CN102817068A - Preparation method of sodium bismuth titanate-lead titanate piezoelectric monocrystal - Google Patents
Preparation method of sodium bismuth titanate-lead titanate piezoelectric monocrystal Download PDFInfo
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- CN102817068A CN102817068A CN2012103246964A CN201210324696A CN102817068A CN 102817068 A CN102817068 A CN 102817068A CN 2012103246964 A CN2012103246964 A CN 2012103246964A CN 201210324696 A CN201210324696 A CN 201210324696A CN 102817068 A CN102817068 A CN 102817068A
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Abstract
The invention discloses a preparation method of a sodium bismuth titanate-lead titanate piezoelectric monocrystal, which uses a crucible descent method. The method comprises the following steps: preparing a monocrystal growth initial material, carrying out monocrystal growth and growth completion by a crucible descent method, cooling to room temperature and the like. The invention adopts the crucible descent method for the first time to prepare the sodium bismuth titanate-lead titanate piezoelectric monocrystal (NBT-PT) with high Curie temperature and depolarization temperature; the size of the prepared NBT-PT monocrystal is up to phi 20mm*70mm; the prepared NBT-PT monocrystal has excellent piezoelectric properties and favorable electric field stability; the Curie temperature is up to 300 DEG C, the depolarization temperature is up to 176 DEG C, the piezoelectric constant d33 is up to 280pC/N, and the electromechanical coupling factor kt is up to 52%; the NBT-PT monocrystal has wide application temperature range; and the lead content is very low, and thus, the NBT-PT monocrystal satisfies the national and international environmental protection requirements, thereby having very wide application prospects.
Description
Technical field
The present invention relates to a kind of preparation method of relaxor ferroelectric monocrystal, specifically, relate to a kind of bismuth-sodium titanate-lead titanate piezoelectric monocrystal [(1-x) Na
0.5Bi
0.5TiO
3-x PbTiO
3, be abbreviated as NBT-PT] the preparation method, belong to the single crystal growing technical field.
Background technology
With PMNT, PZNT is that the lead base composite perofskite type structural relaxation ferro-electricity single crystal of representative gets most of the attention its d with its excellent piezoelectric property
33And k
33Can reach more than 2500pC/N and 92% respectively; The maximum strain amount is up to more than 1.7%; Have a wide range of applications at ultrasonic transducer, piezoelectric transformer, wave filter and ultrasonic motor etc., occupy quite great proportion in field of electronic materials as one type of important functional material.But although these materials have very excellent electric property, Tc that it is lower and three parts-cubic transformation temperature has limited its temperature use range.And in the lead base material, plumbous content has surpassed 60%, and environment and ecology have been brought serious harm.Therefore, improve the Tc and the three parts-cubic transformation temperature of piezoelectric, researching and developing unleaded or lacking plumbous relaxor ferroelectric monocrystal material becomes the hot subject that countries in the world are concerned about.
Bismuth-sodium titanate Na
0.5Bi
0.5TiO
3(being abbreviated as NBT) is that room temperature is a trigonal crystal structure perovskite typed ferroelectrics, has strong (the remnant polarization P of ferroelectricity
rReach 38 μ C/cm
2), characteristic such as specific inductivity is little and acoustical behavior is good, be applicable to fields such as high-frequency transducer, industrial flaw detection and medical supersonic engineering.But its higher coercive electric field, lower depolarize temperature have restricted its application.The appearance of bismuth sodium titanate-barium titanate (NBT-BT) system solid solution has effectively improved its piezoelectric property, and especially near accurate homotype phase boundary (MPB), but its leakage current is bigger, and polarization process is difficulty still.And recent research shows, Tc and depolarize temperature that a kind of novel bismuth-sodium titanate-lead titanate (NBT-PT) system has near accurate homotype phase boundary x=0.11 reach 340 ℃ and 200 ℃ respectively, than NBT-BT system up to about 80 ℃.Yet, do not see the correlation technique report that adopts falling crucible method to prepare large size NBT-PT monocrystalline up to now.
