CN104153000A - Ternary relaxation piezoelectric single crystal material and growing method thereof - Google Patents
Ternary relaxation piezoelectric single crystal material and growing method thereof Download PDFInfo
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- CN104153000A CN104153000A CN201310178564.XA CN201310178564A CN104153000A CN 104153000 A CN104153000 A CN 104153000A CN 201310178564 A CN201310178564 A CN 201310178564A CN 104153000 A CN104153000 A CN 104153000A
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Abstract
The invention discloses a ternary relaxation piezoelectric single crystal material and a growing method thereof. The chemical formula of the single crystal material is xPb(Mg1/3Nb2/3)O3-yBiAlO3-(1-x-y)PbTiO3, wherein x is more than 0 and less than 1; y is more than 0 and less than 1; x+y is less than 1. The growing method comprises the following steps: A) weighing and presintering Bi2O3, MgO, Nb2O5, TiO2 and Al2O3 under high temperature; B) mixing the materials with the oxide of lead and briquetting the mixture; C) putting the briquettes in a crucible and carrying out insulation at 500-1250 DEG C for 3-20 hours, continuously raising the temperature to 1340-1410 DEG C, carrying out insulation for 3-20 hours to melt all the starting materials and cooling at a speed of 0.1-1.2mm/h to gradually carry out crystallization, wherein the interface temperature gradient is 20-100 DEG C/cm; D) after growth is completed, cooling the crystals to the room temperature at a speed of 10-300 DEG C/h. The method can be adopted to grow piezoelectric crystals with different orientations, shapes and dimensions according to the requirements, has the advantages of simple process equipment, convenience in operation, productivity with one furnace and the like and is suitable for large-scale industrial growth or production of crystals.
Description
Technical field
The invention belongs to piezoelectric crystal material field, be specifically related to a kind of three component system piezoelectric monocrystal and the growth method thereof relevant with PMN-PT.
Background technology
Piezoelectric is to utilize piezoelectric effect to realize the critical function material of directly mutually changing between electric energy and mechanical energy, be widely used in the numerous areas such as aviation, the energy, automobile making, communication, household electrical appliances, detection and computer, be the vitals that forms the electronic components such as wave filter, transverter, sensor, piezoelectric transformer, become one of main direction of studying of 21 century new and high technology.Binary piezoelectric ceramics Pb-based lanthanumdoped zirconate titanates (PZT) is because its higher Curie temperature and stable performance are widely used for a long time.But along with scientific and technical development, the making of various high-performance, high precision instrument is had higher requirement again to the performance of piezoelectric.Under this background, scientists has been developed PMN-PT (PMN-PT) and lead zinc niobate-lead titanate (PZN-PT) relaxation Ferroelectric piezoelectric monocrystal, and its dependent variable is the more than 10 times of PZT pottery.Internationally famous Science and Nature impurity are introduced it in March, 1997 and in January, 2000 respectively.The piezoelectric coefficient d of piezoelectric monocrystal PMN-PT
33with electromechanical coupling factor k
33more high than the PZT piezoelectric ceramics that is generally 600pC/N and 70% left and right, more than reaching respectively 2500pC/N and 92%; Its dependent variable exceeds an order of magnitude than common piezoelectric ceramics used, has reached 1.7%, is considered to the most breathtaking once breakthrough of piezoelectricity field over 50 years, causes ferroelectric and very big concern piezoelectricity field scholar.
Relaxation Ferroelectric monocrystalline is because near its piezoelectric property excellent accurate homotype phase boundary (MPB) is developed by the researchist of various places.The IBLE company of Toshiba Corp, Korea S all utilizes PZN-PT crystal to produce ultrasonic transducer array, and compared with the PZT ceramic transducer of same structure, its sensitivity and bandwidth all increase to some extent.Also there is the exploitation of related products in the company such as Philips, GE, has realized commercial applications.Not only application to some extent on medical transducer field of relaxation Ferroelectric monocrystalline PZN-PT and PMN-PT, also has good performance in the field such as underwater acoustic transducer and ultrasonic motor.
