CN107055597A - A kind of quick method for preparing cubic bismuth titanate sodium powder body under low temperature - Google Patents
A kind of quick method for preparing cubic bismuth titanate sodium powder body under low temperature Download PDFInfo
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Abstract
The present invention provides a kind of quick method for preparing cubic bismuth titanate sodium powder body under low temperature, comprises the following steps, step (1), and configuration concentration is 10~16mol/L NaOH settled solutions；Step (2), configuration concentration is 0.1~0.2mol/L Bi (NO3)3·5H2O solution, obtains settled solution A；Step (3), by Ti (OC4H9)4It is added drop-wise in settled solution A, mixed solution B is obtained after stirring；Step (4), NaOH settled solutions are added dropwise in mixed solution B, are uniformly mixed to obtain Na0.5Bi0.5TiO3Precursor liquid；Step (5), by Na0.5Bi0.5TiO3Precursor liquid carries out microwave hydrothermal reaction；Step (6), microwave hydrothermal reaction terminates question response product and is cooled to after room temperature, will obtain a cube Na after the washing of reacted sediment, freeze-day with constant temperature and sieving0.5Bi0.5TiO3Powder.
Description
Technical field
Powder technology is prepared the present invention relates to wet chemistry method, quickly cubic bismuth titanate sodium powder is prepared under specially a kind of low temperature
The method of body.
Background technology
Piezoelectric ceramics is suffered from extensively as a kind of important ceramic material in fields such as machinery, electronics, space flight and aviation
General application.At present, the piezoelectric ceramics used is concentrated mainly in the material of lead base, and PbO content accounts for material in this material
Expect 70% or so of total amount.PbO is a kind of harmful substance, preparation in material, use and discard after processing procedure in ring
Border and human body all produce harm.Therefore, develop new, function admirable, in accordance with natural environment leadless piezoelectric ceramics into
For a research topic that is urgent and having important practical significance.Bismuth-sodium titanate (Na0.5Bi0.5TiO3) (NBT) be that class A is multiple
The ferroelectric material of the perovskite structure in conjunction generation, NBT has stronger ferroelectricity, and numerous scholars are caused with its excellent performance
Concern, it is considered to be one of most promising candidate material of leadless piezoelectric ceramics.
NBT preparation is all prepared using conventional solid-state method mostly, and this method technique is simpler, also is adapted for large-scale production,
But there is high synthesis temperature, easy reunion and be difficult to obtain thinner particle in conventional solid-state method, while the ceramics burnt till are in the presence of densification
Property is poor, sample sintering temperature is too high and excessively recrystallizes and can not meet the requirement of high-technology field.Compared with other method,
Microwave heating is interior heating, can greatly save energy, and control is easy in microwave heating, starts microwave, immediately with reactor
Interior material effect, carries out hydro-thermal reaction, closes microwave, and reaction stops quickly, and hysteresis effect is small.Microwave, which is accelerated, simultaneously reacted
Journey so that the reaction time shortens, and can quickly prepare the uniform powder of complete crystallization, particle diameter distribution.This method, which has, to be prepared
Technique is simple, be widely used without series of advantages such as calcining, the purity height of powder, and reaction temperature is relatively low.
The content of the invention
For problems of the prior art, the present invention provides and quickly prepares cubic bismuth titanate sodium powder body under a kind of low temperature
Method, this method reaction medium is water, safe, and technique is simple, makes reaction more full and uniform using microwave heating, heats
Faster, the cycle is short, and reaction temperature is relatively low and saves the energy, be made that powder grain development is complete, particle diameter distribution is uniform and purity compared with
It is high.
