CN102817068B - A kind of preparation method of sodium bismuth titanate-lead titanate piezoelectric monocrystal - Google Patents
A kind of preparation method of sodium bismuth titanate-lead titanate piezoelectric monocrystal Download PDFInfo
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- CN102817068B CN102817068B CN201210324696.4A CN201210324696A CN102817068B CN 102817068 B CN102817068 B CN 102817068B CN 201210324696 A CN201210324696 A CN 201210324696A CN 102817068 B CN102817068 B CN 102817068B
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Abstract
The invention discloses a kind of preparation method of sodium bismuth titanate-lead titanate piezoelectric monocrystal, described method is falling crucible method, comprise preparation single crystal growing rise expect, adopts falling crucible method carry out single crystal growing and growth end, be cooled to the steps such as room temperature.The sodium bismuth titanate-lead titanate piezoelectric monocrystal (NBT-PT) that the present invention adopts falling crucible method to obtain to have high-curie temperature and depolarize temperature first, obtained NBT-PT monocrystalline size not only can be made to reach Ф 20mm × 70mm, and make obtained NBT-PT monocrystalline show excellent piezoelectric property and good electric field stability, Curie temperature can reach 300 DEG C, umpolarization temperature can reach 176 DEG C, piezoelectric constant d
33280pC/N can be reached, electromechanical coupling factor k
tcan 52% be reached, there is wide use temperature scope; And lead tolerance is extremely low, meet China and International Environmental Protection demand, therefore its application prospect is very wide.
Description
Technical field
The present invention relates to a kind of preparation method of relaxor ferroelectric monocrystal, specifically, relate to a kind of sodium bismuth titanate-lead titanate piezoelectric monocrystal [(1-x) Na
0.5bi
0.5tiO
3-x PbTiO
3, be abbreviated as NBT-PT] preparation method, belong to technical field of single crystal growth.
Background technology
The lead base composite perofskite type structural relaxation ferro-electricity single crystal being representative with PMNT, PZNT gets most of the attention with the piezoelectric property of its excellence, its d
33and k
332500pC/N and more than 92% can be reached respectively, 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., the functional materials important as a class occupies sizable proportion in field of electronic materials.But although these materials have very excellent electric property, its lower Curie temperature and rhombohedral-tetragonal phase temperature limit its temperature use range.And in plumbum-based material, plumbous content has exceeded 60%, brings serious harm to environment and ecology.Therefore, improve Curie temperature and the rhombohedral-tetragonal phase temperature of piezoelectric, researching and developing unleaded or few plumbous relaxor ferroelectric monocrystal material becomes the hot subject be concerned about countries in the world.
Bismuth-sodium titanate Na
0.5bi
0.5tiO
3(being abbreviated as NBT) is room temperature is trigonal crystal structure Ferroelectrics, has strong (the remnant polarization P of ferroelectricity
rreach 38 μ C/cm
2), the feature such as the little and acoustical behavior of specific inductivity is good, be applicable to the fields such as high-frequency transducer, industrial flaw detection and medical supersonic engineering.But its higher coercive electric field, lower depolarize temperature constrain its application.The appearance of bismuth sodium titanate-barium titanate (NBT-BT) system solid solution effectively raises its piezoelectric property, and especially near accurate homotype phase boundary (MPB), but its leakage current is comparatively large, and polarization process is still more difficult.And recent research shows, a kind of novel bismuth-sodium titanate-lead titanate (NBT-PT) system has Curie temperature near accurate homotype phase boundary x=0.11 and depolarize temperature reaches 340 DEG C and 200 DEG C, respectively than NBT-BT system up to about 80 DEG C.But, have no the correlation technique report adopting falling crucible method to prepare large size NBT-PT monocrystalline up to now.
Summary of the invention
For the problems referred to above that prior art exists, the object of this invention is to provide a kind of method adopting falling crucible method to prepare large size sodium bismuth titanate-lead titanate piezoelectric monocrystal.
