CN107055597B - The method of cubic bismuth titanate sodium powder body is quickly prepared under a kind of low temperature - Google Patents
The method of cubic bismuth titanate sodium powder body is quickly prepared under a kind of low temperature Download PDFInfo
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The present invention provides a kind of method that cubic bismuth titanate sodium powder body is quickly prepared under low temperature, includes the following steps, step (1), and configuration concentration is the NaOH clear solution of 10~16mol/L；Step (2), configuration concentration are the Bi (NO of 0.1~0.2mol/L3)3·5H2O solution obtains clear solution A；Step (3), by Ti (OC4H9)4It is added drop-wise in clear solution A, mixed solution B is obtained after stirring；Step (4), NaOH clear solution is added dropwise in mixed solution B, is 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 terminate after reaction product is cooled to room temperature, will obtain a cube Na after sediment washing, freeze-day with constant temperature and the sieving after reaction0.5Bi0.5TiO3Powder.
Description
Technical field
The present invention relates to wet chemistry methods to prepare powder technology, quickly prepares cubic bismuth titanate sodium powder under specially a kind of low temperature
The method of body.
Background technique
Piezoelectric ceramics suffers from extensively as a kind of important ceramic material in fields such as machinery, electronics, space flight and aviation
General application.Currently, the piezoelectric ceramics used is concentrated mainly in the material of lead base, the content of PbO accounts for about material in this material
Expect 70% or so of total amount.PbO is a kind of harmful substance, material preparation, use and discard after treatment process in ring
Border and human body all generate harm.Therefore, develop novel, function admirable, in accordance with natural environment leadless piezoelectric ceramics at
For a research topic that is urgent and having important practical significance.Bismuth-sodium titanate (Na0.5Bi0.5TiO3) (NBT) be a kind of A multiple
The ferroelectric material of the perovskite structure in conjunction generation, NBT have stronger ferroelectricity, cause numerous scholars with its excellent performance
Concern, it is considered to be one of most promising candidate material of leadless piezoelectric ceramics.
The preparation of NBT is all prepared using conventional solid-state method mostly, and this method technique is simpler, is also suitble to large-scale production,
But there are synthesis temperatures that ceramics high, easy to reunite and being difficult to obtain thinner particle, while being burnt into exist is fine and close for conventional solid-state method
The requirement that property is poor, sample sintering temperature is excessively high and excessively recrystallizes without being able to satisfy high-technology field.It is compared with other methods,
Microwave heating is interior heating, can greatly save energy, and microwave heating starts microwave convenient for control, immediately with reactor
Interior material effect, carries out hydro-thermal reaction, closes microwave, and reaction stops quickly, and hysteresis effect is small.Microwave, which accelerates, simultaneously reacted
Journey can quickly prepare the uniform powder of complete crystallization, particle diameter distribution so that the reaction time shortens.This method has preparation
Simple process, without calcining, powder the series of advantages such as purity is high and be widely used, and reaction temperature is lower.
Summary of the invention
Aiming at the problems existing in 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 be water, highly-safe, simple process, using microwave heating make reaction it is more full and uniform, heating
Faster, the period is short, and reaction temperature is lower and saves the energy, be made powder grain development is complete, particle diameter distribution uniformly and purity compared with
It is high.
The present invention is to be achieved through the following technical solutions:
A kind of method that cubic bismuth titanate sodium powder body is quickly prepared under low temperature, includes the following steps,
Step (1), configuration concentration are the NaOH clear solution of 10~16mol/L；
Step (2), configuration concentration are the Bi (NO of 0.1~0.2mol/L3)3·5H2O solution, and to Bi (NO3)3·5H2O
Nitric acid is instilled in solution, continues stirring until Bi (NO3)3·5H2O is completely dissolved, and obtains clear solution A；
Step (3), by Ti (OC4H9)4It is added drop-wise in clear solution A, mixed solution B is obtained after stirring, wherein Ti
(OC4H9)4With Bi (NO in step (2)3)3·5H2The molar ratio of O is 1:1~1:2；
NaOH clear solution obtained in step (1) is added dropwise in mixed solution B, is uniformly mixed by step (4),
Obtain Na0.5Bi0.5TiO3Precursor liquid；
Step (5), by obtained Na in step (4)0.5Bi0.5TiO3Precursor liquid carries out microwave hydrothermal reaction；
Step (6), microwave hydrothermal reaction terminate after reaction product is cooled to room temperature, the sediment after reaction is washed,
A cube Na is obtained after freeze-day with constant temperature and sieving0.5Bi0.5TiO3Powder.