The present invention is to be achieved through the following technical solutions：
The quick method for preparing cubic bismuth titanate sodium powder body, comprises the following steps under a kind of low temperature,
Step (1), configuration concentration is 10~16mol/L NaOH settled solutions；
Step (2), configuration concentration is 0.1~0.2mol/L Bi (NO3)3·5H2O solution, and to Bi (NO3)3·5H2O
Nitric acid is instilled in solution, Bi (NO are continued stirring until3)3·5H2O is completely dissolved, and obtains settled solution A；
Step (3), by Ti (OC4H9)4It is added drop-wise in settled solution A, mixed solution B, wherein Ti is obtained after stirring
(OC4H9)4With Bi (NO in step (2)3)3·5H2O mol ratio is 1:1~1:2；
Step (4), the NaOH settled solutions obtained in step (1) are added dropwise in mixed solution B, are uniformly mixed,
Obtain Na0.5Bi0.5TiO3Precursor liquid；
Step (5), by Na resulting in step (4)0.5Bi0.5TiO3Precursor liquid carries out microwave hydrothermal reaction；
Step (6), microwave hydrothermal reaction terminates question response product and is cooled to after room temperature, reacted sediment is washed,
A cube Na is obtained after freeze-day with constant temperature and sieving0.5Bi0.5TiO3Powder.
It is preferred that, in described step (1), the concentration of NaOH settled solutions is 12~16mol/L.
It is preferred that, in described step (2), the amount for adding nitric acid is 1~2mL.
It is preferred that, in described step (4), NaOH settled solutions are added dropwise in mixed solution B dropwise, stir 0.2~1h
Milky Na is obtained after well mixed0.5Bi0.5TiO3Precursor liquid.
It is preferred that, in described step (5), the reaction temperature of microwave hydrothermal reaction is 150~180 DEG C, and the reaction time is
20~30min.
It is preferred that, in described step (5), microwave reaction power is 300~500W.
It is preferred that, in described step (5), by Na resulting in step (4)0.5Bi0.5TiO3Precursor liquid is put into reaction
In kettle, then reactor is put into microwave hydrothermal parallel projects instrument carries out hydro-thermal reaction.
Further, the filling rate in described reactor is 35%~40%.
It is preferred that, in step (6), treat that temperature is down to room temperature in microwave hydrothermal parallel projects instrument, when pressure is reduced to 0, take out
Reactor, the sediment in reactor is washed respectively with deionized water and absolute ethyl alcohol, is obtained after carrying out freeze-day with constant temperature, sieving
Required powder.
Further, in described step (6), first it is washed with deionized after 3~5 times and washs 4~6 with absolute ethyl alcohol again
It is secondary.
Compared with prior art, the present invention has following beneficial technique effect：
The present invention quickly prepares cubic bismuth titanate sodium powder body at low temperature using method rapidly and efficiently, different from the past
Traditional solid phase method, this method has the advantages that more rapidly and efficiently and saves the energy.Compared to other method is utilized, by this
Plant cube Na prepared by controllable wet chemistry method0.5Bi0.5TiO3Powder purity height, powder granule narrow size distribution and powder granule
Size is controllable, crystal formation is good, and this method prepare powder needed for reaction time be greatly shortened, reaction temperature reduction is easy to get
To suitable stoichiometry thing, high-temperature calcination and ball milling are eliminated, so that impurity and fault of construction are avoided, and operation letter
Single, good process repeatability with low power consuming, pollutes the features such as small, yield is more with high investment less.Use microwave-hydrothermal method simultaneously
When, microwave energy plays oscillation action to reaction solution, is effectively promoted reaction and improves powder grain quality, reduces the group of particle
It is poly-.Prepare that the particle diameter distribution brought during the powder is uneven, sample calcining heat is too high, easy so as to improve conventional solid-state method
Reunite, the shortcomings of experimental period is long.Cube Na prepared by this method0.5Bi0.5TiO3Powder structure is stable, even particle distribution,
Purity is higher, is uniformly distributed in cube.
Further, by controlling NaOH solution drop rate, and multiple washing to sediment and deionization is first used
Washed again with absolute ethyl alcohol after water washing, improve the purity of sample, reduce the reunion of sample, strengthen the powder to the present invention
The degree of controllability of body granule-morphology.
