CN104153000B - Ternary system relaxation type monocrystalline piezoelectric material and growing method thereof - Google Patents
Ternary system relaxation type monocrystalline piezoelectric material and growing method thereof Download PDFInfo
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Abstract
The invention discloses a kind of ternary system relaxation type monocrystalline piezoelectric material and growing method thereof, its chemical formula is xPb (Mg1/3Nb2/3)O3‑yBiAlO3‑(1‑x‑y)PbTiO3, wherein 0 x 1,0 y 1, and x+y 1.Growing method is: step A) weigh Bi2O3、MgO、Nb2O5、TiO2And Al2O3, at high temperature pre-burning；Step B) mix with the oxide of lead again and briquetting；Step C) load in crucible and at 500～1250 DEG C, be incubated 3～20h, continuation liter high-temperature, to 1340～1410 DEG C, is incubated 3～20h, and made to expect all fusings, declining with 0.1～1.2mm/h speed and gradually crystallize, interface temperature gradient is 20～100 DEG C/cm；Step D) grow complete, it is cooled to room temperature with 10～300 DEG C/h speed.The method of the present invention can grow different orientation, difformity and various sizes of piezoquartz as required, has the advantages such as process equipment is simple and convenient to operate, a stove is voluminous, is suitable for growth or the production of industrial scale crystal.
Description
Technical field
The invention belongs to piezoelectric crystal material field, be specifically related to a kind of ternary system relevant with PMN-PT
Piezoelectric monocrystal and growing method thereof.
Background technology
Piezoelectric is the weight utilizing piezoelectric effect to realize the most mutually conversion between electric energy and mechanical energy
Want functional material, be widely used in aviation, the energy, automobile making, communication, household electrical appliances, detect and calculate
The numerous areas such as machine, are to constitute the electronic components such as wave filter, transducer, sensor, piezoelectric transformer
Vitals, it has also become one of main direction of studying of 21 century new and high technology.Binary pressure for a long time
Electroceramics lead zirconate titanate (PZT) is widely used due to its higher Curie temperature and stable performance.
However as science and technology development, various high-performance, high precision instrument making to piezoelectric
Performance also been proposed higher requirement.Scientists have developed lead magnesio-niobate-titanium under this background
Lead plumbate (PMN-PT) and lead zinc niobate-lead titanates (PZN-PT) relaxation Ferroelectric piezoelectric monocrystal, its strain
Amount is more than 10 times of PZT pottery.Internationally famous Science and Nature impurity is respectively 1997
It is described by March in year and in January, 2000.The piezoelectric coefficient d of piezoelectric monocrystal PMN-PT33
With electromechanical coupling factor k33PZT piezoelectric ceramics than usually 600pC/N and about 70% to exceed
Many, respectively reaches 2500pC/N and more than 92%；Its dependent variable is higher than conventionally used piezoelectric ceramics
Go out an order of magnitude, reached 1.7% it is considered to be piezoelectricity field over 50 years the most breathtaking one
Secondary breakthrough, causes the very big concern of ferroelectricity and piezoelectricity field scholar.
Relaxation Ferroelectric monocrystalline is due to its piezoelectric property excellent near quasi-homotype phase boundary (MPB)
Developed by the research worker of various places.Toshiba Corp, the IBLE company of Korea S all utilize
PZN-PT crystal has produced ultrasonic transducer array, compared with mutually isostructural PZT ceramic transducer,
Its sensitivity and bandwidth all increased.Also there are the exploitation of Related product in the companies such as Philips, GE, real
Show business application.Relaxation Ferroelectric monocrystalline PZN-PT and PMN-PT not only leads at medical transducer
Apply on territory, also had well performance in the field such as underwater acoustic transducer and ultrasonic motor.
Summary of the invention
The present invention introduces another set unit on the basis of relaxor ferroelectric monocrystal material PMN-PT
BiAlO3, define a kind of new ternary system relaxation type monocrystalline piezoelectric material with excellent properties
xPb(Mg1/3Nb2/3)O3-yBiAlO3-(1-x-y)PbTiO3.It has superior pressure as PMN-PT
Electricity, mechanical-electric coupling performance and less dielectric loss so that it is in ultrasonic transducer, driver and sensing
The aspects such as device have huge and are widely applied prospect.
