CN103449512A - Method for preparing monodisperse and cuboid nano-barium titanate powder by virtue of microwave hydrothermal method - Google Patents
Method for preparing monodisperse and cuboid nano-barium titanate powder by virtue of microwave hydrothermal method Download PDFInfo
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- CN103449512A CN103449512A CN2013103861972A CN201310386197A CN103449512A CN 103449512 A CN103449512 A CN 103449512A CN 2013103861972 A CN2013103861972 A CN 2013103861972A CN 201310386197 A CN201310386197 A CN 201310386197A CN 103449512 A CN103449512 A CN 103449512A
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Abstract
The invention discloses a method for preparing monodisperse and cuboid nano-barium titanate powder by virtue of a microwave hydrothermal method. The method comprises the following steps: adding oleic acid and tetrabutyl titanate into a barium hydroxide water solution, performing microwave hydrothermal reaction, and synthesizing monodisperse and cuboid nano-barium titanate with the particle size of about 10nm within a short period of time. The method disclosed by the invention has the advantages of simplicity and easiness in operation, low synthesis cost and short time required for synthesis, the obtained nano-barium titanate has the advantages of small particle size, uniform appearance and good dispersion, the follow-up surface treatment is not required, and the industrial batch production is convenient to realize.
Description
Technical field
The invention belongs to the nano material preparing technical field, be specifically related to a kind of method for preparing single dispersion, rectangular parallelepiped nano barium carbonate powder by microwave-hydrothermal method.
Background technology
Barium titanate is widely used in preparing the multiple electronic components such as ferroelectric, piezoelectricity, ceramic condenser (MLCC), PTC thermistor as a kind of important electron ceramic material, in addition, barium titanate also has photochemical catalysis and combustion catalysis activity, in some photoresponses and combustion reactions, as catalyzer, uses.Preparation method about barium titanate mainly contains traditional solid sintering technology, sol-gel method, hydrothermal method, co-precipitation etc. both at home and abroad.The tradition solid sintering technology is to be incorporated in 1300 ℃ of left and right high-temperature calcinations by barium carbonate and titanium dioxide etc. are mixed, and the resulting product purity of this method is not high, the large and skewness of particle diameter; The raw material costliness that sol-gel method is used, complicated operation, the production cycle is long; Co-precipitation is more complicated also, and the presoma prepared must be through high-temperature calcination, and in calcination process, crystal grain is easily grown up, and is unfavorable for the control of particle size.In addition, the nano barium phthalate that aforesaid method makes often exists with the coacervate form, is difficult to obtain monodisperse nanoparticle.Hydrothermal method has longer developing history, and experimentation is simple, and operation is easily gone, and when replace traditional baking oven for heating with microwave heating, hydrothermal synthesis reaction speed can significantly improve, and save the reaction times, so the microwave hydrothermal synthesis method enjoys favor.Before this Song not the people such as Xi Bin (CN101746814A) synthesize favorable dispersity, the barium titanate that spherical, particle diameter is greater than 80nm by microwave method, the people such as Shi Liyi (CN102584219A) also prepare 100nm left and right, spherical barium titanate by microwave method.Yet the research that approaches 10nm, cuboid nano barium phthalate by the single dispersion of microwave method hydrothermal method preparation, particle diameter has no report.The present invention adopts the synthetic nano barium phthalate of microwave-hydrothermal method to have the rectangular parallelepiped pattern, and the about 10nm of particle diameter and being evenly distributed in monodisperse status, occurs without agglomeration between particle.
Summary of the invention
Technical problem to be solved by this invention is to overcome the existing shortcoming for preparing the nano barium phthalate method, as, easily reunite, pattern is uncontrollable, synthesis step is complicated etc.The invention provides a kind of method that microwave-hydrothermal method prepares single dispersion, rectangular parallelepiped nano barium carbonate powder, the method is simple, and synthetic cost is low, synthetic required time is short, the about 10nm of resulting nano barium phthalate particle diameter, good dispersity, do not need it is carried out to follow-up surface treatment.
Solving the problems of the technologies described above adopted technical scheme is: in the baryta water of 0.11～0.14mol/L, add oleic acid and tetrabutyl titanate, the mol ratio of tetrabutyl titanate and hydrated barta, oleic acid is 1:0.9～1.5:0.15～1, stir, 180～220 ℃ of microwave hydrothermals react 2～6 hours, reaction is chilled to room temperature naturally after finishing, product is extremely neutral with deionized water wash, vacuum-drying, grind, obtain the dispersed nano barium carbonate powder.