Summary of the invention
The problems referred to above to prior art exists the purpose of this invention is to provide a kind of method that adopts falling crucible method to prepare large size bismuth-sodium titanate-lead titanate piezoelectric monocrystal.
For realizing the foregoing invention purpose, the technical scheme that the present invention adopts is following:
The preparation method of a kind of bismuth-sodium titanate-lead titanate piezoelectric monocrystal is falling crucible method, comprises following concrete steps:
A) according to general formula (1-x) Na
0.5Bi
0.5TiO
3-xPbTiO
3, wherein 0<x<1, accurately take by weighing each raw material of yellow soda ash, bismuth oxide, titanium oxide and plumbous oxide of stoichiometric ratio, the preparation single crystal growing rises expects;
B) single crystal growing that makes is risen to expect pack in the crucible; Add seed crystal, adopt falling crucible method to carry out single crystal growing: control single crystal growing furnace temperature is 1380～1500 ℃, and the melt soaking time is 3～10 hours; Furnace temperature temperature rise rate in the crystal growing process is 0～3 ℃/day; The crucible fall off rate is 0.2～1mm/h, and the thermograde of solid-liquid interface is 5～10 ℃/mm, and the maximum temperature gradient of crucible descending direction is 1～7 ℃/mm;
C) growth ending is cooled to room temperature.
As a kind of preferred version, it is following that the preparation single crystal growing works the operation of expecting:
According to general formula (1-x) Na
0.5Bi
0.5TiO
3-xPbTiO
3, wherein 0<x<1, accurately take by weighing each raw material of yellow soda ash, bismuth oxide, titanium oxide and plumbous oxide of stoichiometric ratio, ball milling makes abundant mixing, after isostatic cool pressing becomes piece or do not wait static pressure to become piece, rises as single crystal growing then and expects.
As another kind of preferred version, it is following that the preparation single crystal growing works the operation of expecting:
According to general formula (1-x) Na
0.5Bi
0.5TiO
3-xPbTiO
3, wherein 0<x<1; Accurately take by weighing each raw material of yellow soda ash, bismuth oxide, titanium oxide and plumbous oxide of stoichiometric ratio; Ball milling makes abundant mixing, under 1000 ± 100 ℃, carries out 4～6 hours solid state reaction then, sinters the compound of NBT-PT into; Fine grinding again rises as single crystal growing after isostatic cool pressing becomes piece or do not wait static pressure to become piece and expects.
As another kind of preferred version, it is following that the preparation single crystal growing works the operation of expecting:
1) according to chemical formula Na
0.5Bi
0.5TiO
3Accurately take by weighing the yellow soda ash and the bismuth oxide of stoichiometric ratio, ball milling makes and mixes, and under 1000 ± 100 ℃, carries out 4～6 hours solid state reaction then, sinters the polycrystal of NBT into;
2) according to chemical formula PbTiO
3(being abbreviated as PT) accurately takes by weighing the titanium oxide and the plumbous oxide of stoichiometric ratio, and ball milling makes and mixes, and then 1000 ± 100 ℃ of solid state reactions of carrying out 4～6 hours, sinters the polycrystal of PT into;
3) according to general formula (1-x) Na
0.5Bi
0.5TiO
3-xPbTiO
3, wherein 0<x<1, accurately take by weighing the NBT and the PT polycrystal of stoichiometric ratio, ball milling makes and mixes; Then 1000 ± 100 ℃ of solid state reactions of carrying out 4～6 hours; Sinter the compound of NBT-PT into, fine grinding again rises as single crystal growing after isostatic cool pressing becomes piece or do not wait static pressure to become piece and expects.
As further preferred version, each material purity of described yellow soda ash, bismuth oxide, titanium oxide and plumbous oxide is all greater than 99.99%.
As further preferred version, said crucible is a platinum crucible.
As preferred version further, said crucible is individual layer or the bilayer or the three-decker of sealing, and every layer thickness is 0.10～0.20mm.
As further preferred version, said seed crystal is similar PMN-PT (PMN-PT) monocrystalline of NBT-PT monocrystalline or crystalline network, seed crystal be oriented to < 111 >, < 110>or < 100 >.
