CN103449510A - Submicron barium titanate crystal and preparation method thereof - Google Patents
Submicron barium titanate crystal and preparation method thereof Download PDFInfo
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- CN103449510A CN103449510A CN2013101206929A CN201310120692A CN103449510A CN 103449510 A CN103449510 A CN 103449510A CN 2013101206929 A CN2013101206929 A CN 2013101206929A CN 201310120692 A CN201310120692 A CN 201310120692A CN 103449510 A CN103449510 A CN 103449510A
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- titanate crystal
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Abstract
The invention discloses a submicron barium titanate crystal and a preparation method thereof. The preparation method comprises the following steps: mixing barium peroxide with titanium dioxide according to a mol ratio of being not smaller than 1, and carrying out a heat reaction to obtain a reaction product; and successively pickling and drying the reaction product to obtain the submicron barium titanate crystal. The preparation method of the submicron barium titanate crystal is relatively low in preparation temperature, liable easy to control conditions, simple in process, low in requirements on equipment, low in cost and suitable for industrialized production. The submicron barium titanate crystal prepared by the preparation method is of a single-phase tetragonal structure and is good in crystallinity, high in purity and narrow in particle diameter distribution.
Description
Technical field
The invention belongs to the superfine powdery material field, relate in particular to a kind of submicron barium titanate crystal and preparation method thereof.
Background technology
Barium titanate (BaTiO
3) good physicochemical property are arranged, such as character such as: catalysis, gas sensing, ferroelectric, thermoelectricity, piezoelectricity, nonlinear optics, electrical-optical conversions, be widely used in a lot of fields.As everyone knows, the performance of barium titanate powder, depend on some factors of their phase, crystalline size, lattice defect and surface interface, and these all depend on preparation method and reaction conditions.Therefore, Many researchers all is devoted to design the synthetic route of a novelty, with this, synthesizes the barium titanate crystal that controlled phase and good distribution of sizes are arranged, and improves the chemistry of barium titanate crystal and the performance of physics.
Up to the present, the preparation of barium titanate crystal is mainly by solid reaction process, sol-gel method and hydrothermal method.In traditional solid phase synthesis process, barium titanate crystal normally passes through TiO
2and BaCO
3mechanically mixing, at sintering more than 1000 ℃ and.Yet the particle obtained in this way is some bad feature usually, such as: particle shape irregular, size distribution is wider, component inhomogeneous, foreign matter content is high.With traditional solid-phase synthesis, compare, although sol-gel method provides a new method, under cold condition, the synthetic barium titanate crystal that higher degree, nano-scale are arranged, but they have not only consumed more expensive chemical reagent, and in order to decompose completely Gel Precursor, need to carry out sintering more than 700 ℃, making unbodied product crystallization and remove impurity.Hydrothermal synthesis method, in autoclave, under the condition of 300 ℃, prepared the barium titanate nano particle of high crystalline, high purity, homogeneous, and it has opened up a new synthetic method undoubtedly.Yet the synthetic barium titanate nano particle of hydrothermal method is a metastable Emission in Cubic normally, make metastable Emission in Cubic be transformed into Tetragonal, also need to heat-treat 1000 ℃ of left and right.Otherwise, in sintered multilayer ceramic capacitor, the OH ion due to residual in their crystalline structure, will form harmful vesicular structure.In addition, traditional hydrothermal method needs the reaction times very long.
In sum, in order to realize industrial production, require under alap temperature condition, by a kind of technique, method simple, with low cost prepares single-phase, good crystallinity, highly purified barium titanate crystal particle.
Summary of the invention
The object of the invention is to overcome the above-mentioned deficiency of prior art, the preparation method of a kind of single-phase, good crystallinity, submicron barium titanate crystal that purity is high is provided, temperature of reaction is low, technique is simple and cost is low.
Another object of the present invention is to provide a kind of single-phase, good crystallinity, submicron barium titanate crystal that purity is high.
In order to realize the foregoing invention purpose, technical scheme of the present invention is as follows:
A kind of preparation method of submicron barium titanate crystal comprises the following steps:
By after barium peroxide and titanium dioxide in molar ratio >=1 combination treatment, carry out thermal response, obtain reaction product;
Described reaction product is carried out to pickling successively, and drying treatment, obtain the submicron barium titanate crystal.
