CN106478098A - A kind of microwave-hydrothermal method prepares tungsten bronze type nanometer Ba6FeNb9O30The method of powder - Google Patents
A kind of microwave-hydrothermal method prepares tungsten bronze type nanometer Ba6FeNb9O30The method of powder Download PDFInfo
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Abstract
A kind of microwave-hydrothermal method of the present invention prepares tungsten bronze type nanometer Ba6FeNb9O30The method of powder, which comprises the steps：(1) by Ba (NO3)2With Fe (NO3)3·9H2O is weighed respectively and is added in Enough Dl water, is stirred continuously until and is completely dissolved；(2) by the Fe (NO for preparing3)3The aqueous solution is added to Ba (NO3)2Solution colour is continued stirring until in the aqueous solution uniform, and instill 2～5 thereto and drip hydrogen peroxide, obtain mixed solution A；(3) by NbCl5Add in appropriate dilute hydrochloric acid solution, be stirred continuously until NbCl5It is completely dissolved；(4) NbCl will be contained again5Hydrochloric acid solution be added drop-wise in mixed solution A, mix and obtain mixed solution B；(5) dropping NaOH adjusts pH, forms Ba6Feb9O30Co-precipitation presoma；(6) microwave hydrothermal system is utilized, to the Ba for obtaining6FeNb9O30Precursor solution is heated, and obtains powder after reaction, and wash or centrifugal filtration post-drying after obtain nanoscale Ba6FeNb9O30Powder.
Description
Technical field
The present invention relates to wet chemistry method prepares nano-powder technology, specially a kind of microwave-hydrothermal method prepares tungsten bronze type and receives
Rice Ba6FeNb9O30The method of powder
Background technology
With the energy, increasingly the showing especially of environmental problem, the lead contamination caused after wherein scrapping because of leaded electronic material causes
Everybody attention, the therefore exploitation of unleaded dielectric substance have become as the focus of scholars' research.Tungsten bronze type structure
Dielectric substance, as the second big class dielectric material for being only second to perocskite type, with its excellent ferroelectricity, piezoelectricity, pyroelectricity and
The special performance of the aspects such as nonlinear optics and extensively application, gradually get growing concern for.Tungsten bronze type
Ba6FeNb9O30Pottery has quadratic tungsten bronze structure, there is similar giant dielectric effect in pottery, has one near room temperature
Individual huge dielectric constant platform, its dielectric constant is up to 103More than, and be lost relatively small.Tungsten bronze type Ba6FeNb9O30Pottery
A kind of relaxation ferroelectric, low-temperature dielectric behavior similar to relaxation ferroelectric, with strong frequency dispersion, high-temperature dielectric behavior
There is close relationship with high conductance.In addition, tungsten bronze type Ba6FeNb9O30Pottery also has certain ferromagnetism.Therefore, exist
Everyway is widely used.
So far, the method for preparing tungsten bronze type ceramic powder mainly has solid phase method and two kinds of liquid phase method, and solid phase method is
By starting oxides according to proportioning, then calcination forms ceramic powder at high temperature, and the method technique is simpler, also is adapted for big rule
Mould is produced, but the powder of this method synthesis is in irregular shape, and particle diameter distribution is uneven and comes it is difficult to obtain thinner particle
Meet the requirement of high-technology field.
Liquid phase method is also a kind of preparation method for generally adopting, but, reactant is typically added by existing liquid phase method
HTHP operation is carried out in water heating kettle, its preparation condition has high demands dangerous property, and experimental technique precision is big, during
Washing causes the operation cycle long, not easy to operate.
Content of the invention
For problems of the prior art, the present invention provides a kind of microwave-hydrothermal method and prepares tungsten bronze type nanometer
Ba6FeNb9O30The method of powder, the method process is simple, cycle is short and save energy, are obtained diameter of particle little and uniform.