It is an object of the invention to provide a kind of ternary system relaxation type monocrystalline piezoelectric material, described piezoelectric monocrystal
The chemical formula of material is xPb (Mg1/3Nb2/3)O3-yBiAlO3-(1-x-y)PbTiO3, wherein 0 x 1,0
Y 1 and x+y 1.Preferably, 0.2≤x≤0.7,0 y≤0.4, it is highly preferred that 0.5≤x≤0.6,
0.05≤y≤0.2。
Another object of the present invention is to provide a kind of ternary system relaxation type piezoelectric monocrystal growing the present invention
The method of material, described method is Bridgman-Stockbarger method, specifically includes following steps:
Step A) press xPb (Mg1/3Nb2/3)O3-yBiAlO3-(1-x-y)PbTiO3Stoichiometric proportion weigh
Bi2O3、MgO、Nb2O5、TiO2And Al2O3, mix homogeneously, then the temperature of 900～1250 DEG C
Lower pre-burning 2～15h, wherein 0 x 1,0 y 1 and x+y 1；
Step B) by step A) material after pre-burning mixes with the oxide of the lead stoichiometrically weighed
Close uniform crystal growth with expecting；
Step C) use crystal growth to expect and be pressed into block and load in the crucible being placed with seed crystal, by crucible
Insert in decline stove, at a temperature of 500～1250 DEG C, be incubated 3～20h, continue to rise high-temperature to 1340～1410
DEG C, it is incubated 3～20h, makes crystal growth with expecting fusing, and make the top of seed crystal melt, then earthenware
Crucible declines with 0.1～1.2mm/h speed, and gradually crystalline growth becomes crystal, the thermograde of growth interface
It is 20～100 DEG C/cm；
Step D) treat that crystal growth is complete, it is cooled to room temperature with the speed of 10～300 DEG C/h, obtains ternary
It it is relaxation type monocrystalline piezoelectric material.
Step A) in, by the pre-burning of raw material, it is possible to obtain intermediate product, preferably 1100～1250
Pre-burning 8～15h at a temperature of DEG C；Step B) in, the oxide of described lead is PbO, Pb3O4Or they
The mixture of the two.
Step B) can further include: by step A) material after pre-burning with stoichiometrically claim
The oxide mix homogeneously of the lead taken, then at 700～1000 DEG C, pre-burning 1～8h obtains crystal growth and uses
Expect, such as can at 700～800 DEG C pre-burning 2～5h, or pre-burning 1～3h at 800～1000 DEG C
Obtain crystal growth with rise expect.Step B) in there is volatility, so the temperature of pre-burning is less than due to lead
Step A) calcined temperature.Step B) by pre-burning, it is more beneficial for the growth of crystal.
Step C) in seed crystal can be selected to be oriented to (111), (001), (110) or the seed crystal of (211).
Step C) in seed crystal be Pb (Mg1/3Nb2/3)O3-PbTiO3Or xPb (Mg1/3Nb2/3)O3-yBiAlO3-
(1-x-y)PbTiO3Crystal.
Step C) in the material of crucible be platinum or iraurite；When selecting Iridium Crucible, this area is general
Logical technical staff should appreciate that it is to carry out under reducing atmosphere or inert atmosphere protection, such as argon hydrogen gaseous mixture
Or argon etc..Crucible be sealed after insert decline stove in.
Step C) in preferably at a temperature of 800～1200 DEG C be incubated 8～12h, then proceed to a liter high-temperature
To 1350～1400 DEG C, being incubated 4～12h, crucible declines with 0.3～0.8mm/h speed, growth interface
Thermograde is 20～80 DEG C/cm；
Step D) in preferably, rate of cooling is 30～80 DEG C/h.
The size utilizing the monocrystalline that the method for the present invention grows is 1～6 inch, preferably 2～4 inches；Monocrystalline
Be shaped as cylinder, cuboid or other arbitrary shape.