Summary of the invention
The present invention has introduced an other constituent element BiAlO on the basis of relaxor ferroelectric monocrystal material PMN-PT
3, formed a kind of new three component system relaxation type monocrystalline piezoelectric material xPb (Mg with excellent properties
1/3nb
2/3) O
3-yBiAlO
3-(1-x-y) PbTiO
3.It has superior piezoelectricity, electromechanical coupling performance and less dielectric loss as PMN-PT, makes it have huge and application prospect widely at aspects such as ultrasonic transducer, driving mechanism and senser elements.
The object of the present invention is to provide a kind of three component system relaxation type monocrystalline piezoelectric material, the chemical formula of described monocrystalline piezoelectric material is xPb (Mg
1/3nb
2/3) O
3-yBiAlO
3-(1-x-y) PbTiO
3, wherein 0 ﹤ x ﹤ 1,0 ﹤ y ﹤ 1 and x+y ﹤ 1.Preferably, 0.2≤x≤0.7,0 ﹤ y≤0.4, more preferably, 0.5≤x≤0.6,0.05≤y≤0.2.
A kind of method that another object of the present invention is to provide three component system relaxation type monocrystalline piezoelectric material of the present invention of growing, described method is falling crucible method, specifically comprises the steps:
Steps A) press xPb (Mg
1/3nb
2/3) O
3-yBiAlO
3-(1-x-y) PbTiO
3stoichiometric ratio take Bi
2o
3, MgO, Nb
2o
5, TiO
2and Al
2o
3, mix then pre-burning 2～15h at the temperature of 900～1250 DEG C, wherein 0 ﹤ x ﹤ 1,0 ﹤ y ﹤ 1 and x+y ﹤ 1;
Step B) by steps A) material after pre-burning mix with the plumbous oxide compound taking by stoichiometric ratio crystal growth with expecting;
Step C) crystal growth has been used to expect be pressed into block and pack in the crucible that is placed with seed crystal, crucible is inserted in decline stove, at 500～1250 DEG C of temperature, be incubated 3～20h, continue rising temperature to 1340～1410 DEG C, insulation 3～20h, makes crystal growth with working the fusing of expecting, and the top of seed crystal is melted, then crucible declines with 0.1～1.2mm/h speed, and crystalline growth becomes crystal gradually, and the thermograde of growth interface is 20～100 DEG C/cm;
Step D) treat that crystal growth is complete, with the speed cool to room temperature of 10～300 DEG C/h, obtain three component system relaxation type monocrystalline piezoelectric material.
Steps A) in, by the pre-burning of raw material, can obtain intermediate product, preferably pre-burning 8～15h at the temperature of 1100～1250 DEG C; Step B) in, the oxide compound of described lead is PbO, Pb
3o
4or they the two mixture.
Step B) can further include: by steps A) material after pre-burning mixes with the plumbous oxide compound taking by stoichiometric ratio, then at 700～1000 DEG C, pre-burning 1～8h obtains crystal growth with expecting, for example can be at 700～800 DEG C pre-burning 2～5h, or pre-burning 1～3h obtains crystal growth with expecting at 800～1000 DEG C.Step B) in because lead has volatility, so the temperature of pre-burning is lower than steps A) calcined temperature.Step B) by pre-burning, be more conducive to the growth of crystal.
Step C) in seed crystal can be the seed crystal that is oriented to (111), (001), (110) or (211) of selecting.Step C) in seed crystal be Pb (Mg
1/3nb
2/3) O
3-PbTiO
3or xPb (Mg
1/3nb
2/3) O
3-yBiAlO
3-(1-x-y) PbTiO
3crystal.
Step C) in the material of crucible be platinum or iraurite; In the time selecting Iridium Crucible, those of ordinary skill in the art should know under reducing atmosphere or inert atmosphere protection and carry out, as argon hydrogen gas mixture or argon gas etc.Crucible is to insert in decline stove after sealing.
Step C) in preferably at 800～1200 DEG C of temperature, be incubated 8～12h, then continue rising temperature to 1350～1400 DEG C, insulation 4～12h, crucible with 0.3～0.8mm/h speed decline, the thermograde of growth interface is 20～80 DEG C/cm;
Step D) in preferably, speed of cooling is 30～80 DEG C/h.