Preferably, in the step (1), the concentration of NaOH clear solution is 12~16mol/L.
Preferably, in the step (2), the amount that nitric acid is added is 1~2mL.
Preferably, in the step (4), NaOH clear solution is added dropwise to dropwise in mixed solution B, stirs 0.2~1h
Milky Na is obtained after mixing0.5Bi0.5TiO3Precursor liquid.
Preferably, in the step (5), the reaction temperature of microwave hydrothermal reaction is 150~180 DEG C, and the reaction time is
20~30min.
Preferably, in the step (5), microwave reaction power is 300~500W.
Preferably, in the step (5), by obtained Na in step (4)0.5Bi0.5TiO3Precursor liquid is put into reaction
In kettle, then reaction kettle is put into microwave hydrothermal parallel projects instrument and carries out hydro-thermal reaction.
Further, the filling rate in the reaction kettle is 35%~40%.
Preferably, in step (6), it is down to room temperature to temperature in microwave hydrothermal parallel projects instrument, when pressure is reduced to 0, is taken out
Reaction kettle washs the deionized water of the sediment in reaction kettle and dehydrated alcohol respectively, obtains after carrying out freeze-day with constant temperature, sieving
Required powder.
Further, in the step (6), 4~6 are washed with dehydrated alcohol again after being first washed with deionized 3~5 times
It is secondary.
Compared with prior art, the invention has the following beneficial technical effects:
The present invention quickly prepares cubic bismuth titanate sodium powder body using method rapidly and efficiently at low temperature, different from the past
Traditional solid phase method, this method have the advantages that more rapidly and efficiently and save the energy.Compared to other methods are utilized, pass through this
Cube Na of the controllable wet chemistry method preparation of kind0.5Bi0.5TiO3Powder purity height, powder granule narrow size distribution and powder granule
Size is controllable, crystal form is good, and this method prepare powder needed for the reaction time be greatly shortened, reaction temperature reduces, and is easy to get
To suitable stoichiometry object, high-temperature calcination and ball milling are eliminated, so as to avoid impurity and fault of construction, and operates letter
Single, good process repeatability has the characteristics that low power consuming, pollution is small, yield is more with high investment less.Microwave-hydrothermal method is used simultaneously
When, microwave energy plays oscillation action to reaction solution, effectively promotes reaction and improves powder grain quality, reduces the group of particle
It is poly-.Brought particle diameter distribution is uneven when preparing the powder so as to improve conventional solid-state method, sample calcination temperature is excessively high, easy
Reunite, the disadvantages of experimental period is long.Cube Na of this method preparation0.5Bi0.5TiO3Powder structure is stablized, even particle distribution,
Purity is higher, is uniformly distributed in cube.
Further, by controlling NaOH solution drop rate, and deionization is washed and first used to the multiple of sediment
It is washed again with dehydrated alcohol after water washing, improves the purity of sample, reduce the reunion of sample, strengthened to powder of the 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, to guarantee 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, and without calcining, yield is more with high investment less, and powder obtained is uniformly distributed.
Detailed description of the invention
Fig. 1 is cube Na of present example preparation0.5Bi0.5TiO3Powder X ray diffracting spectrum.
Fig. 2 is cube Na of present example preparation0.5Bi0.5TiO3The scan image of powder.
Specific embodiment
Below 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.