And, a kind of submicron barium titanate crystal, described submicron barium titanate crystal is formed by the preparation method of above-mentioned submicron barium titanate crystal, and described submicron barium titanate crystal structure is Tetragonal.
In the preparation method's of above-mentioned submicron barium titanate crystal heat treatment process, barium peroxide (BaO
2) melting, effectively increased itself and solid-phase reactant titanium dioxide (TiO
2) contact area, even both still have higher reactive behavior under relatively low temperature of reaction.Simultaneously, BaO
2with TiO
2the consumption specific energy guarantee TiO
2complete reaction, obtain highly purified BaTiO
3.The submicron barium titanate crystal made by the method is that single-phase, good crystallinity, purity are high, and its preparation temperature is relatively low, and condition is easily controlled, and technique is simple, and not high to equipment requirements, cost is low, is suitable for suitability for industrialized production.
Above-mentioned submicron barium titanate crystal, its crystalline structure is single-phase Tetragonal, good crystallinity, purity is high, and narrow diameter distribution all improves to some extent the chemical physics performances such as it is ferroelectric, thermoelectricity, piezoelectricity, nonlinear optics, electrical-optical conversion.
The accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further described, in accompanying drawing:
The process flow sheet that Fig. 1 is embodiment of the present invention submicron barium titanate crystal preparation method;
The X-ray diffractogram (XRD) that Fig. 2-1 is the presoma of preparation in embodiment 1 step (1);
The scanning electron microscope (SEM) photograph (SEM) that Fig. 2-2 are the presoma of preparation in embodiment 1 step (1);
The XRD figure of reaction product a in the corresponding embodiment 1～3 of (a)～(f) spectrogram difference in Fig. 3-1, final product b, reaction product c, final product d, reaction product e, final product f;
The XPS figure that Fig. 3-2 are the final product f of preparation in embodiment 3;
The SEM figure that Fig. 3-3 are the final product f of preparation in embodiment 3.
Embodiment
In order to make the technical problem to be solved in the present invention, technical scheme and beneficial effect clearer, below in conjunction with embodiment and accompanying drawing, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
The embodiment of the present invention provides the preparation method of a kind of single-phase, good crystallinity, submicron barium titanate crystal that purity is high, and temperature of reaction is low, technique is simple and cost is low.The preparation method's of this submicron barium titanate crystal process flow sheet as shown in Figure 1, comprises the following steps:
Step S01. barium peroxide and titanium dioxide carry out thermal response: by after barium peroxide and titanium dioxide in molar ratio >=1 combination treatment, carry out thermal response, obtain reaction product;
Step S02. carries out pickling, drying treatment successively by reaction product: the reaction product in step S01 is carried out to pickling successively, and drying treatment, obtain the submicron barium titanate crystal.
Particularly, in the thermal response step of step S01, between barium peroxide and titanium dioxide, in heat treated process, react.The contriver studies discovery, and usage ratio and the level of response of barium peroxide and titanium dioxide are closely related, causes the by product difference generated, and makes the complexity of removing impurity in product also different, finally the purity of barium titanate is had to material impact.Particularly, when the thermal response temperature is raised to more than 450 ℃, BaO
2to be melted into liquid state, there is very high reactive behavior, and can be in heat treatment process subsequently, soon and TiO
2the submicron particles reaction generates BaTiO
3and Ba
2tiO
4.Meanwhile, a small amount of BaO
2may be also and airborne CO
2reaction, generate solid phase impurity B aCO
3.But, the impurity B a in product
2tiO
4and BaCO
3can remove by pickling.In addition, bibliographical information BaO was once arranged
2h
2o
2there is thermolability, when 100 ℃ of left and right, resolve into BaO