As preferred version further, said seed crystal is the NBT-PT monocrystalline of < 110>orientation.
As further preferred version, said seed size is Ф (19～20) mm * 50mm.
As further preferred version, when crucible decline 5cm, stop growing, the rate of temperature fall with 50～200 ℃/h is cooled to room temperature then.
As further preferred version, said general formula (1-x) Na
0.5Bi
0.5TiO
3-xPbTiO
3In 0.01≤x≤0.14, best with x=0.09.
Compared with prior art; Bismuth-sodium titanate-lead titanate piezoelectric monocrystal (NBT-PT) that the present invention adopts falling crucible method to make to have high-curie temperature and depolarize temperature first; Not only can make prepared NBT-PT monocrystalline size reach Ф 20mm * 70mm, and make prepared NBT-PT monocrystalline show excellent piezoelectric property and good electric field stability, Tc can reach 300 ℃; The umpolarization temperature can reach 176 ℃, piezoelectric constant d
33Can reach 280pC/N, electromechanical coupling factor k
tCan reach 52%, have wide use temperature scope; And lead tolerance is extremely low, meets China and international environmental protection demand, so its application prospect is very wide.
Description of drawings
Fig. 1 is the XRD figure spectrum of bismuth-sodium titanate-lead titanate piezoelectric monocrystal of making of embodiment 1;
Fig. 2 is the specific inductivity (ε of bismuth-sodium titanate-lead titanate piezoelectric monocrystal of making of embodiment 1
r), dielectric loss (tan δ) and temperature (℃) between function relation curve figure;
Fig. 3 is the ferroelectric hysteresis loop figure and the two-way strain loop line figure of bismuth-sodium titanate-lead titanate piezoelectric monocrystal of making of embodiment 1;
Fig. 4 be bismuth-sodium titanate-lead titanate piezoelectric monocrystal thickness vibration mode of making of embodiment 1 impedance (Ω), phase angle (°) and frequency (Hz) between function relation curve figure.
Embodiment
Below in conjunction with accompanying drawing and embodiment to the present invention do further in detail, intactly explanation.
Piezoelectric coefficient d involved in the present invention
33Be the ZJ-3A type d that makes with Acoustical Inst., Chinese Academy of Sciences
33Tester is directly measured and is obtained; Specific inductivity is to obtain with converting behind the HP4192A type electric impedance analyzer measure sample electric capacity; Electromechanical coupling factor k
tMeasurement be according to the IEEE176-78 standard, measure the impedance under the different frequency with HP4294A type electric impedance analyzer after, according to formula
Calculate, wherein Δ f=f
p-f
sIt is to measure with Aixacct TF-1000 type ferroelectric analytical system to obtain that ferroelectric hysteresis loop causes the strain loop line with the field.
Embodiment 1
According to general formula 0.91Na
0.5Bi
0.5TiO
3-0.09PbTiO
3The purity that accurately takes by weighing stoichiometric ratio is each powder raw material of yellow soda ash, bismuth oxide, titanium oxide and plumbous oxide greater than 99.99%, after thorough drying all, and ball milling made and mixes in 24 hours; Insert then in the platinum crucible of adding a cover, 1000 ℃ of sintering 6 hours; With sintered product through pulverizing, fine grinding, sieve, after isostatic cool pressing becomes piece, rise and expect as single crystal growing;
The platinum crucible of Ф 20mm * 200mm of selecting individual layer for use is as growth crucible, with the NBT-PT monocrystalline of < 110>orientation of being of a size of Ф 19.5mm * 50mm as seed crystal; Pack into seed crystal and single crystal growing rise expect the back sealed crucible; Insert then that (the present invention does not have strict restriction to growth apparatus in the reactors; All can be used for the present invention as long as have the reactors device of temperature ladder, a plurality of patents of this respect Shanghai silicate institute disclose, for example CN1113970A); Adopt falling crucible method to carry out single crystal growing: control single crystal growing furnace temperature is 1390 ℃; The melt soaking time is 6 hours; Furnace temperature temperature rise rate in the crystal growing process is 2 ℃/day; The crucible fall off rate is 0.3mm/h, and the thermograde of solid-liquid interface is 7 ℃/mm, and the maximum temperature gradient of crucible descending direction is 7 ℃/mm;
When crucible decline 5cm, stop growing; Be cooled to room temperature with 50 ℃/hour rate of temperature fall then; Can obtain and seed crystal direction unanimity and the shape complete NBT-PT monocrystalline identical with crucible, the gained monocrystalline is removed the seed crystal part, and the crystal ingot portion size is Ф 20mm * 70mm.