The mol ratio of tetrabutyl titanate of the present invention and hydrated barta, oleic acid is preferably 1:1～1.5:0.35～0.67, and the best is 1:1.2:0.35.
Preferably 180～200 ℃ of reactions 4～6 hours of microwave hydrothermal reaction conditions of the present invention, also can be preferably 200 ℃ of reactions 2～6 hours, the best is 200 ℃ of reactions 4 hours.
Compared with prior art, the present invention has following advantage and beneficial effect:
1, the inventive method energy consumption is low, and cost is low, and preparation cycle is short, and environmental friendliness is simple to operate.
2, the prepared barium titanate of the present invention is Emission in Cubic, is the pattern of rectangular parallelepiped, and particle size is in about 10nm, narrow diameter distribution, good dispersity, during use without carrying out surface treatment.
The accompanying drawing explanation
Fig. 1 is single dispersion of embodiment 1～7 preparation, the XRD figure of rectangular parallelepiped nano barium carbonate powder.
Fig. 2 is single dispersion of embodiment 1 preparation, the TEM figure of rectangular parallelepiped nano barium carbonate powder.
Fig. 3 is single dispersion of embodiment 2 preparations, the TEM figure of rectangular parallelepiped nano barium carbonate powder.
Fig. 4 is single dispersion of embodiment 3 preparations, the TEM figure of rectangular parallelepiped nano barium carbonate powder.
Fig. 5 is single dispersion of embodiment 4 preparations, the TEM figure of rectangular parallelepiped nano barium carbonate powder.
Fig. 6 is single dispersion of embodiment 5 preparations, the TEM figure of rectangular parallelepiped nano barium carbonate powder.
Fig. 7 is single dispersion of embodiment 6 preparations, the TEM figure of rectangular parallelepiped nano barium carbonate powder.
Fig. 8 is single dispersion of embodiment 7 preparations, the TEM figure of rectangular parallelepiped nano barium carbonate powder.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in more detail, but the scope of protection of present invention is not limited to these embodiment.
Embodiment 1
Add 0.12g(0.41mmol in the baryta water of 10.21mL 0.14mol/L) oleic acid and 0.40g(1.18mmol) tetrabutyl titanate, tetrabutyl titanate and hydrated barta, the mol ratio of oleic acid is 1:1.2:0.35, stir, under the condition that the MDS-6 type microwave dissolver that is 1000W with power is 2450MHz in frequency, 200 ℃ are reacted 4 hours, reaction naturally cools to room temperature after finishing, product is extremely neutral with deionized water wash, use again absolute ethanol washing 3 times, 60 ℃ of vacuum-drying 6 hours, grind, obtain single dispersion, the rectangular parallelepiped nano barium carbonate powder.
Resulting product adopts DX-2000 type X-ray diffractometer and JEM-2100 (Japan) type transmission electron microscope to be characterized respectively, the results are shown in Figure curve a and Fig. 2 in 1.As shown in Figure 1, all diffraction peaks of product all match substantially with cubic phase barium titanate standard card (JCPDS No.31-174), learn that thus the gained barium titanate particles is the Emission in Cubic structure.As seen from Figure 2, resulting barium titanate is monodispersed rectangular parallelepiped particle, and particle size is in the 10nm left and right.
Embodiment 2
Add 0.08g(0.26mmol in the baryta water of 10.16mL 0.11mol/L) oleic acid and 0.32g(0.94mmol) tetrabutyl titanate, tetrabutyl titanate and hydrated barta, the mol ratio 1:1.2:0.28 of oleic acid, stir, under the condition that the MDS-6 type microwave dissolver that is 1000W with power is 2450MHz in frequency, 200 ℃ are reacted 4 hours, reaction is chilled to room temperature naturally after finishing, product is extremely neutral with deionized water wash, use again absolute ethanol washing 3 times, 60 ℃ of vacuum-drying 6 hours, grind, obtain single dispersion, the rectangular parallelepiped nano barium carbonate powder, its XRD figure is shown in curve b in Fig. 1, TEM figure is shown in Fig. 3.