The present invention is to be achieved through the following technical solutions：
A kind of microwave-hydrothermal method prepares tungsten bronze type nanometer Ba6FeNb9O30The method of powder, comprises the steps,
(1) by Ba (NO3)2With Fe (NO3)3·9H2O is 2 according to mol ratio:1～3:1 proportioning weighs and adds foot respectively
In amount deionized water, it is stirred continuously until to be completely dissolved and obtains the corresponding aqueous solution；
(2) by the Fe (NO for preparing3)3The aqueous solution adds Ba (NO3)2In the aqueous solution, continuously stirred uniform, and drip thereto
Enter 2～5 drop hydrogen peroxide, obtain mixed solution A；
(3) by NbCl5Add in appropriate dilute hydrochloric acid solution, be stirred continuously until NbCl5It is completely dissolved and obtains NbCl5's
Hydrochloric acid solution, wherein NbCl5Fe (NO with step (1)3)3·9H2The mol ratio of O is 1:1～1:2；
(4) again by NbCl5Hydrochloric acid solution be added drop-wise in mixed solution A, mix and obtain mixed solution B；
(5) 9.00～12.00 are adjusted to the pH of mixed solution B and obtain Ba6Feb9O30Precursor solution；
(6) microwave hydrothermal system is utilized, the mode using heating using microwave is to Ba6FeNb9O30Precursor solution is heated,
The powder that 1～1.5h of reaction is obtained at 200～240 DEG C, powder washed several times with water or centrifugal filtration post-drying obtain nanoscale
Ba6FeNb9O30Powder.
Preferably, in described step (1), the Ba (NO that obtains3)2Concentration of aqueous solution is 0.06～0.09mol/L.
Preferably, in described step (2), the concentration of hydrogen peroxide is 30%.
Preferably, in described step (2), Ba (NO3)2The aqueous solution and Fe (NO3)3When the mixed solution of the aqueous solution is stirred
Between be 1～2h.
Preferably, in described step (3), the concentration of watery hydrochloric acid is 1～3mol/L；NbCl5Dissolving stirring time
For 10～15h.
Preferably, in described step (3), the NbCl that obtains5Concentration of hydrochloric acid solution be 0.03～0.045mol/L.
Preferably, in described step (5), NbCl is added5Hydrochloric acid solution after, when mixed solution B is mixed, stirring
Time is 1～2h.
Preferably, in described step (5), adjust pH using drip sodium hydroxide solution by the way of, NaOH solution dense
Spend for 1～5mol/L；The titration speed of NaOH solution is 2～3mL/min.
Preferably, in described step (5), Ba6FeNb9O30Precursor solution is in uniform sepia.
Preferably, in described step (6), the washing times of material are 8～12 times；Or through 4～6 deionized waters from
Heart washing and filtration post-drying, wherein centrifugation rate are 3000～5000r/min, and the single spin time is 5～10min, dries
Temperature is 80～100 DEG C.
Compared with prior art, the present invention has following beneficial technique effect：
The present invention prepares tungsten bronze type nanometer Ba using microwave-hydrothermal method rapidly and efficiently6FeNb9O30Powder, different from
Toward traditional solid phase method, the method has more rapidly and efficiently and save energy.Compared to additive method is utilized, pass through
This controlled wet chemistry method prepares tungsten bronze type nanometer Ba6FeNb9O30Powder structure is stable, even particle distribution, the method
Reaction time also greatly shortens, and reaction temperature is greatly lowered, and the operation that powder need not be calcined in the later stage, and operates letter
Single, good process repeatability.So as to improve, the particle diameter distribution that is brought when conventional solid-state method prepares the powder is uneven, test week
The high and low shortcoming of sinterability of phase length, calcining heat.And prepare using water heating kettle in HTHP with existing liquid phase method
Under conditions of operation unlike, the present invention prepares tungsten bronze type nanometer Ba using microwave-hydrothermal method6FeNb9O30Powder, need not
HTHP, technological operation are safe and simple, and cycle is short, and the powder purity of preparation is high, and powder is uniform.Tungsten prepared by the method
Bronze type nanometer Ba6FeNb9O30Powder purity is high, and good dispersion is uniformly distributed in corynebacterium, rod length typically 300～
400nm, particle diameter distribution is typically in 20～50nm or so.Tungsten bronze type nanometer Ba prepared using the present invention6FeNb9O30Powder,
The crystallite dimension of later stage pottery not only can be reduced, and the dielectric properties of pottery and magnetic performance can be caused to obtain greatly
Improve, such as：Dielectric constant becomes big, and dielectric loss reduces, and ferromagnetism is improved so that the material is suitable for wider ring
Border condition, drastically increases its using value.
Further, dropping hydrogen peroxide makes powder granule evenly as accelerator and stabilizer.
Further, by controlling NbCl5Mixing time in hydrochloric acid solution so that NbCl5Can be completely dissolved, so as to
Improve the accuracy of stoichiometric proportion.
Further, by the mixing time of control mixed solution such that it is able to improve the uniformity of predecessor, so as to ensure
The purity of product.
Further, by controlling NbCl5Hydrochloric acid solution and NaOH solution drop rate, strengthen the powder granule to the present invention
The degree of controllability of pattern.