The most progressive effect of the present invention is: the present invention is at Pb (Mg1/3Nb2/3)O3-PbTiO3Basis
On introduce a certain amount of BiAlO3, reduce the usage amount of lead in crystal, thus decrease at crystalline substance
The environmental pollution caused due to the existence of lead in body preparation and use.And the crystal tool that the present invention relates to
There is superior piezoelectricity, mechanical-electric coupling performance and less dielectric loss, such as the tripartite's phase crystal grown
(001) direction is through testing its piezoelectric constant d33> 1800pC/N, electromechanical coupling factor k33> 0.90, damage
Consumption angle tangent tan δ 0.5, so that it is at aspects such as ultrasonic transducer, driver and senser elements
Have huge and be widely applied prospect.Additionally, the crystal grown by the present invention to have crystal defect few,
Yield rate is high, and the size of the crystal of growth, shape and orientation are easily controlled, and temperature gradient of solid-liquid interface can
With the least thus prevent the advantages such as crystal cleavage.It is additionally, the method process equipment is simple, easy to operate,
Energy consumption is low, is advantageously implemented industrialized production.
Accompanying drawing explanation
Fig. 1 is the 0.50Pb (Mg that embodiment 1 obtains1/3Nb2/3)O3-0.17BiAlO3-0.33PbTiO3Brilliant
The XRD figure spectrum of body.
Detailed description of the invention
Embodiment 10.50Pb (Mg1/3Nb2/3)O3-0.17BiAlO3-0.33PbTiO3The preparation of monocrystalline
By high pure raw material MgO, Nb2O5、TiO2、Bi2O3And Al2O3By 0.50Pb (Mg1/3Nb2/3)O3-
0.17BiAlO3-0.33PbTiO3After molecular formula dispensing mix homogeneously, it is incubated at a temperature of 1100 DEG C
10h, then mixes with the PbO stoichiometrically weighed and carries out briquetting by isostatic cool pressing the most afterwards, with
The selected seed crystal being oriented to (111) is placed in cylindrical platinum crucible together, and sealed crucible is placed on earthenware
Crucible carries out crystal growth in declining stove, and furnace temperature first rises to 1000 DEG C of insulation 3h, is then further continued for heating up
Make, to 1350 DEG C of insulation 5h, fusing of expecting, and adjusted bushing position and make seed crystal top melt, growth circle
Surface temperature gradient is 50 DEG C/cm, declines crucible with the speed of 0.4mm/h, treats that crystal has all grown
After, it is cooled to room temperature with the speed of 60 DEG C/h, just obtains the complete of cylinder
0.50Pb(Mg1/3Nb2/3)O3-0.17BiAlO3-0.33PbTiO3Monocrystalline, its XRD figure is composed as shown in Figure 1.
Embodiment 20.67Pb (Mg1/3Nb2/3)O3-0.10BiAlO3-0.23PbTiO3The preparation of monocrystalline
By high pure raw material MgO, Nb2O5、TiO2、Bi2O3And Al2O3By 0.67Pb (Mg1/3Nb2/3)O3-
0.10BiAlO3-0.23PbTiO3After molecular formula dispensing mix homogeneously, at a temperature of 1200 DEG C, it is incubated 12h,
Then with the Pb stoichiometrically weighed3O4After mixing all, then at a temperature of 800 DEG C, it is incubated 4h,
Then carry out briquetting by isostatic cool pressing, be placed in cuboid platinum together with the selected seed crystal being oriented to (001)
In gold crucible, sealed crucible is placed in crucible declines stove and carries out crystal growth, first at 1100 DEG C
At a temperature of be incubated 2h, be then further continued for being warming up to 1360 DEG C of insulation 8h and made fusing of expecting, and adjust earthenware
Crucible position makes seed crystal top melt, and growth interface thermograde is 80 DEG C/cm, with the speed of 0.6mm/h
Decline crucible, after crystal has all grown, be cooled to room temperature with the speed of 40 DEG C/h, just obtain
It is shaped as the complete 0.67Pb (Mg of cuboid1/3Nb2/3)O3-0.10BiAlO3-0.23PbTiO3Monocrystalline.