Embodiment 3
Add 0.12g(0.41mmol in the baryta water of 10.21mL 0.14mol/L) oleic acid and 0.40g(1.18mmol) tetrabutyl titanate, tetrabutyl titanate and hydrated barta, the mol ratio of oleic acid is 1:1.2:0.35, stir, under the condition that the MDS-6 type microwave dissolver that is 1000W with power is 2450MHz in frequency, 200 ℃ are reacted 2 hours, reaction is chilled to room temperature naturally after finishing, product is extremely neutral with deionized water wash, use again absolute ethanol washing 3 times, 60 ℃ of vacuum-drying 6 hours, grind, obtain single dispersion, the rectangular parallelepiped nano barium carbonate powder, its XRD figure is shown in curve c in Fig. 1, TEM figure is shown in Fig. 4.
Embodiment 4
Add 0.12g(0.41mmol in the baryta water of 10.21mL 0.14mol/L) oleic acid and 0.40g(1.18mmol) tetrabutyl titanate, tetrabutyl titanate and hydrated barta, the mol ratio of oleic acid is 1:1.2:0.35, stir, under the condition that the MDS-6 type microwave dissolver that is 1000W with power is 2450MHz in frequency, 200 ℃ are reacted 6 hours, reaction is chilled to room temperature naturally after finishing, product is extremely neutral with deionized water wash, use again absolute ethanol washing 3 times, 60 ℃ of vacuum-drying 6 hours, grind, obtain single dispersion, the rectangular parallelepiped nano barium carbonate powder, its XRD figure is shown in curve d in Fig. 1, TEM figure is shown in Fig. 5.
Embodiment 5
Add 0.33g(1.17mmol in the baryta water of 10.21mL 0.14mol/L) oleic acid and 0.40g(1.18mmol) tetrabutyl titanate, tetrabutyl titanate and hydrated barta, the mol ratio of oleic acid is 1:1.2:1, stir, under the condition that the MDS-6 type microwave dissolver that is 1000W with power is 2450MHz in frequency, 200 ℃ are reacted 4 hours, reaction is chilled to room temperature naturally after finishing, product is extremely neutral with deionized water wash, use again absolute ethanol washing 3 times, 60 ℃ of vacuum-drying 6 hours, grind, obtain single dispersion, the rectangular parallelepiped nano barium carbonate powder, its XRD figure is shown in curve e in Fig. 1, TEM figure is shown in Fig. 6.
Embodiment 6
Add 0.12g(0.41mmol in the baryta water of 10.21mL 0.14mol/L) oleic acid and 0.40g(1.18mmol) tetrabutyl titanate, tetrabutyl titanate and hydrated barta, the mol ratio of oleic acid is 1:1.2:0.35, stir, under the condition that the MDS-6 type microwave dissolver that is 1000W with power is 2450MHz in frequency, 180 ℃ are reacted 4 hours, reaction is chilled to room temperature naturally after finishing, product is extremely neutral with deionized water wash, use again absolute ethanol washing 3 times, 60 ℃ of vacuum-drying 6 hours, grind, obtain single dispersion, the rectangular parallelepiped nano barium carbonate powder, its XRD figure is shown in curve f in Fig. 1, TEM figure is shown in Fig. 7.
Embodiment 7
Add 0.12g(0.41mmol in the baryta water of 10.21mL 0.14mol/L) oleic acid and 0.40g(1.18mmol) tetrabutyl titanate, tetrabutyl titanate and hydrated barta, the mol ratio of oleic acid is 1:1.2:0.35, stir, under the condition that the MDS-6 type microwave dissolver that is 1000W with power is 2450MHz in frequency, 220 ℃ are reacted 4 hours, reaction is chilled to room temperature naturally after finishing, product is extremely neutral with deionized water wash, use again absolute ethanol washing 3 times, 60 ℃ of vacuum-drying 6 hours, grind, obtain single dispersion, the rectangular parallelepiped nano barium carbonate powder, its XRD figure is shown in curve g in Fig. 1, TEM figure is shown in Fig. 8.
Embodiment 8
Add 0.07g(0.25mmol in the baryta water of 10.21mL 0.14mol/L) oleic acid and 0.54g(1.59mmol) tetrabutyl titanate, tetrabutyl titanate and hydrated barta, the mol ratio of oleic acid is 1:0.9:0.15, stir, under the condition that the MDS-6 type microwave dissolver that is 1000W with power is 2450MHz in frequency, 200 ℃ are reacted 4 hours, reaction is chilled to room temperature naturally after finishing, product is extremely neutral with deionized water wash, use again absolute ethanol washing 3 times, 60 ℃ of vacuum-drying 6 hours, grind, obtain single dispersion, the rectangular parallelepiped nano barium carbonate powder.