Further, reaction temperature of the present invention is low, without the need for calcining, energy saving, and obtained powder granule is uniform and is and receives
Meter level is other.
Description of the drawings
Fig. 1 is tungsten bronze type nanometer Ba prepared by present example 16FeNb9O30Powder X ray diffracting spectrum.
Fig. 2 is tungsten bronze type nanometer Ba prepared by present example 16FeNb9O30The scanning electron microscope image of powder.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail, described be explanation of the invention and
It is not to limit.
The invention provides a kind of microwave-hydrothermal method prepares tungsten bronze type Ba6FeNb9O30The method of nano-powder, technique letter
Single, reaction temperature is low, and the time is short, and powder, without the need for calcining again, the diameter of particle for can greatly save the energy, preparing is little, and changes
Metering is learned than controlled, to tungsten bronze type Ba6FeNb9O30It is a kind of excellent preparation method for nano-powder synthesis.Specifically such as
Following instance.
Example 1
A kind of microwave-hydrothermal method of the present invention prepares tungsten bronze type nanometer Ba6FeNb9O30The method of powder, including following step
Suddenly, (1) shifts to an earlier date the dilute hydrochloric acid solution that compound concentration is 1mol/L and the NaOH solution that concentration is 1mol/L, standby.By Ba (NO3)2
With Fe (NO3)3·9H2O is 2 according to mol ratio:1 proportioning is weighed respectively and is added in Enough Dl water, is stirred continuously until
It is completely dissolved and obtains the corresponding aqueous solution；Ba (the NO of gained3)2Concentration of aqueous solution is 0.06mol/L；
(2) by the Fe (NO for preparing3)3The aqueous solution adds the Ba (NO of gained3)2Solution colour is continued stirring until in the aqueous solution
Uniformly, 2 and are instilled thereto the hydrogen peroxide that concentration is 30% is dripped, mixed solution A is obtained, when mixing, mixing time is 1h.
(3) require quickly to weigh NbCl5, it is dissolved in the watery hydrochloric acid for preparing in advance, is sealed with horse back preservative film, juxtaposition
10h is stirred in magnetic stirring apparatus.By NbCl5Add in appropriate dilute hydrochloric acid solution, be stirred continuously until NbCl5It is completely dissolved,
Obtain NbCl5Concentration of hydrochloric acid solution be 0.03mol/L；Wherein NbCl5Fe (NO with step (1)3)3·9H2The mol ratio of O is
1:1；
(4) NbCl is dripped under stirring in mixed solution A5Hydrochloric acid solution, be sufficiently mixed uniform after mixed
Solution B is closed, mixing time is 1h.
(5) pH is adjusted by the way of dropping sodium hydroxide solution, with the NaOH solution titration mixing that concentration is 1mol/L
Solution B, control NaOH solution titration speed are 2mL/min, until the pH value of mixed solution B reaches 9.30, when produce sepia
Precipitation, forms Ba6Feb9O30Precursor solution.
(6) microwave hydrothermal system, Ba step (5) obtained using the mode of heating using microwave are utilized6FeNb9O30Presoma
Solution is heated, and reacts 1h, be cooled to room temperature after the completion of reaction at 200 DEG C；Take out reactor in material wash 8 times or
Centrifugation 4 times, single spin time are 5min, rotating speed 5000r/min, obtain final product tungsten bronze type nanometer in 80 DEG C of drying, 300 mesh sieves excessively
Ba6FeNb9O30Powder.
Product is carried out the identification of phases by X-ray diffraction (XRD) analysis, obtains the high tungsten bronze type nanometer of phase purity
Ba6FeNb9O30Powder, wherein, the Ba when pH value of mixed solution is 9.306FeNb9O30Nano-powder XRD spectrum such as Fig. 1 institute
Show.When above-mentioned pH value takes 9.30, product is carried out morphology observation by field emission scanning electron microscope (SEM), finally
To nanoscale, and the Ba of even particle distribution6FeNb9O30Nano-powder, as shown in Fig. 2 tungsten bronze type prepared by the method is received
Rice Ba6FeNb9O30Powder is uniformly distributed in corynebacterium, and, typically in 300～400nm, particle diameter distribution is typically in 50nm or so for rod length.