Embodiment 30.56Pb (Mg1/3Nb2/3) O3-0.08BiAlO3-0.36PbTiO3The preparation of monocrystalline
By high pure raw material MgO, Nb2O5、TiO2、Bi2O3And Al2O3By 0.56Pb (Mg1/3Nb2/3) O3
-0.08BiAlO3-0.36PbTiO3After molecular formula dispensing mix homogeneously, it is incubated at a temperature of 1100 DEG C
6h, is then PbO and Pb of 1:1 with the mol ratio stoichiometrically weighed3O4Mixing is passed through the most afterwards
Isostatic cool pressing carries out briquetting, is placed in cylindrical Iridium Crucible together with the selected seed crystal being oriented to (100)
In, sealed crucible is placed in crucible declines stove and carries out crystal growth, be passed through argon hydrogen gaseous mixture in stove and enter
Row protection, first rises to 1200 DEG C of insulation 3h by furnace temperature, is then further continued for being warming up to 1400 DEG C of insulation 3h
Having melted and expected, and adjusted bushing position and make seed crystal top melt, growth interface thermograde is 80 DEG C
/ cm, declines crucible, after crystal has all grown, with the speed of 80 DEG C/h with the speed of 0.3mm/h
Degree is cooled to room temperature, just obtains complete 0.56Pb (Mg1/3Nb2/3) O of cylinder3-0.08
BiAlO3-0.36PbTiO3Monocrystalline.
Embodiment 40.32Pb (Mg1/3Nb2/3) O3-0.40BiAlO3-0.28PbTiO3The preparation of monocrystalline
By high pure raw material MgO, Nb2O5、TiO2、Bi2O3And Al2O3By 0.32Pb (Mg1/3Nb2/3) O3
-0.40BiAlO3-0.28PbTiO3After molecular formula dispensing mix homogeneously, it is incubated at a temperature of 1180 DEG C
4h, is then PbO and Pb of 2:1 with the mol ratio stoichiometrically weighed3O4Exist again after mixing all
It is incubated 2h at a temperature of 900 DEG C, then carries out briquetting by isostatic cool pressing, be oriented to (211) with selected
Seed crystal be placed in together in circular platinum crucible, sealed crucible is placed in crucible declines stove and carries out crystal
Growth, first rises to 800 DEG C of insulation 12h by furnace temperature, is then further continued for being warming up to 1300 DEG C of insulation 10h and melts
Having changed and expected, and adjusted bushing position and make seed crystal top melt, growth interface thermograde is 60 DEG C/cm,
Declining crucible with the speed of 0.7mm/h, after crystal has all grown, the speed with 70 DEG C/h is cold
But arrive room temperature, just obtain complete 0.32Pb (Mg1/3Nb2/3) O of cylinder3-0.40
BiAlO3-0.28PbTiO3Monocrystalline.
Effect example
0.50Pb (Mg by embodiment 1 gained1/3Nb2/3)O3-0.17BiAlO3-0.33PbTiO3Monocrystalline is pressed
More solito tests its piezoelectric property, electromechanical coupling factor, loss angle and phase transition temperature.
Result shows, the 0.50Pb (Mg that embodiment 1 is grown1/3Nb2/3)O3-0.17BiAlO3-
0.33PbTiO3Piezoelectric constant d in monocrystalline tripartite phase crystal (001) direction33>1800pC/N, mechanical-electric coupling
Coefficient k33> 0.90, losstangenttanδ 0.5.
Claims (11)
1. a ternary system relaxation type monocrystalline piezoelectric material, it is characterised in that described monocrystalline piezoelectric material
Chemical formula is xPb (Mg1/3Nb2/3)O3-yBiAlO3-(1-x-y)PbTiO3, wherein 0 ＜ x ＜ 1,0 ＜ y ＜ 1
And x+y ＜ 1.
Ternary system relaxation type monocrystalline piezoelectric material the most according to claim 1, it is characterised in that
0.2≤x≤0.7,0 ＜ y≤0.4.
Ternary system relaxation type monocrystalline piezoelectric material the most according to claim 2, it is characterised in that
0.5≤x≤0.6,0.05≤y≤0.2.