Utilize the monocrystalline of method growth of the present invention to be of a size of 1～6 inch, preferably 2～4 inches; Monocrystalline be shaped as right cylinder, rectangular parallelepiped or other arbitrary shape.
Positive progressive effect of the present invention is: the present invention is at Pb (Mg
1/3nb
2/3) O
3-PbTiO
3basis on introduced a certain amount of BiAlO
3, reduced usage quantity plumbous in crystal, thereby reduced the environmental pollution causing due to plumbous existence in crystal preparation with in using.And the crystal the present invention relates to has superior piezoelectricity, electromechanical coupling performance and less dielectric loss, if tripartite's phase crystal (001) direction of being grown is through its piezoelectric constant of test d
33>1800pC/N, electromechanical coupling factor k
33>0.90, losstangenttanδ ﹤ 0.5, thus make it have huge and application prospect widely at aspects such as ultrasonic transducer, driving mechanism and senser elements.In addition, it is few that the crystal of growing by the present invention has lattice defect, and yield rate is high, and size, shape and the orientation of the crystal of growth are easily controlled, thereby temperature gradient of solid-liquid interface can very littlely prevent the advantages such as crystal cleavage.In addition, this method processing unit is simple, easy to operate, and energy consumption is low, is conducive to realize suitability for industrialized production.
Brief description of the drawings
Fig. 1 is the 0.50Pb (Mg that embodiment 1 obtains
1/3nb
2/3) O
3-0.17BiAlO
3-0.33PbTiO
3the XRD figure spectrum of crystal.
Embodiment
Embodiment 10.50Pb (Mg
1/3nb
2/3) O
3-0.17BiAlO
3-0.33PbTiO
3the preparation of monocrystalline
By high pure raw material MgO, Nb
2o
5, TiO
2, Bi
2o
3and Al
2o
3press 0.50Pb (Mg
1/3nb
2/3) O
3-0.17BiAlO
3-0.33PbTiO
3after molecular formula batching mixes, at the temperature of 1100 DEG C, be incubated 10h, then mix all and carry out briquetting by isostatic cool pressing afterwards with the PbO taking by stoichiometric ratio, be placed in cylindrical platinum crucible together with the seed crystal that is oriented to (111) of selecting, sealed crucible is placed in crucible decline stove and carries out crystal growth, first furnace temperature is risen to 1000 DEG C of insulation 3h, and then continue to be warming up to 1350 DEG C of insulation 5h fusing that made to expect, and adjust bushing position and make seed crystal top fusing, growth interface thermograde is 50 DEG C/cm, with the speed decline crucible of 0.4mm/h, after crystal has all been grown, with the speed cool to room temperature of 60 DEG C/h, just obtain columniform complete 0.50Pb (Mg
1/3nb
2/3) O
3-0.17BiAlO
3-0.33PbTiO
3monocrystalline, its XRD figure is composed as shown in Figure 1.
Embodiment 20.67Pb (Mg
1/3nb
2/3) O
3-0.10BiAlO
3-0.23PbTiO
3the preparation of monocrystalline
By high pure raw material MgO, Nb
2o
5, TiO
2, Bi
2o
3and Al
2o
3press 0.67Pb (Mg
1/
3nb
2/
3) O
3-0.10BiAlO
3-0.23PbTiO
3after molecular formula batching mixes, at the temperature of 1200 DEG C, be incubated 12h, then with the Pb taking by stoichiometric ratio
3o
4after mixing all, at the temperature of 800 DEG C, be incubated 4h again, then carry out briquetting by isostatic cool pressing, be placed in rectangular parallelepiped platinum crucible together with the seed crystal that is oriented to (001) of selecting, sealed crucible is placed in crucible decline stove and carries out crystal growth, first at the temperature of 1100 DEG C, be incubated 2h, and then continue to be warming up to 1360 DEG C of insulation 8h fusing that made to expect, and adjust bushing position and make seed crystal top fusing, growth interface thermograde is 80 DEG C/cm, with the speed decline crucible of 0.6mm/h, after crystal has all been grown, with the speed cool to room temperature of 40 DEG C/h, just obtain the complete 0.67Pb (Mg that is shaped as rectangular parallelepiped
1/3nb
2/3) O
3-0.10BiAlO
3-0.23PbTiO
3monocrystalline.