Further, by controlling the mixing time of mixed solution, so as to improve Na0.5Bi0.5TiO3Precursor liquid it is equal
Even property, so as to ensure the purity of product and the utilization rate of raw material.
Further, the reaction time of the invention is greatly shortened, and can greatly save energy, reduces the pollution to environment.
Further, reaction temperature of the present invention is low, without calcining, and yield is more with high investment less, and obtained powder is uniformly distributed.
Brief description of the drawings
Fig. 1 is cube Na prepared by present example0.5Bi0.5TiO3Powder X ray diffracting spectrum.
Fig. 2 is cube Na prepared by present example0.5Bi0.5TiO3The scan image of powder.
Embodiment
With reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
Cube Na is prepared the invention provides quick under a kind of low temperature0.5Bi0.5TiO3The method of powder, technique is simple, weight
Renaturation is good, and reaction temperature is low, and the time is short, and powder, without calcining again, yield is with high investment few, can greatly save the energy, preparation
Powder purity it is high, and stoichiometric proportion is controllable, to Na0.5Bi0.5TiO3It is a kind of excellent preparation method for powder synthesis.
Specific such as following instance.
Example 1
The quick method for preparing cubic bismuth titanate sodium powder body, comprises the following steps under a kind of low temperature of the present invention,
(1) configure in NaOH settled solutions, solution, NaOH concentration is 12mol/L；
(2) configuration Bi (NO3)3·5H2In O solution, solution, Bi (NO3)3·5H2O concentration is 0.1mol/L, and to molten
Appropriate nitric acid is instilled in liquid, Bi (NO are continued stirring until3)3·5H2O is completely dissolved, and obtains settled solution A；In this preferred embodiment
Nitric acid used is 1ml；
(3) with pipette by Ti (OC4H9)4It is added drop-wise in settled solution A, obtains mixed solution B, wherein Ti (OC4H9)4With
Bi (NO in step (2)3)3·5H2O mol ratio is 1:1；
(4) by after the mixed solution B magnetic agitations in step (3), then NaOH settled solutions are added dropwise to mixing dropwise
In solution B, then at being uniformly mixed at room temperature, the Na of microwave hydrothermal reaction is obtained0.5Bi0.5TiO3Precursor liquid；
(5) by Na resulting in step (4)0.5Bi0.5TiO3Precursor liquid is put into reactor, then reactor is put into micro-
Hydro-thermal reaction is carried out in ripple hydro-thermal parallel projects instrument, reaction temperature is 160 DEG C, and the reaction time is 30min, and reaction power is
500W；The filling rate of reactor is 35% in this preferred embodiment.
(6) treat that temperature is down to room temperature in microwave hydrothermal parallel projects instrument, when pressure is reduced to 0, reactor is taken out, by reactor
In sediment be washed with deionized 3 times, then washed with absolute ethyl alcohol after 4 times, freeze-day with constant temperature carried out at 80 DEG C, 300 are crossed
Required cube Na is obtained after mesh sieve0.5Bi0.5TiO3Powder.
Example 2
The quick method for preparing cubic bismuth titanate sodium powder body, comprises the following steps under a kind of low temperature of the present invention,
(1) configure in NaOH settled solutions, solution, NaOH concentration is 14mol/L；
(2) configuration Bi (NO3)3·5H2In O solution, solution, Bi (NO3)3·5H2O concentration is 0.2mol/L, and to molten
Appropriate nitric acid is instilled in liquid, Bi (NO are continued stirring until3)3·5H2O is completely dissolved, and obtains settled solution A；In this preferred embodiment
Nitric acid used is 2ml；
(3) with pipette by Ti (OC4H9)4It is added drop-wise in settled solution A, obtains mixed solution B, wherein Ti (OC4H9)4With
Bi (NO in step (2)3)3·5H2O mol ratio is 1:1.5；
(4) by after the mixed solution B magnetic agitations in step (3), then NaOH settled solutions are added dropwise to mixing dropwise
In solution B, then at being uniformly mixed at room temperature, the Na of microwave hydrothermal reaction is obtained0.5Bi0.5TiO3Precursor liquid；
(5) by Na resulting in step (4)0.5Bi0.5TiO3Precursor liquid is put into reactor, then reactor is put into micro-
Hydro-thermal reaction is carried out in ripple hydro-thermal parallel projects instrument, reaction temperature is 180 DEG C, and the reaction time is 30min, and reaction power is
400W；The filling rate of reactor is 40% in this preferred embodiment.