For achieving the above object, the technical solution used in the present invention is as follows:
A preparation method for sodium bismuth 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 takes each raw material of the sodium carbonate of stoichiometric ratio, bismuth oxide, titanium dioxide and plumbous oxide, and preparation single crystal growing rises expects;
B) obtained single crystal growing is risen expect and load in crucible, add seed crystal, falling crucible method is adopted to carry out single crystal growing: controlling single crystal growing furnace temperature is 1380 ~ 1500 DEG C, melt soaking time is 3 ~ 10 hours, furnace temperature temperature rise rate in crystal growing process is 0 ~ 3 DEG C/day, crucible fall off rate is 0.2 ~ 1mm/h, and the thermograde of solid-liquid interface is 5 ~ 10 DEG C/mm, and the maximum temperature gradient of crucible descending direction is 1 ~ 7 DEG C/mm;
C) growth terminates, and is cooled to room temperature.
As a kind of preferred version, it is as follows that preparation single crystal growing works the operation of expecting:
According to general formula (1-x) Na
0.5bi
0.5tiO
3-xPbTiO
3wherein 0<x<1, accurately take each raw material of the sodium carbonate of stoichiometric ratio, bismuth oxide, titanium dioxide and plumbous oxide, ball milling makes abundant mixing, then rises as single crystal growing after isostatic cool pressing becomes block or isostatic pressed does not become block and expects.
As another kind of preferred version, it is as follows that preparation single crystal growing works the operation of expecting:
According to general formula (1-x) Na
0.5bi
0.5tiO
3-xPbTiO
3wherein 0<x<1, accurately take each raw material of the sodium carbonate of stoichiometric ratio, bismuth oxide, titanium dioxide and plumbous oxide, ball milling makes abundant mixing, then at 1000 ± 100 DEG C, carry out the solid state reaction of 4 ~ 6 hours, sinter the compound of NBT-PT into, then fine grinding, rise as single crystal growing after isostatic cool pressing becomes block or isostatic pressed does not become block and expect.
As another kind of preferred version, it is as follows that preparation single crystal growing works the operation of expecting:
1) according to chemical formula Na
0.5bi
0.5tiO
3accurately take sodium carbonate and the bismuth oxide of stoichiometric ratio, ball milling makes to mix, and at 1000 ± 100 DEG C, then carries out the solid state reaction of 4 ~ 6 hours, sinter the polycrystal of NBT into;
2) according to chemical formula PbTiO
3(being abbreviated as PT) accurately takes titanium dioxide and the plumbous oxide of stoichiometric ratio, and ball milling makes to mix, and then carries out the solid state reaction of 4 ~ 6 hours at 1000 ± 100 DEG C, sinters the polycrystal of PT into;
3) according to general formula (1-x) Na
0.5bi
0.5tiO
3-xPbTiO
3wherein 0<x<1, accurately take NBT and the PT polycrystal of stoichiometric ratio, ball milling makes to mix, then the solid state reaction of 4 ~ 6 hours is carried out at 1000 ± 100 DEG C, sinter the compound of NBT-PT into, then fine grinding, rise as single crystal growing after isostatic cool pressing becomes block or isostatic pressed does not become block and expect.
As further preferred version, each material purity of described sodium carbonate, bismuth oxide, titanium dioxide and plumbous oxide is all greater than 99.99%.
As further preferred version, described crucible is platinum crucible.
As further preferred version, described crucible is the individual layer of sealing or double-deck or three-decker, and every layer thickness is 0.10 ~ 0.20mm.
As further preferred version, described 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 further preferred version, described seed crystal is the NBT-PT monocrystalline of <110> orientation.
As further preferred version, described seed size is Ф (19 ~ 20) mm × 50mm.
As further preferred version, stop growing as crucible decline 5cm, be then cooled to room temperature with the rate of temperature fall of 50 ~ 200 DEG C/h.