The present invention provides quickly prepare a cube Na under a kind of low temperature0.5Bi0.5TiO3The method of powder, simple process, weight
Renaturation is good, and reaction temperature is low, and the time is short, and powder no longer needs to calcine, and yield is with high investment few, can greatly save the energy, preparation
Powder purity it is high, and stoichiometric ratio is controllable, to Na0.5Bi0.5TiO3It is a kind of excellent preparation method for powder synthesis.
Specific such as following instance.
Example 1
The method that cubic bismuth titanate sodium powder body is quickly prepared under a kind of low temperature of the present invention, includes the following steps,
(1) NaOH clear solution is configured, in solution, the concentration of NaOH is 12mol/L；
(2) Bi (NO is configured3)3·5H2O solution, in solution, Bi (NO3)3·5H2The concentration of O is 0.1mol/L, and to molten
Suitable nitric acid is instilled in liquid, continues stirring until Bi (NO3)3·5H2O is completely dissolved, and obtains clear solution A；In this preferred embodiment
Nitric acid used is 1ml；
(3) with pipette by Ti (OC4H9)4It is added drop-wise in clear solution A, obtains mixed solution B, wherein Ti (OC4H9)4With
Bi (NO in step (2)3)3·5H2The molar ratio of O is 1:1；
(4) by after the mixed solution B magnetic agitation in step (3), then NaOH clear solution is 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 obtained Na in step (4)0.5Bi0.5TiO3Precursor liquid is put into reaction kettle, then reaction kettle is put into micro-
Hydro-thermal reaction is carried out in wave hydro-thermal parallel projects instrument, reaction temperature is 160 DEG C, reaction time 30min, and reaction power is
500W；The filling rate of reaction kettle is 35% in this preferred embodiment.
(6) it is down to room temperature to temperature in microwave hydrothermal parallel projects instrument, when pressure is reduced to 0, reaction kettle is taken out, by reaction kettle
In sediment be washed with deionized 3 times, then after washing 4 times with dehydrated alcohol, freeze-day with constant temperature is carried out at 80 DEG C, crosses 300
Cube Na required for being obtained after mesh0.5Bi0.5TiO3Powder.
Example 2
The method that cubic bismuth titanate sodium powder body is quickly prepared under a kind of low temperature of the present invention, includes the following steps,
(1) NaOH clear solution is configured, in solution, the concentration of NaOH is 14mol/L；
(2) Bi (NO is configured3)3·5H2O solution, in solution, Bi (NO3)3·5H2The concentration of O is 0.2mol/L, and to molten
Suitable nitric acid is instilled in liquid, continues stirring until Bi (NO3)3·5H2O is completely dissolved, and obtains clear solution A；In this preferred embodiment
Nitric acid used is 2ml；
(3) with pipette by Ti (OC4H9)4It is added drop-wise in clear solution A, obtains mixed solution B, wherein Ti (OC4H9)4With
Bi (NO in step (2)3)3·5H2The molar ratio of O is 1:1.5；
(4) by after the mixed solution B magnetic agitation in step (3), then NaOH clear solution is 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 obtained Na in step (4)0.5Bi0.5TiO3Precursor liquid is put into reaction kettle, then reaction kettle is put into micro-
Hydro-thermal reaction is carried out in wave hydro-thermal parallel projects instrument, reaction temperature is 180 DEG C, reaction time 30min, and reaction power is
400W；The filling rate of reaction kettle is 40% in this preferred embodiment.
(6) it is down to room temperature to temperature in microwave hydrothermal parallel projects instrument, when pressure is reduced to 0, reaction kettle is taken out, by reaction kettle
In sediment be first washed with deionized 4 times, then carry out freeze-day with constant temperature after washing 4 times with dehydrated alcohol, at 80 DEG C, cross 300
Cube Na required for being obtained after sieve0.5Bi0.5TiO3Powder.
