CN109280975A - A kind of bismuth sodium titanate nanometer line and preparation method thereof - Google Patents
A kind of bismuth sodium titanate nanometer line and preparation method thereof Download PDFInfo
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- CN109280975A CN109280975A CN201811310707.7A CN201811310707A CN109280975A CN 109280975 A CN109280975 A CN 109280975A CN 201811310707 A CN201811310707 A CN 201811310707A CN 109280975 A CN109280975 A CN 109280975A
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- 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
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- C30B29/32—Titanates; Germanates; Molybdates; Tungstates
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- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
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- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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Abstract
The invention discloses a kind of bismuth sodium titanate nanometer lines of high tension electricity coefficient with striped domain structure.The striped farmland is alternately arranged along the length direction of bismuth sodium titanate nanometer line.The invention also discloses a kind of preparation methods of bismuth sodium titanate nanometer line, comprising the following steps: (1) prepares bismuth-sodium titanate precursor solution (2) hydrothermal synthesis bismuth sodium titanate nanometer line.The bismuth sodium titanate nanometer line with regular striped domain structure can be prepared in the method.The rule striped domain structure can effectively improve the piezoelectric modulus of bismuth sodium titanate nanometer line.
Description
Technical field
The present invention relates to a kind of bismuth sodium titanate nanometer line and preparation method thereof with striped domain structure, belongs to inorganic non-gold
Belong to field of material technology.
Background technique
The development that the reduction of ferroelectric piezoelectric material dimension, the reduction of size have further pushed microelectronics industry integrated,
Also it is more in line with the trend of semicon industry.The characteristics of one-dimensional lead-free piezoelectric material is due to small in size and large specific surface area,
There is potential application prospect in fields such as Ferroelectric Random Access Memory (FRAM), Nano electro-mechanical system, energy harvesters.
Mi-Ri Joung et al. is 120 DEG C in temperature with hydro-thermal method, and KOH concentration is that reaction 144h is successfully prepared under 14M
Orthorhombic phase KNbO3Nano wire, piezoelectric modulus are about 11.6pm/V [Joung M R, Seo I T, Kim J S, et
al.Structural dependence of the piezoelectric properties of KNbO3,nanowires
synthesized by the hydrothermal method[J].Acta Materialia,2013, 61(10):3703-
3708.], the technical problems such as the preparation method is long there are the reaction time, piezoelectric modulus is small.
K Liu H et al. is 120 DEG C in temperature with hydro-thermal method, and NaOH concentration is that reaction 3h is successfully prepared under 12.5M
NaNbO3Nano wire, piezoelectric modulus are about 4pm/V [K Liu H, Zhang Z, Hu L, et al.New UV-A
Photodetector Based on Individual Potassium Niobate Nanowires with High
Performance [J] .Advanced Optical Materials, 2015,2 (8): 771-778.], which exists
The technical problems such as piezoelectric modulus is small.
And bismuth-sodium titanate (Na0.5Bi0.5TiO3, hereinafter referred to as NBT) and it is typical ABO3Type perovskite structure, Curie's temperature
Degree is 320 DEG C, has biggish remanent polarization P at room temperaturer(38μC/cm2), it is considered to be one kind has excellent piezoelectricity
The unleaded perovskite material of performance.
Mohammad Bagher Ghasemian et al. is 200 DEG C in temperature with hydro-thermal method, and NaOH concentration is anti-under 12M
The BNT nanofiber that 20h successfully prepares diameter 150-200nm, length is 5 μm is answered, piezoelectric modulus is about 15pm/V
[Ghasemian M B,Lin Q,Adabifiroozjaei E,et al.Morphology control and large
piezoresponse of hydrothermally synthesized lead-free piezoelectric
(Bi0.5Na0.5)TiO3Nanofibres [J] .Rsc Advances, 2017,7 (25): 15020-15026.], the preparation method
Still remain the technical problems such as reaction temperature is high, piezoelectric modulus is small.