(6) treat that temperature is down to room temperature in microwave hydrothermal parallel projects instrument, when pressure is reduced to 0, reactor is taken out, by reactor
In sediment be first washed with deionized 4 times, then washed with absolute ethyl alcohol after 4 times, freeze-day with constant temperature carried out at 80 DEG C, 300 are crossed
Required cube Na is obtained after sieve0.5Bi0.5TiO3Powder.
Example 3
It is quick under a kind of low temperature of the present invention to prepare cube Na0.5Bi0.5TiO3The method of powder, comprises the following steps, (1) matches somebody with somebody
Put in NaOH settled solutions, solution, NaOH concentration is 15mol/L；
(2) configuration Bi (NO3)3·5H2In O solution, solution, Bi (NO3)3·5H2O concentration is 0.1mol/L, and to molten
Appropriate nitric acid is instilled in liquid, Bi (NO are continued stirring until3)3·5H2O is completely dissolved, and obtains settled solution A；In this preferred embodiment
Nitric acid used is 1.5ml；
(3) with pipette by Ti (OC4H9)4It is added drop-wise in settled solution A, obtains mixed solution B, wherein Ti (OC4H9)4With
Bi (NO in step (2)3)3·5H2O mol ratio is 3:4；
(4) by after the mixed solution B magnetic agitations in step (3), then NaOH settled solutions are added dropwise to mixing dropwise
In solution B, then at being uniformly mixed at room temperature, the Na of microwave hydrothermal reaction is obtained0.5Bi0.5TiO3Precursor liquid；
(5) by Na resulting in step (4)0.5Bi0.5TiO3Precursor liquid is put into reactor, then reactor is put into micro-
Hydro-thermal reaction is carried out in ripple hydro-thermal parallel projects instrument, reaction temperature is 180 DEG C, and the reaction time is 20min, and reaction power is
300W；The filling rate of reactor is 36% in this preferred embodiment.
(6) treat that temperature is down to room temperature in microwave hydrothermal parallel projects instrument, when pressure is reduced to 0, reactor is taken out, by reactor
In sediment be first washed with deionized 4 times, then washed with absolute ethyl alcohol after 4 times, freeze-day with constant temperature carried out at 80 DEG C, 300 are crossed
Required cube Na is obtained after mesh sieve0.5Bi0.5TiO3Powder.
Example 4
It is quick under a kind of low temperature of the present invention to prepare cube Na0.5Bi0.5TiO3The method of powder, comprises the following steps, (1) matches somebody with somebody
Put in NaOH settled solutions, solution, NaOH concentration is 10mol/L；
(2) configuration Bi (NO3)3·5H2In O solution, solution, Bi (NO3)3·5H2O concentration is 0.15mol/L, and to molten
Appropriate nitric acid is instilled in liquid, Bi (NO are continued stirring until3)3·5H2O is completely dissolved, and obtains settled solution A；In this preferred embodiment
Nitric acid used is 1ml；
(3) with pipette by Ti (OC4H9)4It is added drop-wise in settled solution A, obtains mixed solution B, wherein Ti (OC4H9)4With
Bi (NO in step (2)3)3·5H2O mol ratio is 3:5；
(4) by after the mixed solution B magnetic agitations in step (3), then NaOH settled solutions are added dropwise to mixing dropwise
In solution B, then at being uniformly mixed at room temperature, the Na of microwave hydrothermal reaction is obtained0.5Bi0.5TiO3Precursor liquid；
(5) by Na resulting in step (4)0.5Bi0.5TiO3Precursor liquid is put into reactor, then reactor is put into micro-
Hydro-thermal reaction is carried out in ripple hydro-thermal parallel projects instrument, reaction temperature is 180 DEG C, and the reaction time is 25min, and reaction power is
360W；The filling rate of reactor is 36% in this preferred embodiment.