Fig. 1 is the XRD figure spectrum of bismuth-sodium titanate-lead titanate piezoelectric monocrystal of making of present embodiment, and can be known by Fig. 1: said NBT-PT monocrystalline at room temperature presents pure tripartite uhligite phase structure.
Fig. 2 is the specific inductivity (ε of bismuth-sodium titanate-lead titanate piezoelectric monocrystal of making of present embodiment
r), dielectric loss (tan δ) and temperature (℃) between function relation curve figure, can be known by Fig. 2: the depolarize temperature of said NBT-PT monocrystalline can reach 176 ℃, Tc can reach 300 ℃.
Fig. 3 is the ferroelectric hysteresis loop figure and the two-way strain loop line figure of bismuth-sodium titanate-lead titanate piezoelectric monocrystal of making of present embodiment, and can be known by Fig. 3: the coercive electric field of said NBT-PT monocrystalline can reach 43kV/cm, and remnant polarization can reach 23 μ C/cm
2, maximum strain reaches 0.17%, and piezoelectric constant can reach 280pC/N;
Fig. 4 be bismuth-sodium titanate-lead titanate piezoelectric monocrystal thickness vibration mode of making of present embodiment impedance (Ω), phase angle (°) and frequency (Hz) between function relation curve figure, calculate by Fig. 4 and according to ieee standard and to learn that the thickness mode electromechanical coupling factor of said NBT-PT monocrystalline reaches 52%.
Embodiment 2
The difference of present embodiment and embodiment 1 only is:
It is following that the preparation single crystal growing works the operation of expecting: according to general formula 0.99Na
0.5Bi
0.5TiO
3-0.01PbTiO
3The purity that accurately takes by weighing stoichiometric ratio is each powder raw material of yellow soda ash, bismuth oxide, titanium oxide and plumbous oxide greater than 99.99%, after thorough drying all, and ball milling made and mixes in 24 hours; After isostatic cool pressing becomes piece or do not wait static pressure to become piece, rise then and expect as single crystal growing.
All the other contents are all with identical described in the embodiment 1.
Experimental result shows: present embodiment also can grow the crystal ingot size and reach Ф 20mm * 70mm, Tc about 300 ℃, the umpolarization temperature about 176 ℃, piezoelectric constant d
33Reach 280pC/N, electromechanical coupling factor k
t Surpass 50% the few plumbous bismuth-sodium titanate-lead titanate piezoelectric monocrystal of high-curie temperature.
Embodiment 3
The difference of present embodiment and embodiment 1 only is:
It is following that the preparation single crystal growing works the operation of expecting:
1) according to chemical formula Na
0.5Bi
0.5TiO
3The purity that accurately takes by weighing stoichiometric ratio is greater than 99.99% yellow soda ash and bismuth oxide, and ball milling made and mixes in 24 hours, under 1100 ℃, carried out 4 hours solid state reaction then, sintered the polycrystal of NBT into;
2) according to chemical formula PbTiO
3The purity that accurately takes by weighing stoichiometric ratio is greater than 99.99% titanium oxide and plumbous oxide, and ball milling made and mixes in 24 hours, then 1100 ℃ of solid state reactions of carrying out 4 hours, sintered the polycrystal of PT into;
3) according to general formula 0.86Na
0.5Bi
0.5TiO
3-0.14PbTiO
3Accurately take by weighing the NBT and the PT polycrystal of stoichiometric ratio; Ball milling made and mixes in 24 hours, then 1100 ℃ of solid state reactions of carrying out 6 hours, sintered the compound of NBT-PT into; Fine grinding again rises as single crystal growing after isostatic cool pressing becomes piece or do not wait static pressure to become piece and expects.