In conclusion the one-dimensional lead-free piezoelectric material of preparation method preparation that there is reaction temperatures is high, the hydro-thermal time is long,
The technical problems such as piezoelectric modulus is small.
Summary of the invention
The first purpose of the invention is to provide one kind to have the alternate striped domain structure of different contrasts, high tension electricity coefficient
One-dimensional unleaded perovskite NBT nano wire.
A second object of the present invention is to provide a kind of preparation methods of NBT nano wire.
A kind of NBT nano wire of the present invention, has striped farmland.
Inventors discovered through research that the NBT nano wire is in the state of unpolarized (no applied voltage) by the inner
There is alternately arranged striated domain structure along its length in portion, there are certain directionality for spontaneous polarization.Moreover, described
NBT nano wire is NBT monocrystalline, and the presence of the specific domain structure of this aligned transfer tends to the nano wire along its direction of growth
High piezoelectric modulus is presented so that nano wire be made to show stronger piezoelectric property in higher anisotropy.After polarization,
The striped farmland of NBT nano wire arranges more regular, and polarization direction can more have directionality, so that its piezoelectric property can table
Now it is more excellent.
The striped farmland is alternately arranged along the length direction of NBT nano wire.
The width of the striped farmland is 20-65nm.
The NBT nanowire surface is smooth, and structure is uniform, there is the lattice fringe of clear rule, and interplanar distance is
0.991nm corresponds to (101) crystal face.
The length of the NBT nano wire is 4-10 μm, width 70-200nm.
A kind of preparation method of NBT nano wire of the present invention, includes the following steps:
Step 1: NBT precursor solution is prepared；
Bi is dissolved in organic acid, obtains solution A；Ti is dissolved in Organic Alcohol, obtains solution B；By Na salt
It is dissolved in H2In O, solution C is obtained；
Solution A is added in solution B, is added in solution C after stirring, pH adjusting agent is added into obtained mixed solution,
Obtain NBT precursor solution；
Step 2: hydrothermal synthesis NBT nano wire；
The resulting NBT precursor solution of step 1 is subjected to hydro-thermal reaction, is then centrifuged for, it is dry, it obtains NBT nanometers described
Line.
The source Bi includes Bi salt, and the Bi salt includes bismuth nitrate；
The source Ti includes titanate esters, and the titanate esters include butyl titanate；
The Na salt includes sodium nitrate.
The organic acid includes glacial acetic acid, and the Organic Alcohol includes ethyl alcohol.
The pH adjusting agent includes NaOH solution, and the concentration of the NaOH solution is 10-14mol/L.
The Na salt, the source Bi and the molar ratio in the source Ti are 1:1:2-1:1.1:2.1.
The NaNO3: Bi (NO3)3: Ti (OC4H9)4Molar ratio be 1:1:2-1:1.1:2.1.
The temperature of the hydro-thermal reaction is 150-180 DEG C, and the time of hydro-thermal reaction is 40-50h.
The temperature of the hydro-thermal reaction is 160-175 DEG C, and the time of hydro-thermal reaction is 45-49h.
Inventors discovered through research that the initial phase of the hydro-thermal reaction, NBT product morphology is spherical nanocrystalline and is permitted
Mostly tiny bulk crystals.TiO with the further progress of reaction, in solution2·nH2The solubility of O increases,
And Na+And Bi3+Ion is largely assembled, and the saturation degree of solution reaches the critical saturation of hydro-thermal reaction, provides one at this moment
Form the control environment of striped farmland NBT nano wire.