(6) treat that temperature is down to room temperature in microwave hydrothermal parallel projects instrument, when pressure is reduced to 0, reactor is taken out, by reactor
In sediment be first washed with deionized 5 times, then washed with absolute ethyl alcohol after 6 times, freeze-day with constant temperature carried out at 80 DEG C, 300 are crossed
Required cube Na is obtained after mesh sieve0.5Bi0.5TiO3Powder.
Example 5
It is quick under a kind of low temperature of the present invention to prepare cube Na0.5Bi0.5TiO3The method of powder, comprises the following steps, (1) matches somebody with somebody
Put in NaOH settled solutions, solution, NaOH concentration is 16mol/L；
(2) configuration Bi (NO3)3·5H2In O solution, solution, Bi (NO3)3·5H2O concentration is 0.1mol/L, and to molten
Appropriate nitric acid is instilled in liquid, Bi (NO are continued stirring until3)3·5H2O is completely dissolved, and obtains settled solution A；In this preferred embodiment
Nitric acid used is 2ml；
(3) with pipette by Ti (OC4H9)4It is added drop-wise in settled solution A, obtains mixed solution B, wherein Ti (OC4H9)4With
Bi (NO in step (2)3)3·5H2O mol ratio is 1:2；
(4) by after the mixed solution B magnetic agitations in step (3), then NaOH settled solutions are added dropwise to mixing dropwise
In solution B, then at being uniformly mixed at room temperature, the Na of microwave hydrothermal reaction is obtained0.5Bi0.5TiO3Precursor liquid；
(5) by Na resulting in step (4)0.5Bi0.5TiO3Precursor liquid is put into reactor, then reactor is put into micro-
Hydro-thermal reaction is carried out in ripple hydro-thermal parallel projects instrument, reaction temperature is 180 DEG C, and the reaction time is 20min；, reaction power is
360W；The filling rate of reactor is 36% in this preferred embodiment.
(6) treat that temperature is down to room temperature in microwave hydrothermal parallel projects instrument, when pressure is reduced to 0, reactor is taken out, by reactor
In sediment be first washed with deionized 5 times, then washed with absolute ethyl alcohol after 6 times, freeze-day with constant temperature carried out at 80 DEG C, 300 are crossed
Required cube Na is obtained after mesh sieve0.5Bi0.5TiO3Powder.
Product is subjected to the identification of phases by X-ray diffraction (XRD) analysis, the high Na of phase purity is obtained0.5Bi0.5TiO3Powder
Body, wherein, the Na when concentration of NaOH solution is 160.5Bi0.5TiO3Powder XRD spectrum is as shown in Figure 1.In above-mentioned NaOH solution
Concentration when taking 16, product is subjected to morphology observation by field emission scanning electron microscope (SEM), finally obtains and is evenly distributed
Cube Na0.5Bi0.5TiO3Powder, as shown in Figure 2.
Claims (10)
1. a kind of quick method for preparing cubic bismuth titanate sodium powder body under low temperature, it is characterised in that comprise the following steps,
Step (1), configuration concentration is 10~16mol/L NaOH settled solutions；
Step (2), configuration concentration is 0.1~0.2mol/L Bi (NO3)3·5H2O solution, and to Bi (NO3)3·5H2O solution
Middle instillation nitric acid, continues stirring until Bi (NO3)3·5H2O is completely dissolved, and obtains settled solution A；
Step (3), by Ti (OC4H9)4It is added drop-wise in settled solution A, mixed solution B, wherein Ti (OC is obtained after stirring4H9)4With
Bi (NO in step (2)3)3·5H2O mol ratio is 1:1~1:2；
Step (4), the NaOH settled solutions obtained in step (1) are added dropwise in mixed solution B, is uniformly mixed, obtains
Na0.5Bi0.5TiO3Precursor liquid；
Step (5), by Na resulting in step (4)0.5Bi0.5TiO3Precursor liquid carries out microwave hydrothermal reaction；
Step (6), microwave hydrothermal reaction terminates question response product and is cooled to after room temperature, by the washing of reacted sediment, constant temperature
A cube Na is obtained after dried and screened0.5Bi0.5TiO3Powder.