All the other contents are all with identical described in the embodiment 1.
Experimental result shows: present embodiment also can grow the crystal ingot size and reach Ф 20mm * 70mm, Tc about 300 ℃, the umpolarization temperature about 176 ℃, piezoelectric constant d
33Reach 280pC/N, electromechanical coupling factor k
t Surpass 50% the few plumbous bismuth-sodium titanate-lead titanate piezoelectric monocrystal of high-curie temperature.
Be necessary at last in this explanation to be: above embodiment only is used for technical scheme of the present invention is done explanation in further detail; Can not be interpreted as the restriction to protection domain of the present invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.
Claims (10)
1. the preparation method of bismuth-sodium titanate-lead titanate piezoelectric monocrystal is characterized in that, is falling crucible method, comprises following concrete steps:
A) according to general formula (1-x) Na
0.5Bi
0.5TiO
3-xPbTiO
3, wherein 0<x<1, accurately take by weighing each raw material of yellow soda ash, bismuth oxide, titanium oxide and plumbous oxide of stoichiometric ratio, the preparation single crystal growing rises expects;
B) single crystal growing that makes is risen to expect pack in the crucible; Add seed crystal, adopt falling crucible method to carry out single crystal growing: control single crystal growing furnace temperature is 1380～1500 ℃, and the melt soaking time is 3～10 hours; Furnace temperature temperature rise rate in the crystal growing process is 0～3 ℃/day; The crucible fall off rate is 0.2～1mm/h, and the thermograde of solid-liquid interface is 5～10 ℃/mm, and the maximum temperature gradient of crucible descending direction is 1～7 ℃/mm;
C) growth ending is cooled to room temperature.
2. the preparation method of bismuth-sodium titanate according to claim 1-lead titanate piezoelectric monocrystal is characterized in that, it is following that the preparation single crystal growing works the operation of expecting: according to general formula (1-x) Na
0.5Bi
0.5TiO
3-xPbTiO
3, wherein 0<x<1, accurately take by weighing each raw material of yellow soda ash, bismuth oxide, titanium oxide and plumbous oxide of stoichiometric ratio, ball milling makes abundant mixing, after isostatic cool pressing becomes piece or do not wait static pressure to become piece, rises as single crystal growing then and expects.
3. the preparation method of bismuth-sodium titanate according to claim 1-lead titanate piezoelectric monocrystal is characterized in that, it is following that the preparation single crystal growing works the operation of expecting: according to general formula (1-x) Na
0.5Bi
0.5TiO
3-xPbTiO
3, wherein 0<x<1; Accurately take by weighing each raw material of yellow soda ash, bismuth oxide, titanium oxide and plumbous oxide of stoichiometric ratio; Ball milling makes abundant mixing, under 1000 ± 100 ℃, carries out 4～6 hours solid state reaction then, sinters the compound of NBT-PT into; Fine grinding again rises as single crystal growing after isostatic cool pressing becomes piece or do not wait static pressure to become piece and expects.
4. the preparation method of bismuth-sodium titanate according to claim 1-lead titanate piezoelectric monocrystal is characterized in that, it is following that the preparation single crystal growing works the operation of expecting:
1) according to chemical formula Na
0.5Bi
0.5TiO
3Accurately take by weighing the yellow soda ash and the bismuth oxide of stoichiometric ratio, ball milling makes and mixes, and under 1000 ± 100 ℃, carries out 4～6 hours solid state reaction then, sinters the polycrystal of NBT into;
2) according to chemical formula PbTiO
3Accurately take by weighing the titanium oxide and the plumbous oxide of stoichiometric ratio, ball milling makes and mixes, and then 1000 ± 100 ℃ of solid state reactions of carrying out 4～6 hours, sinters the polycrystal of PT into;
3) according to general formula (1-x) Na
0.5Bi
0.5TiO
3-xPbTiO
3, wherein 0<x<1, accurately take by weighing the NBT and the PT polycrystal of stoichiometric ratio, ball milling makes and mixes; Then 1000 ± 100 ℃ of solid state reactions of carrying out 4～6 hours; Sinter the compound of NBT-PT into, fine grinding again rises as single crystal growing after isostatic cool pressing becomes piece or do not wait static pressure to become piece and expects.