NBT nano wire is to be based on oriented growth mechanism and long great achievement line from the small nanometer blocks when reaction time being for 24 hours, adjacent
Small nanometer blocks combined automatically along identical crystal orientation, spontaneous and oriented attachment driving force can cause particle surface free
The significantly reduction of energy, and then the NBT nano wire with striped domain structure is formed, see Fig. 6 (c) and figure of Detailed description of the invention of the present invention
11.60h will further be extended to the reaction time, NBT product morphology is transformed into single NBT micron block by linear NBT is nanocrystalline,
See comparative example 2.And under the same reaction time, hydrothermal temperature is improved, crystal structure rate can further increase, glomeration
Nano wire, at sharp-featured NBT micron block, is shown in comparative example 4 along c-axis fast-growth.Shorten and extend reaction time and raising
Hydrothermal temperature is all unfavorable for the formation of striped farmland NBT nano wire, so the optimal parameter group of preparation striped farmland NBT nano wire is combined into
Hydrothermal temperature is 170 DEG C and the reaction time is 48h.
Compared with the existing technology, the present invention have it is following the utility model has the advantages that
(1) the preparation method equipment of NBT nano wire of the invention is simple, easy to operate, easy control of process conditions, energy consumption
Low, non-environmental-pollution, it is easy to industrialized production.
(2) the NBT nano wire that the present invention is prepared has striped domain structure, which effectively improves NBT nano wire
Piezoelectric property.
(3) effective piezoelectric coefficient d of NBT nano wire prepared by the present invention33About 24pm/V.
Detailed description of the invention
Fig. 1 is the experiment flow figure for preparing NBT precursor solution；
Fig. 2 is the XRD diagram of NBT powder under the differential responses time；
Using X-ray diffractometer (XRD, X'PertPRO, Panaco company, Holland) to resulting under the differential responses time
NBT powder is tested, and resulting XRD diagram is as shown in Figure 2.It can be seen from the figure that being compared to the reaction time in comparative example 1
Diffraction maximum measured by powder when for 24 hours, the product obtained after extending the reaction time to 48h in embodiment 1, diffraction peak intensity with
The increase of time and become strong, diffraction maximum is in comparison more sharp.It is obtained after the reaction time reaches 60h in comparative example 2
Product, the product that diffraction peak intensity obtains when 48h compared with the reaction time are weakened.When the reaction time increases in comparative example 3
The product obtained after to 72h, diffraction peak intensity further weaken.Illustrate that the reaction time appropriate plays promotion to crystallinity
Effect, overlong time or too short, crystallization effect is bad.
Fig. 3 is the SEM figure of NBT powder under the differential responses time；
Using scanning electron microscope (SEM, MIRA3 LMU, Tai Siken company, Czech) to gained under the differential responses time
NBT powder tested, resulting SEM figure is as shown in Figure 3.
Fig. 3 (a) be in comparative example 1 of the present invention the reaction time be that the SEM of NBT nanosphere is descended to scheme for 24 hours, product NBT is nanocrystalline
It is divided into two kinds of forms, it is small blocky and spherical, wherein spherical nanocrystalline size is larger, in 300nm or so.
Fig. 3 (b) is the SEM figure that the reaction time is NBT nano wire under 48h in the embodiment of the present invention 1, a large amount of line occurs
Shape NBT is nanocrystalline and to be mingled with the different spherical NBT of a little diameter nanocrystalline.Wherein nanowire surface is very flat and smooth, diameter
It is smaller, in 70nm between 200nm.Linear nanocrystalline accumulated by many tiny bulk crystals is reunited.
Fig. 3 (c) is the SEM figure that the reaction time is the micro- cubic block of NBT under 60h in comparative example 2 of the present invention, and product morphology occurs
The variation of essence, the spherical nanocrystalline and linear nanocrystalline disappearance of script, it is brilliant to generate single lumpy nanometer, lumpy nanometer
For brilliant size between 0.5 μm -1 μm, corner is clearly demarcated, smooth surface.
Fig. 3 (d) is the SEM figure that the reaction time is NBT nanometer sheet under 72h in comparative example 3 of the present invention, is generated in 60h
The clearly demarcated lumpy nanometer of corner angle brilliant further division, the sheet for foring intersection is nanocrystalline.
It is possible thereby to illustrate, the reaction time plays certain regulating and controlling effect to nanocrystalline pattern, but too long anti-
It can promote nanocrystalline division between seasonable, it is suppressed that the progress of reaction.