Example 2
A kind of microwave-hydrothermal method of the present invention prepares tungsten bronze type nanometer Ba6FeNb9O30The method of powder, including following step
Suddenly, (1) shifts to an earlier date the dilute hydrochloric acid solution that compound concentration is 3mol/L and the NaOH solution that concentration is 5mol/L, standby.By Ba (NO3)2
With Fe (NO3)3·9H2O is 3 according to mol ratio:1 proportioning is weighed respectively and is added in Enough Dl water, is stirred continuously until
It is completely dissolved and obtains the corresponding aqueous solution；Ba (the NO of gained3)2Concentration of aqueous solution is 0.09mol/L；
(2) by the Fe (NO for preparing3)3The aqueous solution adds the Ba (NO of gained3)2Solution colour is continued stirring until in the aqueous solution
Uniformly, 3 and are instilled thereto the hydrogen peroxide that concentration is 30% is dripped, mixed solution A is obtained, when mixing, mixing time is 2h.
(3) require quickly to weigh NbCl5, it is dissolved in the watery hydrochloric acid for preparing in advance, is sealed with horse back preservative film, juxtaposition
15h is stirred in magnetic stirring apparatus.By NbCl5Add in appropriate dilute hydrochloric acid solution, be stirred continuously until NbCl5It is completely dissolved,
Obtain NbCl5Concentration of hydrochloric acid solution be 0.04mol/L；Wherein NbCl5Fe (NO with step (1)3)3·9H2The mol ratio of O is
1:2；
(4) NbCl is dripped under stirring in mixed solution A5Hydrochloric acid solution, be sufficiently mixed uniform after mixed
Solution B is closed, mixing time is 2h.
(5) pH is adjusted by the way of dropping sodium hydroxide solution, with the NaOH solution titration mixing that concentration is 5mol/L
Solution B, control NaOH solution titration speed are 3mL/min, until the pH value of mixed solution B reaches 9.00, when produce sepia
Precipitation, forms comprising Ba6Feb9O30The Ba of co-precipitation presoma6Feb9O30Precursor solution.
(6) microwave hydrothermal system, Ba step (5) obtained using the mode of heating using microwave are utilized6FeNb9O30Presoma
Solution is heated, and reacts 1h, be cooled to room temperature after the completion of reaction at 220 DEG C；Take out reactor in material wash 9 times or
Centrifugation 6 times, single spin time are 10min, rotating speed 3000r/min, obtain final product tungsten bronze type and receive in 90 DEG C of drying, excessively 300 mesh sieves
Rice Ba6FeNb9O30Powder.
Example 3
A kind of microwave-hydrothermal method of the present invention prepares tungsten bronze type nanometer Ba6FeNb9O30The method of powder, including following step
Suddenly, (1) shifts to an earlier date the dilute hydrochloric acid solution that compound concentration is 1mol/L and the NaOH solution that concentration is 3mol/L, standby.By Ba (NO3)2
With Fe (NO3)3·9H2O is 2 according to mol ratio:1 proportioning is weighed respectively and is added in Enough Dl water, is stirred continuously until
It is completely dissolved and obtains the corresponding aqueous solution；Ba (the NO of gained3)2Concentration of aqueous solution is 0.08mol/L；
(2) by the Fe (NO for preparing3)3·9H2O adds the Ba (NO for being joined3)2Solution colour is continued stirring until in the aqueous solution
Uniformly, 5 and are instilled thereto the hydrogen peroxide that concentration is 30% is dripped, mixed solution A is obtained, when mixing, mixing time is
1.5h.
(3) require quickly to weigh NbCl5, it is dissolved in the watery hydrochloric acid for preparing in advance, is sealed with horse back preservative film, juxtaposition
12h is stirred in magnetic stirring apparatus.By NbCl5Add in appropriate dilute hydrochloric acid solution, be stirred continuously until NbCl5It is completely dissolved,
Obtain NbCl5Concentration of hydrochloric acid solution be 0.045mol/L；Wherein NbCl5Fe (NO with step (1)3)3·9H2The mol ratio of O
For 2:3；
(4) NbCl is dripped under stirring in mixed solution A5Hydrochloric acid solution, be sufficiently mixed uniform after mixed
Solution B is closed, mixing time is 1.5h.
(5) pH is adjusted by the way of dropping sodium hydroxide solution, with the NaOH solution titration mixing that concentration is 1mol/L
Solution B, control NaOH solution titration speed are 2mL/min, until the pH value of mixed solution B reaches 12.00, when produce sepia
Precipitation, forms Ba6Feb9O30Co-precipitation precursor solution.
(6) microwave hydrothermal system, Ba step (5) obtained using the mode of heating using microwave are utilized6FeNb9O30Presoma
Solution is heated, and reacts 1.5h, be cooled to room temperature after the completion of reaction at 240 DEG C；Take out the material washing 12 in reactor
Secondary or centrifugation 5 times, the single spin time be 8min, rotating speed 4000r/min, 100 DEG C dry, cross 300 mesh sieves obtain final product tungsten bronze
Type nanometer Ba6FeNb9O30Powder.