5. the preparation method of bismuth-sodium titanate according to claim 1-lead titanate piezoelectric monocrystal is characterized in that: said crucible is a platinum crucible.
6. the preparation method of bismuth-sodium titanate according to claim 5-lead titanate piezoelectric monocrystal is characterized in that: said crucible adopts individual layer or the bilayer or the three-decker of sealing, and every layer thickness is 0.10～0.20mm.
7. the preparation method of bismuth-sodium titanate according to claim 1-lead titanate piezoelectric monocrystal is characterized in that: said seed crystal is NBT-PT monocrystalline or the similar niobic magnesium acid lead-lead titanate single-crystal of crystalline network, seed crystal be oriented to < 111 >, < 110>or < 100 >.
8. the preparation method of bismuth-sodium titanate according to claim 1-lead titanate piezoelectric monocrystal is characterized in that: said seed size is Ф (19～20) mm * 50mm.
9. the preparation method of bismuth-sodium titanate according to claim 1-lead titanate piezoelectric monocrystal is characterized in that: when crucible decline 5cm, stop growing, reduce to room temperature with the rate of temperature fall of 50～200 ℃/h then.
10. the preparation method of bismuth-sodium titanate according to claim 1-lead titanate piezoelectric monocrystal is characterized in that: said general formula (1-x) Na
0.5Bi
0.5TiO
3-xPbTiO
3In 0.01≤x≤0.14.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105624791A (en) * | 2014-10-28 | 2016-06-01 | 中国科学院上海硅酸盐研究所 | Preparation method of tetragonal phase bismuth magnesium titanate-lead titanate base piezoelectric monocrystals |
| CN113113582A (en) * | 2021-03-19 | 2021-07-13 | 上海利物盛纳米科技有限公司 | Preparation method of graphene-titanate lead-acid battery electrode active substance additive with layered structure |
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| WO2001077501A2 (en) * | 2000-04-11 | 2001-10-18 | Massachusetts Institute Of Technology | Electromechanical actuators |
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| WO2001077501A2 (en) * | 2000-04-11 | 2001-10-18 | Massachusetts Institute Of Technology | Electromechanical actuators |
Non-Patent Citations (2)
| Title |
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| GUISHENG XU, ET AL.: "Growth and some electrical properties of lead-free piezoelectric crystals (Na1/2Bi1/2)TiO3 and (Na1/2Bi1/2)TiO3-BaTiO3 prepared by a Bridgman method", 《JOURNAL OF CRYSTAL GROWTH》, vol. 275, 1 January 2005 (2005-01-01), pages 114 - 115 * |
| SARAB PREET SINGH ET AL.: "Structural phase transition study of the morphotropic phase boundary compositions of Na0.5Bi0.5TiO3–PbTiO3", 《JOURNAL OF PHYSICS: CONDENSED MATTER》, vol. 21, 17 August 2009 (2009-08-17), XP020164442, DOI: doi:10.1088/0953-8984/21/37/375902 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105624791A (en) * | 2014-10-28 | 2016-06-01 | 中国科学院上海硅酸盐研究所 | Preparation method of tetragonal phase bismuth magnesium titanate-lead titanate base piezoelectric monocrystals |
| CN105624791B (en) * | 2014-10-28 | 2018-05-08 | 中国科学院上海硅酸盐研究所 | A kind of preparation method of Tetragonal titanium magnesium acid bismuth-lead titanate piezoelectric monocrystal |
| CN113113582A (en) * | 2021-03-19 | 2021-07-13 | 上海利物盛纳米科技有限公司 | Preparation method of graphene-titanate lead-acid battery electrode active substance additive with layered structure |
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