Fig. 4 is the XRD diagram of NBT powder under different hydrothermal temperatures；
NBT powder resulting under different hydrothermal temperatures is tested using XRD, resulting XRD diagram is as shown in Figure 4.From
As can be seen that spreading out for typical perovskite phase structure occurs in NBT nano-powder when reaction temperature is 170 DEG C and 200 DEG C in figure
Peak is penetrated, and diffraction peak intensity variation is less, have no miscellaneous phase generation, shows that improving hydrothermal temperature influences not the crystallization effect of NBT
Greatly.
Fig. 5 is the SEM figure of NBT powder under different hydrothermal temperatures；
NBT powder resulting under different hydrothermal temperatures is tested using SEM, resulting SEM figure is as shown in Figure 5.
Fig. 5 (a) is the SEM figure that hydrothermal temperature is NBT nanosphere at 170 DEG C in the embodiment of the present invention 1.As shown,
It is nanocrystalline that the spherical NBT that a large amount of threadiness NBT is nanocrystalline and inclusion diameter size is in 100nm-500nm is generated at 170 DEG C,
Wherein nanowire diameter is smaller, and diameter is in 70nm-200nm or so.
Fig. 5 (b) is the SEM figure that hydrothermal temperature is NBT nano wire at 200 DEG C in comparative example 4 of the present invention, can from SEM figure
To find out, generate cube microlith of the size at 0.5 μm -1 μm, and there are the crystal of lamella cross-like in product, this be because
For with the raising of reaction temperature, a degree of division occurs in a cube microlith, from without generating nano wire.
Fig. 6 is the mechanism schematic diagram of the NBT powder of hydrothermal synthesis different-shape；
Fig. 6 (a) is the mechanism schematic diagram of hydrothermal synthesis NBT nanosphere.Hydro-thermal reaction is in initial phase, due to TiO2·
nH2The solution rate of O is far below Bi (NO3)3·nH2The solution rate of O has led to lentissimo dissolution-recrystallization mistake
Journey, the stage is mainly based on converted in-situ mechanism.The Na of dissolution+And Bi3+Ion and undissolved TiO2Particle surface occurs
Reaction, then forms continuous NBT structure sheaf on surface by growth in situ mechanism, until TiO2Particle is consumed, and is obtained
Spherical nanocrystalline and many tiny bulk crystals.
Fig. 6 (b) is the mechanism schematic diagram of hydrothermal synthesis NBT nano wire.Due to the extension of the hydro-thermal reaction time, in solution
TiO2·nH2The solubility of O increases,And Na+And Bi3+Ion is largely assembled, and the saturation degree of solution reaches hydro-thermal reaction
Critical saturation, dissolution-recrystallization mechanism starts working, the growth in situ mechanism and dissolution-recrystallization mechanism in the stage
It works simultaneously.Dissolution-recrystallization makes unstable spheric grain be recrystallized into more stable and clear-cut NBT nanometer
Ball.NBT nano wire be from the small nanometer blocks of initial phase based on oriented growth mechanism long great achievement line.Lesser adjacent receives
Rice block combines automatically along identical crystal orientation, and for thermodynamics, the driving force of spontaneous oriented attachment can cause
The significantly reduction of particle surface free energy, and then formed with striped farmland NBT nano wire, see Figure 11 of Detailed description of the invention of the present invention
It is shown.
Fig. 6 (c) is the mechanism schematic diagram of the micro- cubic block of hydrothermal synthesis NBT.The hydro-thermal reaction time extends again, in solution
TiO2·nH2O and Bi (NO3)3·nH2O further dissolves, Ti-O key withIon exists, and the saturation degree of solution is greater than
The critical saturation of hydro-thermal reaction, the stage is mainly based on dissolution-recrystallization mechanism.NBT nano wire aggregates into microballoon, gathers
The nano wire of integrated ball along c-axis fast-growth at micron block, the cu μ m block gradually sharp-featured NBT micron block of long great achievement.
