 1:7)
The ratio mixed grinding of (mol ratio), loads platinum crucible.
Wherein, the step 2 in said method) in intensification before step be specially：
Crucible is put in molten salt furnace, in tune, seed crystal platinum wire is tied up in seed rod one end, and barre is mounted in
On grate, in tune, during stove, crucible and seed rod three are adjusted together, it is ensured that its center is in straight line
On, cover bell.
Wherein, step B in said method) in intensification before step be specially：
Crucible is put in molten salt furnace, in tune, platinum wire is tied up in seed rod one end, and barre is mounted on grate,
In tune, during stove, crucible and seed rod three are adjusted together, it is ensured that its center point-blank, covers
Bell.
Wherein, the step 2 in said method) or step B) in annealing after temperature be room temperature, about 10～30 DEG C
(preferably 20～30 DEG C).
The PSN-PMN-PT crystal of the present invention, by methods described, and the setting of the x and y is (e.g.,
Wherein, 0<x<1, it is preferred that 0.2≤x≤0.7, it is furthermore preferred that 0.4≤x≤0.6；0<y<1, it is preferred that y=0.1～0.4)
Can obtain consisting of the PSN-PMN-PT crystal in MPB areas, that is, there is a quasi- homotype phase boundary regions, tool
Be improved Curie temperature (>200 DEG C, e.g., from about 230 DEG C) and phase transition temperature (>130 DEG C), higher than PMN-PT
With the Curie temperature (about 170 DEG C) and phase transition temperature (about 60 DEG C) of PZN-PT.Specifically, it is described
Ternary ferroelectric solid solution crystals, while excellent piezoelectric property is kept, with the Curie temperature for improving, energy
Enough meet the higher application demand of temperature range requirements.
The invention has the beneficial effects as follows：
There are a quasi- homotype phase boundary regions in the PSN-PMN-PT of the present invention, and be oriented growth, as
The ferroelectric sosoloid material of B positions composite construction, with excellent piezoelectric property and high Curie temperature, can
The demand of the satisfaction medical science very high to stability of material requirement and Military Application, with good researching value.
Meanwhile, the present invention can realize the solid solution of any ratio of PSN, PMN and PT, can be according to practical application
Demand, grow the PSN-PMN-PT crystal of any ratio, break the growth bottleneck of Bridgman-Stockbarger method.
The invention also discloses a kind of growing method of new PSN-PMN-PT, it was found that a kind of brand-new
Flux (PbO and B2O3Composite fluxing agent), it was found that the growth temperature of an optimum is interval
(1040-950 DEG C), grows the unlimited miscible high-quality PSN-PMN-PT crystal of different compositions.
Determine that crystal is pure perovskite structure with X-ray powder diffraction；(001) dielectric of the crystal cut in direction
Temperature spectrum shows its Curie temperature>200 DEG C, phase transition temperature>130℃；Ferroelectric hysteresis loop has perfectly rectangular degree,
Coercive field is about 4kV/cm, and residual polarization is about 30 μ C/cm2；Piezoelectric constant is 1500pC/N to the maximum.
Description of the drawings：
The PSN-PMN-PT crystal that Fig. 1 growths are obtained
The powder diffraction spectrum of Fig. 2 PSN-PMN-PT crystal
The dielectric temperature spectrum of Fig. 3 PSN-PMN-PT crystal
The ferroelectric hysteresis loop of Fig. 4 PSN-PMN-PT crystal
Fig. 5 PSN-PMN-PT ternary system phasors
Specific embodiment
Below by way of specific embodiment, the present invention is described in further detail, but should not be interpreted as this
The scope of the present invention is only limitted to Examples below.In the case of without departing from said method thought of the present invention, root
The various replacements made according to ordinary skill knowledge and customary means or change, should be included in the present invention
In the range of.
Embodiment 1：PSN-PMN-PT crystal is grown using top-seeded solution growth, the chemical formula of the crystal is：
(1-x-y)Pb(Sc1/2Nb1/2)O3-yPb(Mg1/3Nb2/3)O3-xPbTiO3, wherein, x=0.4～0.6,
Y=0.1～0.4,0.1<1-x-y<0.4.
Prepare seed crystal：
A () dispensing, by the stoichiometric proportion of above-mentioned chemical formula PbO, Sc are weighed2O3、Nb2O5、TiO2With
B2O3Raw material, mixing, grinding, loads platinum crucible.
B () ties up seed crystal, platinum wire is tied up in one end of seed rod.
C () shove charge, crucible is put in molten salt furnace, seed rod is fixed on grate, in tune, it is ensured that stove,
Crucible, seed crystal three center point-blank, cover bell.