4. the method growing ternary system relaxation type monocrystalline piezoelectric material described in claim 1, its
Being characterised by, described method is Bridgman-Stockbarger method, specifically includes following steps:
Step A) press xPb (Mg1/3Nb2/3)O3-yBiAlO3-(1-x-y)PbTiO3Stoichiometric proportion weigh
Bi2O3、MgO、Nb2O5、TiO2And Al2O3, mix homogeneously, then the temperature of 900～1250 DEG C
Lower pre-burning 2～15h, wherein 0 ＜ x ＜ 1,0 ＜ y ＜ 1 and x+y ＜ 1；
Step B) by step A) material after pre-burning mixes with the oxide of the lead stoichiometrically weighed
Close uniform crystal growth with expecting；
Step C) use crystal growth to expect and be pressed into block and load in the crucible being placed with seed crystal, by crucible
Insert in decline stove, at a temperature of 500～1250 DEG C, be incubated 3～20h, continue to rise high-temperature extremely
1340～1410 DEG C, it is incubated 3～20h, makes crystal growth with expecting fusing, and make the top of seed crystal melt,
Then crucible declines with 0.1～1.2mm/h speed, and gradually crystalline growth becomes crystal, the temperature of growth interface
Degree gradient is 20～100 DEG C/cm；
Step D) treat that crystal growth is complete, it is cooled to room temperature with the speed of 10～300 DEG C/h, obtains ternary
It it is relaxation type monocrystalline piezoelectric material.
Method the most according to claim 4, it is characterised in that step A) in, at 1100～1250 DEG C
At a temperature of pre-burning 8～15h；Step B) in, the oxide of described lead is PbO, Pb3O4Or they two
The mixture of person.
Method the most according to claim 4, it is characterised in that step B) may further comprise: by
Step A) material after pre-burning mixs homogeneously with the oxide of the lead stoichiometrically weighed, then exists
At 700～1000 DEG C pre-burning 1～8h obtain crystal growth with rise expect.
Method the most according to claim 6, it is characterised in that by step A) material after pre-burning
Mix homogeneously with the oxide of the lead stoichiometrically weighed, then pre-burning at 700～800 DEG C
2～5h, or at 800～1000 DEG C pre-burning 1～3h obtain crystal growth with rise expect.
Method the most according to claim 4, it is characterised in that step C) in seed crystal be selected taking
To for (111), (001), (110) or the seed crystal of (211).
Method the most according to claim 4, it is characterised in that step C) in seed crystal be
Pb(Mg1/3Nb2/3)O3-PbTiO3Or xPb (Mg1/3Nb2/3)O3-yBiAlO3-(1-x-y)PbTiO3Crystal.
Method the most according to claim 4, it is characterised in that step C) in the material of crucible be platinum
Gold or iraurite；Insert after crucible is sealed in decline stove.
11. methods according to claim 4, it is characterised in that step C) at 800～1200 DEG C
At a temperature of be incubated after 8～12h, continue to rise high-temperature to 1350～1400 DEG C, be incubated 4～12h, crucible with
0.3～0.8mm/h speed declines, and the thermograde of growth interface is 20～80 DEG C/cm；Step D) in
Rate of cooling is 30～80 DEG C/h.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1382841A (en) * | 2002-03-12 | 2002-12-04 | 中国科学院上海硅酸盐研究所 | Melt method for growing sosoloid monocrystal of lead lead-titanate niobium-zincate |
| CN102817080A (en) * | 2012-09-04 | 2012-12-12 | 中国科学院上海硅酸盐研究所 | Lead lutetioniobate-lead magnesioniobate-lead titanate ternary-system relaxation ferroelectric monocrystal and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1382841A (en) * | 2002-03-12 | 2002-12-04 | 中国科学院上海硅酸盐研究所 | Melt method for growing sosoloid monocrystal of lead lead-titanate niobium-zincate |
| CN102817080A (en) * | 2012-09-04 | 2012-12-12 | 中国科学院上海硅酸盐研究所 | Lead lutetioniobate-lead magnesioniobate-lead titanate ternary-system relaxation ferroelectric monocrystal and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| Structural, Dielectric, and Ferroelectric Properties of BiAlO3–PbTiO3 Solid Solution Thin Films on Indium Tin Oxide-Coated Glass Substrates;Guangheng Wu, et al.;《J. Am. Ceram. Soc.》;20101231;第93卷(第4期);权利要求2 * |
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