Embodiment 30.56Pb (Mg1/3Nb2/3) O3-0.08BiAlO
3-0.36PbTiO
3the preparation of monocrystalline
By high pure raw material MgO, Nb
2o
5, TiO
2, Bi
2o
3and Al
2o
3press 0.56Pb (Mg1/3Nb2/3) O
3-0.08BiAlO
3-0.36PbTiO
3after molecular formula batching mixes, at the temperature of 1100 DEG C, be incubated 6h, then with the mol ratio taking by stoichiometric ratio be 1:1 PbO and Pb
3o
4mix and all carry out briquetting by isostatic cool pressing afterwards, be placed in cylindrical Iridium Crucible together with the seed crystal that is oriented to (100) of selecting, sealed crucible is placed in crucible decline stove and carries out crystal growth, in stove, passing into argon hydrogen gas mixture protects, first furnace temperature is risen to 1200 DEG C of insulation 3h, and then continue to be warming up to 1400 DEG C of insulation 3h and melted and expect, and adjust bushing position and make seed crystal top fusing, growth interface thermograde is 80 DEG C/cm, with the speed decline crucible of 0.3mm/h, after crystal has all been grown, with the speed cool to room temperature of 80 DEG C/h, just obtain columniform complete 0.56Pb (Mg1/3Nb2/3) O
3-0.08BiAlO
3-0.36PbTiO
3monocrystalline.
Embodiment 40.32Pb (Mg1/3Nb2/3) O
3-0.40BiAlO
3-0.28PbTiO
3the preparation of monocrystalline
By high pure raw material MgO, Nb
2o
5, TiO
2, Bi
2o
3and Al
2o
3press 0.32Pb (Mg1/3Nb2/3) O
3-0.40BiAlO
3-0.28PbTiO
3after molecular formula batching mixes, at the temperature of 1180 DEG C, be incubated 4h, then with the mol ratio taking by stoichiometric ratio be 2:1 PbO and Pb
3o
4after mixing all, at the temperature of 900 DEG C, be incubated 2h again, then carry out briquetting by isostatic cool pressing, be placed in circular platinum crucible together with the seed crystal that is oriented to (211) of selecting, sealed crucible is placed in crucible decline stove and carries out crystal growth, first furnace temperature is risen to 800 DEG C of insulation 12h, and then continue to be warming up to 1300 DEG C of insulation 10h and melted and expect, and adjust bushing position and make seed crystal top fusing, growth interface thermograde is 60 DEG C/cm, with the speed decline crucible of 0.7mm/h, after crystal has all been grown, with the speed cool to room temperature of 70 DEG C/h, just obtain columniform complete 0.32Pb (Mg1/3Nb2/3) O
3-0.40BiAlO
3-0.28PbTiO
3monocrystalline.
Effect embodiment
By the 0.50Pb (Mg of embodiment 1 gained
1/
3nb
2/
3) O
3-0.17BiAlO
3-0.33PbTiO
3monocrystalline is tested its piezoelectric property, electromechanical coupling factor, loss angle and phase transition temperature according to ordinary method.
Result shows, the 0.50Pb (Mg that embodiment 1 grows
1/
3nb
2/
3) O
3-0.17BiAlO
3-0.33PbTiO
3the piezoelectric constant d of monocrystalline tripartite phase crystal (001) direction
33>1800
pc/N, electromechanical coupling factor k
33>0.90, losstangenttanδ ﹤ 0.5.
Claims (10)
1. a three component system relaxation type monocrystalline piezoelectric material, the chemical formula that it is characterized in that described monocrystalline piezoelectric material is xPb (Mg
1/3nb
2/3) O
3-yBiAlO
3-(1-x-y) PbTiO
3, wherein 0 ﹤ x ﹤ 1,0 ﹤ y ﹤ 1 and x+y ﹤ 1.