2, H
2o, O
2.Therefore, if adopt the barium peroxide crystal, the generation that also can cause the by products such as steam and oxygen to generate.Therefore, in the thermal process reactor in above-mentioned steps S01, may there is following chemical reaction:
BaO
2·H
2O
2=BaO
2+H
2O+1/2O
2
BaO
2+TiO
2=BaTiO
3+1/2O
2
2BaO
2+TiO
2=Ba
2TiO
4+O
2
BaO
2+CO
2=BaCO
3+1/2O
2
Ba
2TiO
4+4HNO
3=2Ba(NO
3)
2+H
4TiO
4
BaCO
3+2HNO
3=Ba(NO
3)
2+H
2O+CO
2
Thus, when the barium peroxide consumption is not enough, may cause TiO
2can not be by complete reaction, therefore, products therefrom is BaTiO
3, Ba
2tiO
4, TiO
2and BaCO
3mixture, again due to TiO
2chemical stability strong, acid-fast alkali-proof, the product after pickling still contains TiO
2.When adding excessive barium peroxide, products therefrom is BaTiO
3, Ba
2tiO
4and BaCO
3mixture; Obtain highly purified BaTiO after pickling
3crystal.Therefore, add excessive barium peroxide can guarantee TiO
2complete reaction generates BaTiO
3, Ba
2tiO
4and BaCO
3, more just can obtain highly purified BaTiO by purification process
3particle, because by product Ba
2tiO
4and BaCO
3than reactant TiO
2more easily from the finished product, remove.But the barium peroxide of too many amount has not only increased preparation BaTiO
3the cost of crystal, also can cause purification process after the thermal response pressure as pickling work, and therefore, as preferred embodiment, barium peroxide and titanium dioxide mol ratio are 1:(0.8～1).As another preferred embodiment, in the thermal response step of step S01, the thermal response temperature is 600～800 ℃, and the thermal response time is 8～12h.Further preferably, the thermal response temperature is 700 ℃, and the thermal response time is 10h.BaO
2be melted into liquid in the time of about 450 ℃, when approaching 800 ℃, will resolve into BaO and O
2.Thereby, in above-mentioned range of reaction temperature, reactant B aO
2liquefy, when participating in reaction, improve widely the contact area with other solid-phase reactants, and then also improved speed of reaction, the performance that is conducive to reduce temperature of reaction and improves product.
In another is preferably implemented, in the thermal response step of step S01, be that the temperature rise rate with 12～16 ℃/min is heated to described thermal response temperature.14 ℃/min more preferably.In the process that is heated to described thermal response temperature, the crystallization again of barium peroxide and titanium dioxide, with above-mentioned preferred temperature rise rate heating, more easily form tiny and the uniform barium peroxide of size distribution and titanium dioxide crystal particle, thereby reaction generates the uniform barium titanate crystal particle of size distribution.
In the thermal response of above-mentioned steps S01, barium peroxide can be directly commercial, also can be prepared as follows, to obtain highly purified barium peroxide:
Bariumchloride is dissolved in superoxol, drips ammoniacal liquor, the pH value of regulating mixing solutions is 7～9, carries out precipitin reaction, filters successively, washing, drying precipitated, obtains barium peroxide.
Particularly, in the preparation method of above-mentioned barium peroxide, the concentration of superoxol is preferably 2～4%(volume ratio), the mol ratio of bariumchloride and hydrogen peroxide is preferably 1:(6.6～7.5).Drip the consumption of ammoniacal liquor by control, the pH value of regulating mixing solutions is preferably 8.
In the preparation method of above-mentioned barium peroxide, the NH4 in ammoniacal liquor
+with the Cl in bariumchloride
-ionic bond, make the Ba in bariumchloride
2+spin off, thus with oxidants hydrogen peroxide (H
2o
2) reaction obtains barium peroxide (BaO
2h
2o
2); In addition, by regulate pH be the weak base value to control ammonia volume, make Cl
-ion is participated in reaction fully, and then makes Ba
2+can spin off fully and participate in follow-up reaction.
In acid pickling step in above-mentioned steps S02, the acid solution of above-mentioned cleanup acid treatment is salpeter solution, hydrochloric acid soln or sulphuric acid soln, wherein preferred salpeter solution.The concentration of acid solution is preferably 0.5～1.5mol/L.
Further preferably, above-mentioned drying treatment temperature is 70～90 ℃.