D () grows, set temperature program, is warming up to 1060 DEG C, and constant temperature 2d, lower platinum wire, 5 DEG C/d drops
Temperature, starts crystal growth；Lift crystal when being down to 950 DEG C, be annealed to room temperature, take out crystal, cutting is ground
Mill prepares the seed crystal.
Prepare PSN-PMN-PT crystal：
(1) dispensing, by the stoichiometric proportion of above-mentioned chemical formula PbO, Sc are weighed2O3、Nb2O5、TiO2With
B2O3Raw material, mixing, grinding, loads platinum crucible.
(2) seed crystal is tied up, the above-mentioned seed crystal platinum wire for cutting is tied up in one end of seed rod.
(3) shove charge, crucible is put in molten salt furnace, and seed rod is fixed on grate, in tune, it is ensured that stove,
Crucible, seed crystal three center point-blank, cover bell.
(4) grow, set temperature program, be warming up to 1060 DEG C, constant temperature 2d, lower seed crystal determines saturation
Point is 1040 DEG C, 1 DEG C/d coolings, starts crystal growth.
(5) anneal, temperature is down to 950 DEG C or so, and crystalline size is sufficiently large, slowly lift crystal, 2d drops
To room temperature, crystal is taken out in blow-on.
The ferroelectric crystal that sample derived above is present invention development is as shown in Figure 1.
Embodiment 2：The structure determination of crystal.
Using X-ray powder diffraction, the structure of crystal is determined.Instrument is Japan
RIGAKU-DMAX2500 powder diffractometers (Cu targets, λ=0.154056nm, graphite monochromator),
Concrete test condition is that under room temperature, measurement angular range is 10-80 °, and the step-length for adopting is 0.02 ° (2 θ), when
Between 2s/step.The powder diffraction result for obtaining is as shown in Figure 2.
As it is clear from fig. 2 that PSN-PMN-PT crystal is respectively provided with pure perovskite structure, and with PT contents
Be incremented by, the transition in tripartite-MPB- four directions is presented.
Embodiment 3：The electricity performance measurement of crystal.
Part wear down, polishing are cut from bulky crystal along (001) direction, silver paste is coated on two sides, for electricity
The measurement of performance.
Dielectricity is measured：Instrument be Alpha's dielectric/impedance Analytical high resolution instrument (Novolcontrol,
German), temperature-measuring range -50～400 DEG C, 1～1kHz of frequency range, small-signal test voltage 1Vrms.
Ferroelectricity is measured：Instrument is the standard ferroelectricity measuring systems of TF 2000, and temperature conditionss are room temperature,
Frequency used is 2Hz.
Piezoelectricity is measured：ZJ-4AN quasistatics d that instrument is developed by Chinese Academy of Sciences's acoustics33Measuring instrument,
Test condition is room temperature.
Specific measurement result is as shown in Figure 3 and Figure 4.
It can be seen from figure 3 that PSN-PMN-PT crystal shows as common ferroelectric dielectric response behavior, its residence
In temperature be about 230 DEG C, phase transition temperature>130℃.
As seen from Figure 4, there is the ferroelectric hysteresis loop of perfect rectangular configuration under PSN-PMN-PT crystal room temperature, its
Coercive field is about 4kV/cm, and residual polarization is about 30 μ C/cm2。
Claims (10)
1. a kind of ferroelectric sosoloid monocrystalline lead scandate columbate-PMN-PT, it is characterised in that the list
Brilliant chemical formula is (1-x-y) Pb (Sc1/2Nb1/2)O3-yPb(Mg1/3Nb2/3)O3-xPbTiO3, wherein,
0<x<1,0<y<1,0<1-x-y<1, it is the unlimited miscible perovskite type ferroelectric sosoloid monocrystal of a class ternary,
There are a quasi- homotype phase boundary regions in the crystal.
2. ferroelectric sosoloid monocrystalline lead scandate columbate-PMN-PT according to claim 1, its
It is characterised by, wherein, 0.2≤x≤0.7；It is furthermore preferred that 0.4≤x≤0.6.It is also preferred that y=0.1～0.4.