Example 3
A cube Na is quickly prepared under a kind of low temperature of the present invention0.5Bi0.5TiO3The method of powder, includes the following steps, (1) matches
Set NaOH clear solution, in solution, the concentration of NaOH is 15mol/L；
(2) Bi (NO is configured3)3·5H2O solution, in solution, Bi (NO3)3·5H2The concentration of O is 0.1mol/L, and to molten
Suitable nitric acid is instilled in liquid, continues stirring until Bi (NO3)3·5H2O is completely dissolved, and obtains clear solution A；In this preferred embodiment
Nitric acid used is 1.5ml；
(3) with pipette by Ti (OC4H9)4It is added drop-wise in clear solution A, obtains mixed solution B, wherein Ti (OC4H9)4With
Bi (NO in step (2)3)3·5H2The molar ratio of O is 3:4；
(4) by after the mixed solution B magnetic agitation in step (3), then NaOH clear solution is 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 obtained Na in step (4)0.5Bi0.5TiO3Precursor liquid is put into reaction kettle, then reaction kettle is put into micro-
Hydro-thermal reaction is carried out in wave hydro-thermal parallel projects instrument, reaction temperature is 180 DEG C, reaction time 20min, and reaction power is
300W；The filling rate of reaction kettle is 36% in this preferred embodiment.
(6) it is down to room temperature to temperature in microwave hydrothermal parallel projects instrument, when pressure is reduced to 0, reaction kettle is taken out, by reaction kettle
In sediment be first washed with deionized 4 times, then carry out freeze-day with constant temperature after washing 4 times with dehydrated alcohol, at 80 DEG C, cross 300
Cube Na required for being obtained after mesh0.5Bi0.5TiO3Powder.
Example 4
A cube Na is quickly prepared under a kind of low temperature of the present invention0.5Bi0.5TiO3The method of powder, includes the following steps, (1) matches
Set NaOH clear solution, in solution, the concentration of NaOH is 10mol/L；
(2) Bi (NO is configured3)3·5H2O solution, in solution, Bi (NO3)3·5H2The concentration of O is 0.15mol/L, and to molten
Suitable nitric acid is instilled in liquid, continues stirring until Bi (NO3)3·5H2O is completely dissolved, and obtains clear solution A；In this preferred embodiment
Nitric acid used is 1ml；
(3) with pipette by Ti (OC4H9)4It is added drop-wise in clear solution A, obtains mixed solution B, wherein Ti (OC4H9)4With
Bi (NO in step (2)3)3·5H2The molar ratio of O is 3:5；
(4) by after the mixed solution B magnetic agitation in step (3), then NaOH clear solution is 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 obtained Na in step (4)0.5Bi0.5TiO3Precursor liquid is put into reaction kettle, then reaction kettle is put into micro-
Hydro-thermal reaction is carried out in wave hydro-thermal parallel projects instrument, reaction temperature is 180 DEG C, reaction time 25min, and reaction power is
360W；The filling rate of reaction kettle is 36% in this preferred embodiment.
(6) it is down to room temperature to temperature in microwave hydrothermal parallel projects instrument, when pressure is reduced to 0, reaction kettle is taken out, by reaction kettle
In sediment be first washed with deionized 5 times, then carry out freeze-day with constant temperature after washing 6 times with dehydrated alcohol, at 80 DEG C, cross 300
Cube Na required for being obtained after mesh0.5Bi0.5TiO3Powder.
Example 5
A cube Na is quickly prepared under a kind of low temperature of the present invention0.5Bi0.5TiO3The method of powder, includes the following steps, (1) matches
Set NaOH clear solution, in solution, the concentration of NaOH is 16mol/L；
(2) Bi (NO is configured3)3·5H2O solution, in solution, Bi (NO3)3·5H2The concentration of O is 0.1mol/L, and to molten
Suitable nitric acid is instilled in liquid, continues stirring until Bi (NO3)3·5H2O is completely dissolved, and obtains clear solution A；In this preferred embodiment
Nitric acid used is 2ml；
(3) with pipette by Ti (OC4H9)4It is added drop-wise in clear solution A, obtains mixed solution B, wherein Ti (OC4H9)4With
Bi (NO in step (2)3)3·5H2The molar ratio of O is 1:2；
(4) by after the mixed solution B magnetic agitation in step (3), then NaOH clear solution is 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 obtained Na in step (4)0.5Bi0.5TiO3Precursor liquid is put into reaction kettle, then reaction kettle is put into micro-
Hydro-thermal reaction is carried out in wave hydro-thermal parallel projects instrument, reaction temperature is 180 DEG C, reaction time 20min；, reaction power is
360W；The filling rate of reaction kettle is 36% in this preferred embodiment.