As further preferred version, described 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, the sodium bismuth titanate-lead titanate piezoelectric monocrystal (NBT-PT) that the present invention adopts falling crucible method to obtain to have high-curie temperature and depolarize temperature first, obtained NBT-PT monocrystalline size not only can be made to reach Ф 20mm × 70mm, and make obtained NBT-PT monocrystalline show excellent piezoelectric property and good electric field stability, Curie temperature can reach 300 DEG C, umpolarization temperature can reach 176 DEG C, piezoelectric constant d
33280pC/N can be reached, electromechanical coupling factor k
tcan 52% be reached, there is wide use temperature scope; And lead tolerance is extremely low, meet China and International Environmental Protection demand, therefore its application prospect is very wide.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the sodium bismuth titanate-lead titanate piezoelectric monocrystal that embodiment 1 obtains;
Fig. 2 is the specific inductivity (ε of the sodium bismuth titanate-lead titanate piezoelectric monocrystal that embodiment 1 obtains
r), function relation curve figure between dielectric loss (tan δ) and temperature (DEG C);
Fig. 3 is the ferroelectric hysteresis loop figure of the sodium bismuth titanate-lead titanate piezoelectric monocrystal that embodiment 1 obtains and two-way strain loop line figure;
Fig. 4 is the obtained impedance (Ω) of sodium bismuth titanate-lead titanate piezoelectric monocrystal thickness vibration mode of embodiment 1, the function relation curve figure between phase angle (°) and frequency (Hz).
Embodiment
Do to illustrate in detail, intactly further to the present invention below in conjunction with drawings and Examples.
Piezoelectric coefficient d involved in the present invention
33the ZJ-3A type d manufactured with Acoustical Inst., Chinese Academy of Sciences
33tester directly measures and obtains; Specific inductivity obtains with converting after HP4192A type electric impedance analyzer measure sample electric capacity; Electromechanical coupling factor k
tmeasurement be according to IEEE176-78 standard, measure the impedance under different frequency with HP4294A type electric impedance analyzer after, according to formula
calculate, wherein Δ f=f
p-f
s; Ferroelectric hysteresis loop and field-induced strain loop line measure by Aixacct TF-1000 Ferroelectric analytical system to obtain.
Embodiment 1
According to general formula 0.91Na
0.5bi
0.5tiO
3-0.09PbTiO
3accurately take stoichiometric ratio purity is all greater than 99.99%, through abundant dried sodium carbonate, bismuth oxide, titanium dioxide and each powder raw material of plumbous oxide, ball milling makes to mix for 24 hours; Then insert in the platinum crucible of adding a cover, sinter 6 hours at 1000 DEG C; Using sintered product through pulverizing, fine grinding, sieve, become to rise as single crystal growing after block through isostatic cool pressing and expect;
Select the platinum crucible of the Ф 20mm × 200mm of individual layer as growth crucible, to be of a size of the NBT-PT monocrystalline of the <110> orientation of Ф 19.5mm × 50mm as seed crystal; Sealed crucible after loading seed crystal and single crystal growing rise and expect, then insert in growth furnace that (the present invention does not strictly limit growth apparatus, as long as have temperature ladder growth furnace device all can be used for the present invention, this respect Shanghai silicate institute multiple patents disclose, such as CN1113970A); Falling crucible method is adopted to carry out single crystal growing: controlling single crystal growing furnace temperature is 1390 DEG C, melt soaking time is 6 hours, furnace temperature temperature rise rate in crystal growing process is 2 DEG C/day, crucible fall off rate is 0.3mm/h, the thermograde of solid-liquid interface is 7 DEG C/mm, and the maximum temperature gradient of crucible descending direction is 7 DEG C/mm;
Stop growing as crucible decline 5cm, then room temperature is cooled to the rate of temperature fall of 50 DEG C/h, can obtain consistent with seed crystal direction and that shape is identical with crucible complete NBT-PT monocrystalline, gained monocrystalline removes seed portion, and crystal ingot portion size is Ф 20mm × 70mm.
Fig. 1 is the XRD figure spectrum of the sodium bismuth titanate-lead titanate piezoelectric monocrystal that the present embodiment obtains, as shown in Figure 1: described NBT-PT monocrystalline at room temperature presents pure tripartite's Perovskite Phase structure.