And reacting is influenced by dissolution-recrystallization mechanism, NBT nanosphere, which gradually dissolves, to become smaller until disappearing.According to classical crystal growth
Theory, NBT particle can undergo an of short duration forming core phase.When reactant is reacted because of particle growth to be exhausted, i.e., reactant is dense
When Cmin needed for degree is less than forming core, forming core stops, and Ostwald curing will occur, and biggish particle continues to grow
Greatly, lesser particle can be smaller and smaller until disappearing, and spherical and linear NBT is nanocrystalline in such as present invention is transformed into single NBT
Micron block is the same, shown in the Fig. 3 (b) and Fig. 3 (c) for seeing Detailed description of the invention of the present invention.
Fig. 7 (a) is the TEM figure of single NBT nano wire in the embodiment of the present invention 1；
Using transmission electron microscope (JEM-2000CX, Jeol Ltd., Japan) to the resulting powder of embodiment 1
Body is tested, and resulting transmission electron microscope picture (TEM) is such as shown in Fig. 6 (a), and as can be seen from the figure the size of nano wire is in 70-
Between 100nm, structure is uniform, and surface is smooth, straight state.
Fig. 7 (b) is HRTEM and the SAED figure of single NBT nano wire in the embodiment of the present invention 1；
The resulting high resolution electron microscope (HREM) figure (HRTEM) of embodiment 1 and selective electron diffraction figure (SAED) such as Fig. 6
(b) shown in, the lattice fringe of clear rule, illustrates that its crystallinity is good, interplanar distance is as we can see from the figure
0.991nm corresponds to (101) crystal face, and the Fast Fourier Transform (FFT) figure (FFT) shown in illustration confirms that NBT nano wire is monocrystalline
Body.
Fig. 8 is the shape appearance figure of single NBT nano wire in the embodiment of the present invention 1；
Using the inner piezoelectricity force microscope of atomic force microscope (AFM, MFP-3D Infinity, Asylum Research)
(PFM) module compares example 1, gained using microstructure of the contact mode to the single NBT nano wire that embodiment 1 obtains
Shape appearance figure it is as shown in Figure 8.As can be seen from Figure 8 single NBT nano wire has smooth surface, and diameter is about 200nm.
Fig. 9 is the three-dimensional farmland state figure of single NBT nano wire in the embodiment of the present invention 2；
It is tested using microstructure of the PFM to the single NBT nano wire that embodiment 1 obtains, obtained three-dimensional farmland state
Figure is as shown in Figure 9.
Fig. 9 (a)-(b), Fig. 9 (c)-(d), Fig. 9 (e)-(f) are respectively the single direction NBT nano wire z, x, y in embodiment 1
Phase diagram and amplitude image, wherein the acquisition of y direction signal (is detailed in by the way that the sample is rotated clockwise 90 ° of acquisitions in face
Illustration), to construct NBT nano wire completely three-dimensional farmland state information.In these VPFM and LPFM images, NBT nano wire
Inside present arrangement along its length and the striated domain structure that is alternately present of contrast color, each striped farmland width it is uniform and
It is each unequal, there is clearly domain boundary between striped farmland (white dashed line indicates striped domain boundary).The specific domain structure of this aligned transfer
So that nano wire integrally tends to higher anisotropy, so that so that nano wire is shown stronger piezoelectric property is presented high piezoelectricity
Coefficient.
Figure 10 is the phase-voltage ferroelectric hysteresis loop figure and amplitude-voltage control of single NBT nano wire in the embodiment of the present invention 1
Shape curve graph.
It is tested, is obtained as shown in Figure 10 using piezoelectric property of the PFM to the single NBT nano wire that embodiment 1 obtains
Phase-voltage ferroelectric hysteresis loop figure and amplitude-voltage butterfly curve.