3. the system of the ferroelectric sosoloid monocrystalline lead scandate columbate-PMN-PT described in claim 1 or 2
Preparation Method, it is characterised in that methods described adopts top seed crystal growth technique, comprises the steps：
1) raw material is weighed according to the stoichiometric proportion of the chemical formula of the lead scandate columbate-PMN-PT；
Prepare flux；The raw material is mixed with flux, loads platinum crucible；
2) crucible is put in molten salt furnace, seed crystal is fixed in seed rod；Be warming up to 1050～1070 DEG C it is (excellent
Select 1060 DEG C), 1～4d of constant temperature (preferably 2～3d), lower seed crystal determines saturation point for 1030-1040 DEG C,
Then crystal growth is carried out with the speed cooling of 0.5～2 DEG C/d (preferably 1～1.5 DEG C/d), is down to 900～1000 DEG C
Lift crystal when (preferably 950 DEG C), anneal, obtain the ferroelectric sosoloid monocrystalline lead scandate columbate-niobium of the present invention
Magnesium titanate-zirconate.
4. preparation method according to claim 3, it is characterised in that the seed crystal is adopted with the following method
It is obtained：
A) raw material is weighed according to the stoichiometric proportion of the chemical formula of the lead scandate columbate-PMN-PT；
Prepare flux；The raw material is mixed with flux, loads platinum crucible；
B) crucible is put in molten salt furnace, platinum wire is fixed in seed rod；Be warming up to 1050～1070 DEG C it is (excellent
Select 1060 DEG C), 1～4d of constant temperature (preferably 2～3d), lower platinum wire, with 2～10 DEG C/d (preferably 4～6 DEG C/d,
More preferably 5 DEG C/d) speed cooling carry out crystal growth, when being down to 900～1000 DEG C (preferably 950 DEG C)
Lift crystal, anneal, take out crystal, cutting and grinding prepares the seed crystal.
5. the preparation method according to claim 3 or 4, it is characterised in that the step in said method
1) or step A) in flux include PbO and B2O3, preferably by PbO and B2O3Composition.Wherein,
PbO and B2O3Mol ratio be 4～8:1, preferably 6:1.
6. the preparation method according to any one of claim 3-5, it is characterised in that in said method
Step 1) or step A) in raw material include PbO, Sc2O3、MgO、Nb2O5And TiO2。
7. the preparation method according to any one of claim 3-6, it is characterised in that in said method
Step 1) or step A) in the mol ratio of raw material and flux be 1:5～10, preferably 1:6～8, more preferably
1:7。
8. the preparation method according to any one of claim 3-7, it is characterised in that in said method
Step 1) or step A) be specially：
By initial feed PbO, Sc2O3、MgO、Nb2O5And TiO2According to the lead scandate columbate-magnoniobate
The stoichiometric proportion of the chemical formula of lead-lead titanates is weighed, and including PbO and B2O3(the two mole
Compare PbO:B2O3For 4～8:1, preferably 6:1) flux is with 1:5～10 (preferably 1:6～8, more preferably 1:7)
The ratio mixed grinding of (mol ratio), loads platinum crucible.
9. the preparation method according to any one of claim 3-8, it is characterised in that in said method
Step 2) in intensification before step be specially：
Crucible is put in molten salt furnace, in tune, seed crystal platinum wire is tied up in seed rod one end, and barre is mounted in
On grate, in tune, during stove, crucible and seed rod three are adjusted together, it is ensured that its center is in straight line
On, cover bell.
Wherein, step B in said method) in intensification before step be specially：
Crucible is put in molten salt furnace, in tune, platinum wire is tied up in seed rod one end, and barre is mounted on grate,
In tune, during stove, crucible and seed rod three are adjusted together, it is ensured that its center point-blank, covers
Bell.
10. the preparation method according to any one of claim 3-9, it is characterised in that in said method
Step 2) or step B) in annealing after temperature be room temperature, about 10～30 DEG C (preferably 20～30 DEG C).
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| CN112853467A (en) * | 2019-11-28 | 2021-05-28 | 中国科学院福建物质结构研究所 | Boron potassium niobate crystal, preparation method thereof and application thereof as antiferroelectric material |
| CN117105663A (en) * | 2023-09-03 | 2023-11-24 | 森霸传感科技股份有限公司 | Low-temperature sintered ternary solid solution medium ceramic material and preparation method thereof |
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| CN112853467A (en) * | 2019-11-28 | 2021-05-28 | 中国科学院福建物质结构研究所 | Boron potassium niobate crystal, preparation method thereof and application thereof as antiferroelectric material |
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| CN112062564B (en) * | 2020-09-17 | 2022-05-17 | 广西大学 | Preparation method of PMN-PSN ultrahigh breakdown electric field thin film material |
| CN117105663A (en) * | 2023-09-03 | 2023-11-24 | 森霸传感科技股份有限公司 | Low-temperature sintered ternary solid solution medium ceramic material and preparation method thereof |
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