(6) it is down to room temperature to temperature in microwave hydrothermal parallel projects instrument, when pressure is reduced to 0, reaction kettle is taken out, by reaction kettle
In sediment be first washed with deionized 5 times, then carry out freeze-day with constant temperature after washing 6 times with dehydrated alcohol, at 80 DEG C, cross 300
Cube Na required for being obtained after mesh0.5Bi0.5TiO3Powder.
Product is subjected to the identification of phases by X-ray diffraction (XRD) analysis, obtains the Na of mutually purity is high0.5Bi0.5TiO3Powder
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 (6)
1. quickly preparing the method for cubic bismuth titanate sodium powder body under a kind of low temperature, which is characterized in that include the following steps,
Step (1), configuration concentration are the NaOH clear solution of 14~16mol/L；
Step (2), configuration concentration are the Bi (NO of 0.1~0.2mol/L3)3·5H2O solution, and to Bi (NO3)3·5H2O solution
The middle nitric acid for instilling 1~2mL, continues stirring until Bi (NO3)3·5H2O is completely dissolved, and obtains clear solution A；
Step (3), by Ti (OC4H9)4It is added drop-wise in clear solution A, mixed solution B is obtained after stirring, wherein Ti (OC4H9)4With
Bi (NO in step (2)3)3·5H2The molar ratio of O is 1:1~1:2；
NaOH clear solution obtained in step (1) is added dropwise in mixed solution B, is uniformly mixed, obtains by step (4)
Na0.5Bi0.5TiO3Precursor liquid；
Step (5), by obtained Na in step (4)0.5Bi0.5TiO3Precursor liquid under the microwave reaction power of 300~500W into
The reaction of row microwave hydrothermal, reaction temperature are 150~180 DEG C, and the reaction time is 20~30min；
Step (6), microwave hydrothermal reaction terminate after reaction product is cooled to room temperature, by the sediment washing after reaction, constant temperature
A cube Na is obtained after dried and screened0.5Bi0.5TiO3Powder.
2. quickly preparing the method for cubic bismuth titanate sodium powder body under a kind of low temperature according to claim 1, which is characterized in that
In the step (4), NaOH clear solution is added dropwise to dropwise in mixed solution B, and 0.2~1h of stirring obtains cream after mixing
The Na of white0.5Bi0.5TiO3Precursor liquid.
3. quickly preparing the method for cubic bismuth titanate sodium powder body under a kind of low temperature according to claim 1, which is characterized in that
In the step (5), by obtained Na in step (4)0.5Bi0.5TiO3Precursor liquid is put into reaction kettle, then by reaction kettle
It is put into microwave hydrothermal parallel projects instrument and carries out hydro-thermal reaction.
4. quickly preparing the method for cubic bismuth titanate sodium powder body under a kind of low temperature according to claim 3, which is characterized in that
Filling rate in the reaction kettle is 35%~40%.
5. quickly preparing the method for cubic bismuth titanate sodium powder body under a kind of low temperature according to claim 1, which is characterized in that
In step (6), it is down to room temperature to temperature in microwave hydrothermal parallel projects instrument, when pressure is reduced to 0, reaction kettle is taken out, by reaction kettle
In sediment deionized water and dehydrated alcohol wash respectively, carry out freeze-day with constant temperature, obtain required powder after sieving.
6. a kind of method for quickly preparing cubic bismuth titanate sodium powder body under low temperature according to claim 1 or 5, feature exist
In being first washed with deionized after 3~5 times and washed 4~6 times with dehydrated alcohol again in the step (6).
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| 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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