In the preparation method's of above-mentioned submicron barium titanate crystal heat treatment process, barium peroxide (BaO
2) melting, effectively increased itself and solid-phase reactant titanium dioxide (TiO
2) contact area, even both still have higher reactive behavior under relatively low temperature of reaction.Simultaneously, BaO
2with TiO
2the consumption specific energy guarantee TiO
2complete reaction, obtain highly purified BaTiO
3.The submicron barium titanate crystal made by the method is that single-phase, good crystallinity, purity are high, and its preparation temperature is relatively low, and condition is easily controlled, and technique is simple, and not high to equipment requirements, cost is low, is suitable for suitability for industrialized production.
Above-mentioned submicron barium titanate crystal, its crystalline structure is single-phase Tetragonal, good crystallinity, purity is high, and narrow diameter distribution all improves to some extent the chemical physics performances such as it is ferroelectric, thermoelectricity, piezoelectricity, nonlinear optics, electrical-optical conversion.
Below illustrate the aspects such as above-mentioned submicron barium titanate crystal and preparation method thereof by a plurality of embodiment.
Embodiment 1
A kind of submicron barium titanate crystal and preparation method thereof, this preparation method is specific as follows:
(1) take 1.2213g(0.005mol) bariumchloride (BaCl
22H
2o, A.R., pilot plant of Shanghai Chemistry High School) in the 100mL beaker, add the hydrogen peroxide (H that the 40ml volume ratio is 3%
2o
2, A.R., Chemical Reagent Co., Ltd., Sinopharm Group), stir, dissolve complete, then drip ammoniacal liquor (NH
4oH, A.R., Shanghai Su Yi chemical reagent company limited), regulate the pH=8 of mixing solutions, then, by reaction solution at room temperature standing 30 minutes, separate out light-yellow precipitate, suction filtration is precipitated, and then uses respectively deionized water and dehydrated alcohol (CH
3cH
2oH, A.R., Chemical Reagent Co., Ltd., Sinopharm Group) wash 6 times after, in the air at room temperature drying, obtain presoma.
(2) presoma (0.002mol) prepared by step (1) and commercially available titanium dioxide granule (TiO
2c.R., Shanghai fine materials No.2 Research Institute) (0.002mol) mix, fully grind with agate mortar, then said mixture is placed in to retort furnace, be heated to 700 ℃, heat-up rate is 14 ℃/minute, under 700 ℃, reaction is 10 hours, then naturally cools to room temperature, obtains reaction product a.
(3) reaction product prepared with the abundant washing step of 1mol/L nitric acid (2), the 80 ℃ of dryings 40 minutes in air of the reaction product after then washing, obtain final product b.
A kind of submicron barium titanate crystal and preparation method thereof, except the consumption of the presoma consumption that is 0.002mol, titanium dioxide is 0.0018mol, other preparation methods are identical with embodiment 1.Obtain reaction product c and final product d.
Embodiment 3
A kind of submicron barium titanate crystal and preparation method thereof, except the consumption of the presoma consumption that is 0.002mol, titanium dioxide is 0.0016mol, other preparation methods are identical with embodiment 1.Obtain reaction product e and final product f.
By presoma, reaction product and the final product of embodiment 1～3 preparation formed respectively, the analysis of structure and pattern aspect.Analytical results is as follows:
The XRD figure that Fig. 2-1 is the presoma of preparation in embodiment 1 step (1).With standard card (JCPDSNo.19-0129), contrast, and the unit cell parameters a=4.132 calculated according to the diffraction peak in figure
b=9.464
c=8.308
α=γ=90 °, β=98.58 °, known this presoma is oblique system BaO
2h
2o
2.Simultaneously, diffraction peak strong and sharp-pointed from figure can be learnt, this BaO
2h
2o
2crystallinity fine.And there is no the diffraction peak of impurity in figure, BaO is described
2h
2o
2purity very high.
The SEM figure that Fig. 2-2 are the presoma of preparation in embodiment 1 step (1).Can find out: the submicron particles that this presoma is particle diameter 130～450nm.
The XRD figure of reaction product a in the corresponding embodiment 1～3 of (a)～(f) spectrogram difference in Fig. 3-1, final product b, reaction product c, final product d, reaction product e, final product f.
With standard card (JCPDS No.03-0725), contrast, and the unit cell parameters a=b=3.994 calculated according to the diffraction peak in figure
c=4.038
the BaTiO that known final product f is Tetragonal
3.Simultaneously, diffraction peak strong and sharp-pointed in figure can be learnt, this BaTiO
3crystallinity fine.In addition, (f) spectrogram is compared with (e) spectrogram, the diffraction peak of impurity do not occur, and the impurity in the reaction product in this explanation embodiment 3 can wash and remove by nitric acid, thereby obtains highly purified BaTiO
3.