2. three component system relaxation type monocrystalline piezoelectric material according to claim 1, is characterized in that 0.2≤x≤0.7,0 ﹤ y≤0.4, preferably 0.5≤x≤0.6,0.05≤y≤0.2.
3. a method for growth three component system relaxation type monocrystalline piezoelectric material claimed in claim 1, is characterized in that, described method is falling crucible method, specifically comprises the steps:
Steps A) press xPb (Mg
1/3nb
2/3) O
3-yBiAlO
3-(1-x-y) PbTiO
3stoichiometric ratio take Bi
2o
3, MgO, Nb
2o
5, TiO
2and Al
2o
3, mix then pre-burning 2～15h at the temperature of 900～1250 DEG C, wherein 0 ﹤ x ﹤ 1,0 ﹤ y ﹤ 1 and x+y ﹤ 1;
Step B) by steps A) material after pre-burning mix with the plumbous oxide compound taking by stoichiometric ratio crystal growth with expecting;
Step C) crystal growth has been used to expect be pressed into block and pack in the crucible that is placed with seed crystal, crucible is inserted in decline stove, at 500～1250 DEG C of temperature, be incubated 3～20h, continue rising temperature to 1340～1410 DEG C, insulation 3～20h, makes crystal growth with working the fusing of expecting, and the top of seed crystal is melted, then crucible declines with 0.1～1.2mm/h speed, and crystalline growth becomes crystal gradually, and the thermograde of growth interface is 20～100 DEG C/cm;
Step D) treat that crystal growth is complete, with the speed cool to room temperature of 10～300 DEG C/h, obtain three component system relaxation type monocrystalline piezoelectric material.
4. method according to claim 3, is characterized in that, steps A) in, pre-burning 8～15h at the temperature of 1100～1250 DEG C; Step B) in, the oxide compound of described lead is PbO, Pb
3o
4or they the two mixture.
5. method according to claim 3, it is characterized in that step B) also further comprise: by steps A) material after pre-burning mixes with the plumbous oxide compound taking by stoichiometric ratio, then at 700～1000 DEG C, pre-burning 1～8h obtains crystal growth with expecting.
6. method according to claim 5, it is characterized in that, by steps A) material after pre-burning mixes with the plumbous oxide compound taking by stoichiometric ratio, then pre-burning 2～5h at 700～800 DEG C, or at 800～1000 DEG C, pre-burning 1～3h obtains crystal growth with expecting.
7. method according to claim 3, is characterized in that step C) in seed crystal be the seed crystal that is oriented to (111), (001), (110) or (211) of selecting.
8. method according to claim 3, is characterized in that step C) in seed crystal be Pb (Mg
1/3nb
2/3) O
3-PbTiO
3or xPb (Mg
1/3nb
2/3) O
3-yBiAlO
3-(1-x-y) PbTiO
3crystal.
9. method according to claim 3, is characterized in that step C) in the material of crucible be platinum or iraurite; Crucible is inserted in decline stove after sealing.
10. method according to claim 3, it is characterized in that step C) at 800～1200 DEG C of temperature, be incubated after 8～12h, continue rising temperature to 1350～1400 DEG C, insulation 4～12h, crucible declines with 0.3～0.8mm/h speed, and the thermograde of growth interface is 20～80 DEG C/cm; Step D) in speed of cooling be 30～80 DEG C/h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115094519A (en) * | 2022-07-18 | 2022-09-23 | 中材人工晶体研究院有限公司 | Preparation method of raw material for growth of relaxor ferroelectric single crystal |
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 |
-
2013
- 2013-05-14 CN CN201310178564.XA patent/CN104153000B/en active Active
Patent Citations (2)
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| 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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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115094519A (en) * | 2022-07-18 | 2022-09-23 | 中材人工晶体研究院有限公司 | Preparation method of raw material for growth of relaxor ferroelectric single crystal |
| CN115094519B (en) * | 2022-07-18 | 2024-03-26 | 中材人工晶体研究院有限公司 | Preparation method of raw material for growth of relaxor ferroelectric single crystal |
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