Fig. 2 is the specific inductivity (ε of the sodium bismuth titanate-lead titanate piezoelectric monocrystal that the present embodiment obtains
r), function relation curve figure between dielectric loss (tan δ) and temperature (DEG C), as shown in Figure 2: the depolarize temperature of described NBT-PT monocrystalline can reach 176 DEG C, and Curie temperature can reach 300 DEG C.
Fig. 3 is the ferroelectric hysteresis loop figure of the sodium bismuth titanate-lead titanate piezoelectric monocrystal that the present embodiment obtains and two-way strain loop line figure, and as shown in Figure 3: the coercive electric field of described NBT-PT monocrystalline can reach 43kV/cm, remnant polarization can reach 23 μ C/cm
2, maximum strain reaches 0.17%, and piezoelectric constant can reach 280pC/N;
Fig. 4 is the impedance (Ω) of the sodium bismuth titanate-lead titanate piezoelectric monocrystal thickness vibration mode that the present embodiment obtains, the function relation curve figure between phase angle (°) and frequency (Hz), learns that the thickness mode electromechanical coupling factor of described NBT-PT monocrystalline reaches 52% by Fig. 4 and according to ieee standard calculating.
Embodiment 2
The difference of the present embodiment and embodiment 1 is only:
It is as follows that preparation single crystal growing works the operation of expecting: according to general formula 0.99Na
0.5bi
0.5tiO
3-0.01PbTiO
3accurately take stoichiometric ratio purity is all greater than 99.99%, through abundant dried sodium carbonate, bismuth oxide, titanium dioxide and each powder raw material of plumbous oxide, ball milling makes to mix for 24 hours; Then rise as single crystal growing after isostatic cool pressing becomes block or isostatic pressed does not become block and expect.
All the other contents are all identical with described in embodiment 1.
Experimental result shows: the present embodiment also can grow crystal ingot size and reach Ф 20mm × 70mm, Curie temperature at about 300 DEG C, umpolarization temperature at about 176 DEG C, piezoelectric constant d
33reach 280pC/N, electromechanical coupling factor k
tthe few plumbous sodium bismuth titanate-lead titanate piezoelectric monocrystal of high-curie temperature more than 50%.
Embodiment 3
The difference of the present embodiment and embodiment 1 is only:
It is as follows that preparation single crystal growing works the operation of expecting:
1) according to chemical formula Na
0.5bi
0.5tiO
3the purity accurately taking stoichiometric ratio is greater than sodium carbonate and the bismuth oxide of 99.99%, and ball milling makes to mix for 24 hours, at 1100 DEG C, then carries out the solid state reaction of 4 hours, sinter the polycrystal of NBT into;
2) according to chemical formula PbTiO
3the purity accurately taking stoichiometric ratio is greater than titanium dioxide and the plumbous oxide of 99.99%, and ball milling makes to mix for 24 hours, then carries out the solid state reaction of 4 hours at 1100 DEG C, sinters the polycrystal of PT into;
3) according to general formula 0.86Na
0.5bi
0.5tiO
3-0.14PbTiO
3accurately take NBT and the PT polycrystal of stoichiometric ratio, ball milling makes to mix for 24 hours, then carries out the solid state reaction of 6 hours at 1100 DEG C, sinters the compound of NBT-PT into, fine grinding again, rises as single crystal growing and expects after isostatic cool pressing becomes block or isostatic pressed does not become block.
All the other contents are all identical with described in embodiment 1.
Experimental result shows: the present embodiment also can grow crystal ingot size and reach Ф 20mm × 70mm, Curie temperature at about 300 DEG C, umpolarization temperature at about 176 DEG C, piezoelectric constant d
33reach 280pC/N, electromechanical coupling factor k
tthe few plumbous sodium bismuth titanate-lead titanate piezoelectric monocrystal of high-curie temperature more than 50%.