Claims (10)
1. a kind of microwave-hydrothermal method prepares tungsten bronze type nanometer Ba6FeNb9O30The method of powder, it is characterised in that including following step
Suddenly,
(1) by Ba (NO3)2With Fe (NO3)3·9H2O is 2 according to mol ratio:1～3:1 proportioning weighs and adds enough going respectively
In ionized water, it is stirred continuously until to be completely dissolved and obtains the corresponding aqueous solution；
(2) by the Fe (NO for preparing3)3The aqueous solution adds Ba (NO3)2In the aqueous solution, continuously stirred uniform, and instill 2～5 thereto
Drop hydrogen peroxide, obtains mixed solution A；
(3) by NbCl5Add in appropriate dilute hydrochloric acid solution, be stirred continuously until NbCl5It is completely dissolved and obtains NbCl5Hydrochloric acid
Solution, wherein NbCl5Fe (NO with step (1)3)3·9H2The mol ratio of O is 1:1～1:2；
(4) again by NbCl5Hydrochloric acid solution be added drop-wise in mixed solution A, mix and obtain mixed solution B；
(5) 9.00～12.00 are adjusted to the pH of mixed solution B and obtain Ba6Feb9O30Precursor solution；
(6) microwave hydrothermal system is utilized, the mode using heating using microwave is to Ba6FeNb9O30Precursor solution is heated, 200
The powder that 1～1.5h of reaction is obtained at～240 DEG C, powder washed several times with water or centrifugal filtration post-drying obtain nanoscale
Ba6FeNb9O30Powder.
2. a kind of microwave-hydrothermal method according to claim 1 prepares tungsten bronze type nanometer Ba6FeNb9O30The method of powder, its
It is characterised by, in described step (1), the Ba (NO that obtains3)2Concentration of aqueous solution is 0.06～0.09mol/L.
3. a kind of microwave-hydrothermal method according to claim 1 prepares tungsten bronze type nanometer Ba6FeNb9O30The method of powder, its
It is characterised by, in described step (2), the concentration of hydrogen peroxide is 30%.
4. a kind of microwave-hydrothermal method according to claim 1 prepares tungsten bronze type nanometer Ba6FeNb9O30The method of powder, its
It is characterised by, in described step (2), Ba (NO3)2The aqueous solution and Fe (NO3)3The mixed solution mixing time of the aqueous solution be 1～
2h.
5. a kind of microwave-hydrothermal method according to claim 1 prepares tungsten bronze type nanometer Ba6FeNb9O30The method of powder, its
It is characterised by, in described step (3), the concentration of watery hydrochloric acid is 1～3mol/L；NbCl5Dissolving stirring time be 10～
15h.
6. a kind of microwave-hydrothermal method according to claim 1 prepares nanometer Ba6FeNb9O30The method of powder, its feature exist
In, in described step (3), the NbCl that obtains5Concentration of hydrochloric acid solution be 0.03～0.045mol/L.
7. a kind of microwave-hydrothermal method according to claim 1 prepares tungsten bronze type nanometer Ba6FeNb9O30The method of powder, its
It is characterised by, in described step (5), adds NbCl5Hydrochloric acid solution after, when mixed solution B is mixed, mixing time is
1～2h.
8. a kind of microwave-hydrothermal method according to claim 1 prepares tungsten bronze type nanometer Ba6FeNb9O30The method of powder, its
Be characterised by, in described step (5), by the way of adjusting pH using dropping sodium hydroxide solution, the concentration of NaOH solution for 1～
5mol/L；The titration speed of NaOH solution is 2～3mL/min.
9. a kind of microwave-hydrothermal method according to claim 1 prepares tungsten bronze type nanometer Ba6FeNb9O30The method of powder, its
It is characterised by, in described step (5), Ba6FeNb9O30Precursor solution is in uniform sepia.
10. a kind of microwave-hydrothermal method according to claim 1 prepares nanometer Ba6FeNb9O30The method of powder, its feature exist
In, in described step (6), the washing times of material are 8～12 times；Or through 4～6 deionized water centrifuge washings and filtration
Post-drying, wherein centrifugation rate are 3000～5000r/min, and the single spin time is 5～10min, and drying temperature is 80～100
℃.
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| CN107235725A (en) * | 2017-05-11 | 2017-10-10 | 陕西科技大学 | Tungsten bronze sections barium tantalate powder and method prepared by a kind of coprecipitation |
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