It can be seen from fig. 11 that NBT nano wire occurs typical " butterfly curve ", the both wings of curve are very symmetrical,
It is uniform and full, and the crosspoint of curve is 0V or so in voltage, and symmetrical centre illustrates NBT nano wire almost without offset
Piezoelectric property it is excellent, and have high piezoelectric modulus.Simultaneously it can also be seen that phase is all completed when voltage is about ± 45V
180 ° of overturning illustrates that NBT nano wire has excellent ferroelectric properties.
Figure 11 is the microprocess schematic diagram of hydrothermal synthesis striped farmland NBT nano wire；
Hydrothermal synthesis striped farmland NBT nano wire is to be based on oriented growth mechanism from the small nanometer blocks of reaction initial phase and grow
Great achievement line, adjacent small nanometer blocks combine automatically along identical crystal orientation.For thermodynamics, spontaneous orientation is inhaled
Attached driving force can cause the significantly reduction of particle surface free energy, and then form the NBT nano wire with striped domain structure.
Specific embodiment
The microstructure and piezoelectric property for testing NBT nano wire, include the following steps:
(1) it takes above-mentioned resulting a small amount of NBT powder to be directly scattered in ethanol solution, it is then made using ultrasonic vibration instrument
It is uniformly dispersed；
(2) a resulting NBT nanowire dispersion of drop step (1) is taken to be placed in Pt/Ti/SiO using rubber head dropper2/ Si base
Then on piece places the substrate above 80 DEG C of vacuum ovens and is dried；
(3) step (2) resulting substrate being placed in annealing furnace, setting sintering temperature is 200 DEG C, 3 DEG C of heating rate/
Min keeps the temperature 1h, then cooled to room temperature after being warming up to 200 DEG C；
(4) aobvious using atomic force microscope (AFM, MFP-3D Infinity, Asylum Research) inner piezoelectric forces
Micro mirror (PFM) module is tested using microstructure and piezoelectric property of the contact mode to NBT nano wire.
Comparative example 1:
A kind of NBT raw powder's production technology, includes the following steps:
Step 1: NBT precursor solution is prepared
(1) by Bi (NO3)3·5H2O is dissolved in CH3In COOH and magnetic agitation, it is denoted as solution A；
(2) to Ti (OC4H9)4A small amount of CH is added dropwise in solution3CH2OH is simultaneously stirred evenly, and is denoted as B solution；
(3) by NaNO3It is dissolved in H2In O, it is denoted as C solution；
(4) solution A is added into B solution dropwise, C solution is added dropwise after stirring evenly 5min, resulting mixing is molten
Liquid carries out magnetic agitation 10min；
(5) NaOH is dissolved in H2In O, the NaOH solution that concentration is 12mol/L is obtained；
(6) that step (5) resulting NaOH solution is slowly added to step (4) by the way of glass bar drainage is resulting molten
Liquid, then uses magnetic stirring apparatus high-speed stirred 1h, and the precursor solution being uniformly mixed is shown in Fig. 1 of Detailed description of the invention of the present invention；
Above-mentioned Ti (OC4H9)4、Bi(NO3)3Aqueous solution, NaNO3The dosage of aqueous solution, by NaNO3: Bi (NO3)3: Ti
(OC4H9)4Molar ratio be 1:1:2 ratio calculate；
Step 2: hydrothermal synthesis NBT powder
(1) that the resulting precursor solution of step 1 is transferred to 50ml polytetrafluoroethylene (PTFE) hydro-thermal according to 80% compactedness is anti-
It answers in kettle, is placed in vacuum oven, setting reaction temperature is 170 DEG C, and the reaction time is for 24 hours；
(2) therefrom control drying box takes out hydrothermal reaction kettle cooled to room temperature after reaction；
(3) step (2) resulting product is centrifuged to obtain sediment by 5000r/min, then is cleaned directly with deionized water
Until the pH of solution is 7；
(4) product that step (3) obtains 80 DEG C of baking ovens are placed in be dried to get NBT powder.