Finally be necessary described herein: above embodiment is only for being described in more detail technical scheme of the present invention; can not be interpreted as limiting the scope of the 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 (6)
1. a preparation method for sodium bismuth titanate-lead titanate piezoelectric monocrystal, is characterized in that, is falling crucible method, comprises following concrete steps:
A) prepare single crystal growing to rise and expect, concrete operations are as follows:
According to general formula (1-x) Na
0.5bi
0.5tiO
3-xPbTiO
3, accurately take each raw material of the sodium carbonate of stoichiometric ratio, bismuth oxide, titanium dioxide and plumbous oxide, ball milling makes abundant mixing, then rises as single crystal growing after isostatic cool pressing becomes block or isostatic pressed does not become block and expects;
Or,
According to general formula (1-x) Na
0.5bi
0.5tiO
3-xPbTiO
3accurately take each raw material of the sodium carbonate of stoichiometric ratio, bismuth oxide, titanium dioxide and plumbous oxide, ball milling makes abundant mixing, then at 1000 ± 100 DEG C, carry out the solid state reaction of 4 ~ 6 hours, sinter the compound of NBT-PT into, fine grinding again, rises as single crystal growing and expects after isostatic cool pressing becomes block or isostatic pressed does not become block;
Or,
A1) according to chemical formula Na
0.5bi
0.5tiO
3accurately take sodium carbonate and the bismuth oxide of stoichiometric ratio, ball milling makes to mix, and at 1000 ± 100 DEG C, then carries out the solid state reaction of 4 ~ 6 hours, sinter the polycrystal of NBT into;
A2) according to chemical formula PbTiO
3accurately take titanium dioxide and the plumbous oxide of stoichiometric ratio, ball milling makes to mix, and then carries out the solid state reaction of 4 ~ 6 hours at 1000 ± 100 DEG C, sinters the polycrystal of PT into;
A3) according to general formula (1-x) Na
0.5bi
0.5tiO
3-xPbTiO
3, accurately take NBT and the PT polycrystal of stoichiometric ratio, ball milling makes to mix, then the solid state reaction of 4 ~ 6 hours is carried out at 1000 ± 100 DEG C, sinter the compound of NBT-PT into, then fine grinding, rise as single crystal growing after isostatic cool pressing becomes block or isostatic pressed does not become block and expect;
B) obtained single crystal growing is risen expect and load in crucible, add seed crystal, falling crucible method is adopted to carry out single crystal growing: controlling single crystal growing furnace temperature is 1380 ~ 1500 DEG C, melt soaking time is 3 ~ 10 hours, furnace temperature temperature rise rate in crystal growing process is 0 ~ 3 DEG C/day, crucible fall off rate is 0.2 ~ 1mm/h, and the thermograde of solid-liquid interface is 5 ~ 10 DEG C/mm, and the maximum temperature gradient of crucible descending direction is 1 ~ 7 DEG C/mm;
C) growth terminates, and is cooled to room temperature;
Described general formula (1-x) Na
0.5bi
0.5tiO
3-xPbTiO
3in 0.01≤x≤0.14.
2. preparation method according to claim 1, is characterized in that: described crucible is platinum crucible.
3. preparation method according to claim 2, is characterized in that: described crucible adopts the individual layer of sealing or double-deck or three-decker, and every layer thickness is 0.10 ~ 0.20mm.
4. preparation method according to claim 1, it is characterized in that: described seed crystal is the similar niobic magnesium acid lead-lead titanate single-crystal of NBT-PT monocrystalline or crystalline network, seed crystal be oriented to <111>, <110> or <100>.
5. preparation method according to claim 1, is characterized in that: described seed size is Ф (19 ~ 20) mm × 50mm.
6. preparation method according to claim 1, is characterized in that: stop growing as crucible decline 5cm, be then down to room temperature with the rate of temperature fall of 50 ~ 200 DEG C/h.
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| CN113113582B (en) * | 2021-03-19 | 2022-11-22 | 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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| Title |
|---|
| 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;Guisheng Xu, et al.;《Journal of Crystal Growth》;20050101;第275卷;第114-115页 * |
| Structural phase transition study of the morphotropic phase boundary compositions of Na0.5Bi0.5TiO3–PbTiO3;Sarab Preet Singh et al.;《Journal of physics: condensed matter》;20090817;第21卷;第375902(2)页第2和第375902(6)页第3.3部分 * |
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