In addition, final product b, d from pickling and the XRD figure of f can be found out, faint but observable impurity diffraction peak has appearred in spectrogram (b), and spectrogram (d) and the diffraction peak of impurity (f) almost do not occur illustrates that final product d and the f after pickling is higher than the purity of final product b.Therefore, the barium peroxide of excessive mole dosage reacts with titanium dioxide and the barium peroxide of same molar reacts with titanium dioxide, and the purity of the final product after the reaction product pickling obtained is higher.
By XPS and ICP, the contriver has further studied the surface of the final product f of preparation in embodiment 3 and purity and the stoichiometric ratio of body phase.Wherein the XPS analysis result is as shown in Fig. 3-2.In XPS photoelectron spectrum from figure, in known final product f, except containing C(, usually using C1s peak (284.6eV) as N Reference Alignment), only contain Ti, Ba and O, there do not is other possible impurity.Ba3d
5/2and Ti2p
3/2in conjunction with can be respectively 778.0 and 457.2eV, BaTiO in this and document
3ba
2+and Ti
4+numerical value consistent.From Ba
2+and Ti
4+the numerical evaluation of peak area known, in final product f, the element number ratio of contained Ba and Ti is about 0.83:1, this illustrates that its sample surfaces (degree of depth is 5nm usually) is rich in Ti.In addition, the XPS analysis result also shows that, in its block sample, the element number ratio of Ba and Ti is 0.994:1, or relatively close to BaTiO
3the stoichiometric ratio of middle Ba and Ti.
The SEM figure that Fig. 3-3 are the final product f of preparation in embodiment 3, from figure, we can see, and this final product is sub-micron crystal, and its particle diameter is 180～400nm.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. the preparation method of a submicron barium titanate crystal comprises the following steps:
By after barium peroxide and titanium dioxide in molar ratio >=1 combination treatment, carry out thermal response, obtain reaction product;
Described reaction product is carried out to pickling successively, and drying treatment, obtain the submicron barium titanate crystal.
2. the preparation method of submicron barium titanate crystal as claimed in claim 1, it is characterized in that: in the step of described thermal response, the mol ratio of described barium peroxide and titanium dioxide is 1:(0.8～1).
3. the preparation method of submicron barium titanate crystal as claimed in claim 1, it is characterized in that: in the step of described thermal response, described thermal response temperature is 600～800 ℃, and the thermal response time is 8～12h.
4. the preparation method of submicron barium titanate crystal as described as claim 1 or 3, it is characterized in that: in the step of described thermal response, described thermal response temperature is 700 ℃, and the thermal response time is 10h.
5. the preparation method of submicron barium titanate crystal as described as claim 1 or 3 is characterized in that: in the step of described thermal response, be that the temperature rise rate with 12～16 ℃/min is heated to described thermal response temperature.
6. the preparation method of submicron barium titanate crystal as claimed in claim 1, it is characterized in that: in the step of described thermal response, the preparation method of barium peroxide is:
Bariumchloride is dissolved in superoxol, drips ammoniacal liquor, the pH value of regulating mixing solutions is 7～9, carries out precipitin reaction, filters successively, washing, drying precipitated, obtains barium peroxide.
7. the preparation method of submicron barium titanate crystal as claimed in claim 6, it is characterized in that: the mol ratio of described bariumchloride and hydrogen peroxide is 1:(6.6～7.5).
8. the preparation method of submicron barium titanate crystal as claimed in claim 1, it is characterized in that: in the step of described pickling, the acid solution of described cleanup acid treatment is nitric acid, hydrochloric acid or sulphuric acid soln.
9. a submicron barium titanate crystal, it is characterized in that: described submicron barium titanate crystal is formed by the preparation method of described claim 1～8 any one submicron barium titanate crystal, and described submicron barium titanate crystal is the Tetragonal crystalline structure.
10. submicron barium titanate crystal as claimed in claim 9, it is characterized in that: its particle diameter is 180～400nm.
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