Embodiment 1:
Implement a kind of NBT raw powder's production technology, includes the following steps:
Only step 2 (1) the hydro-thermal reaction time extends to 48h, other are identical as comparative example 1, finally obtain NBT powder
Body.
Comparative example 2:
A kind of NBT raw powder's production technology, includes the following steps:
Only step 2 (1) the hydro-thermal reaction time extends to 60h, other are identical as comparative example 1, finally obtain NBT powder
Body.
Comparative example 3:
A kind of NBT raw powder's production technology, includes the following steps:
Only step 2 (1) the hydro-thermal reaction time extends to 72h, other are identical as comparative example 1, finally obtain NBT powder
Body；
Comparative example 4:
A kind of NBT raw powder's production technology, includes the following steps:
Only step 2 (1) hydrothermal temperature is improved to 200 DEG C, other are same as Example 1, finally obtain NBT powder
Body；
In conclusion the present invention provides a kind of NBT nano wire and preparation method thereof with striped domain structure, hydro-thermal temperature
Degree and reaction time play regulating and controlling effect to the microscopic appearance of NBT powder.By the formation for comparing different-shape NBT nano wire
Mechanism has found the best preparation parameter combination for the nano wire to form regular domain structure: when hydrothermal temperature is 170 DEG C, reacts
Between to obtain the good NBT nano wire of crystallinity under the conditions of 48h.The different alternate striped domain structures of contrast are presented in its inside, into
And obtain high piezoelectric modulus.
Claims (10)
1. a kind of bismuth sodium titanate nanometer line, it is characterised in that: have striped farmland.
2. bismuth sodium titanate nanometer line as described in claim 1, it is characterised in that: the striped farmland is along bismuth sodium titanate nanometer line
Length direction is alternately arranged.
3. bismuth sodium titanate nanometer line as claimed in claim 1 or 2, it is characterised in that: the width of the striped farmland is 20-
65nm。
4. bismuth sodium titanate nanometer line as described in any one of claims 1-3, it is characterised in that: the bismuth sodium titanate nanometer line
Length is 4-10 μm, width 70-200nm.
5. the preparation method based on bismuth sodium titanate nanometer line described in claim 1-4, which is characterized in that include the following steps:
Step 1: bismuth-sodium titanate precursor solution is prepared；
Bi is dissolved in organic acid, obtains solution A；Ti is dissolved in Organic Alcohol, obtains solution B；Na salt is dissolved in
H2In O, solution C is obtained；
Solution A is added in solution B, is added in solution C after stirring, pH adjusting agent is added into obtained mixed solution, obtains
Bismuth-sodium titanate precursor solution；
Step 2: hydrothermal synthesis bismuth sodium titanate nanometer line；
The resulting bismuth-sodium titanate precursor solution of step 1 is subjected to hydro-thermal reaction, is then centrifuged for, it is dry, it obtains the NBT and receives
Rice noodles.
6. the preparation method of bismuth sodium titanate nanometer line as claimed in claim 5, it is characterised in that: the source Ti includes metatitanic acid
Ester.
7. the preparation method of bismuth sodium titanate nanometer line as claimed in claim 5, it is characterised in that: the pH adjusting agent includes
NaOH solution, the concentration of the NaOH solution are 10-14mol/L.
8. such as the preparation method of the described in any item bismuth sodium titanate nanometer lines of claim 5, it is characterised in that: the Na salt, Bi
The molar ratio in source and the source Ti is 1:1:2-1:1.1:2.1.
9. the preparation method of bismuth sodium titanate nanometer line as claimed in claim 5, it is characterised in that: the temperature of the hydro-thermal reaction
It is 150-180 DEG C, the time of hydro-thermal reaction is 40-50h.
10. the preparation method of the bismuth sodium titanate nanometer line as described in claim 5 or 9, it is characterised in that: the hydro-thermal reaction
Temperature is 160-175 DEG C, and the time of hydro-thermal reaction is 45-49h.
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