2. the quick method for preparing cubic bismuth titanate sodium powder body under a kind of low temperature according to claim 1, it is characterised in that
In described step (1), the concentration of NaOH settled solutions is 12~16mol/L.
3. the quick method for preparing cubic bismuth titanate sodium powder body under a kind of low temperature according to claim 1, it is characterised in that
In described step (2), the amount for adding nitric acid is 1~2mL.
4. the quick method for preparing cubic bismuth titanate sodium powder body under a kind of low temperature according to claim 1, it is characterised in that
In described step (4), NaOH settled solutions are added dropwise in mixed solution B dropwise, and breast is obtained after 0.2~1h of stirring is well mixed
The Na of white0.5Bi0.5TiO3Precursor liquid.
5. the quick method for preparing cubic bismuth titanate sodium powder body under a kind of low temperature according to claim 1, it is characterised in that
In described step (5), the reaction temperature of microwave hydrothermal reaction is 150~180 DEG C, and the reaction time is 20~30min.
6. the quick method for preparing cubic bismuth titanate sodium powder body under a kind of low temperature according to claim 1, it is characterised in that
In described step (5), microwave reaction power is 300~500W.
7. the quick method for preparing cubic bismuth titanate sodium powder body under a kind of low temperature according to claim 1, it is characterised in that
In described step (5), by Na resulting in step (4)0.5Bi0.5TiO3Precursor liquid is put into reactor, then by reactor
It is put into microwave hydrothermal parallel projects instrument and carries out hydro-thermal reaction.
8. the quick method for preparing cubic bismuth titanate sodium powder body under a kind of low temperature according to claim 7, it is characterised in that
Filling rate in described reactor is 35%~40%.
9. the quick method for preparing cubic bismuth titanate sodium powder body under a kind of low temperature according to claim 1, it is characterised in that
In step (6), treat that temperature is down to room temperature in microwave hydrothermal parallel projects instrument, when pressure is reduced to 0, reactor is taken out, by reactor
In sediment washed respectively with deionized water and absolute ethyl alcohol, obtain required powder after carrying out freeze-day with constant temperature, sieving.
10. the quick method for preparing cubic bismuth titanate sodium powder body, its feature under a kind of low temperature according to claim 1 or 9
It is, in described step (6), is first washed with deionized after 3~5 times and is washed again with absolute ethyl alcohol 4~6 times.
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| CN108660544A (en) * | 2018-03-30 | 2018-10-16 | 常州大学 | A kind of preparation method of semiconductor nano fiber |
| CN108341667B (en) * | 2018-03-30 | 2020-10-02 | 常州大学 | Preparation method of nano cubic ferroelectric material |
| CN108660544B (en) * | 2018-03-30 | 2020-10-02 | 常州大学 | Preparation method of semiconductor nano-fiber |
| CN109280975A (en) * | 2018-11-06 | 2019-01-29 | 湘潭大学 | A kind of bismuth sodium titanate nanometer line and preparation method thereof |
| CN110105064A (en) * | 2019-05-08 | 2019-08-09 | 陕西科技大学 | A kind of A compound ion Ferroelectrics fuel ceramic nano-powder body material preparation method and its application |
| CN110734086A (en) * | 2019-11-19 | 2020-01-31 | 湖南博深实业集团有限公司 | Preparation method of titanate based on electronic industry |
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