Embodiment 9
Add 0.28g(0.96mmol in the baryta water of 10.21mL 0.14mol/L) oleic acid and 0.48g(1.43mmol) tetrabutyl titanate, tetrabutyl titanate and hydrated barta, the mol ratio of oleic acid is 1:1:0.67, stir, under the condition that the MDS-6 type microwave dissolver that is 1000W with power is 2450MHz in frequency, 200 ℃ are reacted 4 hours, reaction is chilled to room temperature naturally after finishing, product is extremely neutral with deionized water wash, use again absolute ethanol washing 3 times, 60 ℃ of vacuum-drying 6 hours, grind, obtain single dispersion, the rectangular parallelepiped nano barium carbonate powder.
Add 0.28g(0.95mmol in the baryta water of 10.21mL 0.14mol/L) oleic acid and 0.32g(0.95mmol) tetrabutyl titanate, the mol ratio of tetrabutyl titanate and hydrated barta, oleic acid is 1:1.5:1, stir, under the condition that the MDS-6 type microwave dissolver that is 1000W with power is 2450MHz in frequency, 220 ℃ are reacted 4 hours, reaction is chilled to room temperature naturally after finishing, product is extremely neutral with deionized water wash, use again absolute ethanol washing 3 times, 60 ℃ of vacuum-drying 6 hours, grind, obtain single dispersion, rectangular parallelepiped nano barium carbonate powder.
Claims (6)
1. a microwave-hydrothermal method prepares the singly method of dispersion, rectangular parallelepiped nano barium carbonate powder, it is characterized in that: in the baryta water of 0.11～0.14mol/L, add oleic acid and tetrabutyl titanate, the mol ratio of tetrabutyl titanate and hydrated barta, oleic acid is 1:0.9～1.5:0.15～1, stir, 180～220 ℃ of microwave hydrothermals react 2～6 hours, reaction is chilled to room temperature naturally after finishing, product is extremely neutral with deionized water wash, vacuum-drying, grind, obtain the dispersed nano barium carbonate powder.
2. microwave-hydrothermal method according to claim 1 prepares the method for single dispersion, rectangular parallelepiped nano barium carbonate powder, and it is characterized in that: the mol ratio of described tetrabutyl titanate and hydrated barta, oleic acid is 1:1～1.5:0.35～0.67.
3. microwave-hydrothermal method according to claim 1 prepares the method for single dispersion, rectangular parallelepiped nano barium carbonate powder, and it is characterized in that: the mol ratio of described tetrabutyl titanate and hydrated barta, oleic acid is 1:1.2:0.35.
4. prepare the method for single dispersion, rectangular parallelepiped nano barium carbonate powder according to the described microwave-hydrothermal method of claim 1～3 any one, it is characterized in that: described microwave hydrothermal reaction conditions is 180～200 ℃ of reactions 4～6 hours.
5. microwave-hydrothermal method according to claim 3 prepares the method for single dispersion, rectangular parallelepiped nano barium carbonate powder, it is characterized in that: described microwave hydrothermal reaction conditions is 200 ℃ of reactions 2～6 hours.
6. microwave-hydrothermal method according to claim 3 prepares the method for single dispersion, rectangular parallelepiped nano barium carbonate powder, it is characterized in that: described microwave hydrothermal reaction conditions is 200 ℃ of reactions 4 hours.
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Cited By (2)
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| JP2016041641A (en) * | 2014-08-19 | 2016-03-31 | 日本化学機械製造株式会社 | Fine particle of perovskite type titanium compound and production method of the same |
| CN117602667A (en) * | 2023-12-01 | 2024-02-27 | 同济大学 | Mesoporous barium titanate nano material and preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2016041641A (en) * | 2014-08-19 | 2016-03-31 | 日本化学機械製造株式会社 | Fine particle of perovskite type titanium compound and production method of the same |
| CN117602667A (en) * | 2023-12-01 | 2024-02-27 | 同济大学 | Mesoporous barium titanate nano material and preparation method and application thereof |
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