CN105967228A - Preparation method of graded porous barium titanate submicron-level particle sphere - Google Patents
Preparation method of graded porous barium titanate submicron-level particle sphere Download PDFInfo
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- CN105967228A CN105967228A CN201610565938.7A CN201610565938A CN105967228A CN 105967228 A CN105967228 A CN 105967228A CN 201610565938 A CN201610565938 A CN 201610565938A CN 105967228 A CN105967228 A CN 105967228A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/006—Alkaline earth titanates
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/01—Particle morphology depicted by an image
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
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- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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Abstract
The invention discloses a preparation method of a graded porous barium titanate submicron-level particle sphere. The preparation method comprises the following steps: adding n-butyl titanate and an organic mixed solution into a high-pressure reaction kettle; heating the high-pressure reaction kettle to a preset temperature, maintaining at the preset temperature for a preset time period, and then naturally cooling from the preset temperature to the room temperature, so as to obtain white porous dititanate submicron-level particle sphere precursor; and adding the white porous dititanate submicron-level particle sphere precursor, a barium salt solution and a hydroxide solution into the high-pressure reaction kettle, heating the high-pressure reaction kettle to the preset temperature, maintaining at the preset temperature for a preset time period, and then naturally cooling from the preset temperature to the room temperature, so as to obtain the graded porous barium titanate submicron-level particle sphere with good dispersity. The preparation method has the advantages that the production process is simple and safe, the cost is low, the yield is high, the phase of the produced product is a cubic crystalline phase, and the products are of a graded porous sphere shape and have uniform particle sizes and shapes.
Description
Technical field
The present invention relates to the preparation method of a kind of classifying porous Barium metatitanate. submicron particles ball, belong to functional material
Field.
Background technology
Barium metatitanate. has the performances such as outstanding dielectric, piezoelectricity, ferroelectricity, pyroelectricity, and Barium metatitanate. extensively should
For preparing the electronic devices such as multilayer ceramic capacitor, transducer, ceramic filter, temperature sensor.
Owing to classifying porous micro-sphere material has many outstanding special performances, the most classifying porous microsphere has extensively
General purposes.Such as, the character such as the porosity big, big due to specific surface area and outstanding optical, electrical, because of
This classifying porous microsphere has a wide range of applications in fields such as energy storage material, chemical catalysis and offal treatments.Mesh
Before, people the most successfully synthesize the barium titanate nano granule of the different-shapes such as nano wire, rod, cubic block, ball.
But it is the most little to the research of Barium metatitanate. hierarchy granule ball.
Summary of the invention
It is an object of the invention to provide one and be prone to industrialized production and low production cost, production technology peace
Entirely, the scale topography of product particle is homogeneous, the preparation of the classification Barium metatitanate. submicron particles ball of favorable dispersibility
Method.
To achieve these goals, the present invention is by the following technical solutions:
The present invention proposes the preparation method of a kind of classifying porous Barium metatitanate. submicron particles ball, including walking as follows
Rapid:
S1, tetrabutyl titanate and isopropanol and dimethylformamide mixed solution are carried out heat in autoclave
Reaction obtains product A；
S2, the product A sucking filtration that step S1 is prepared, precipitation, with absolute ethanol washing three times, obtain
The porous two metatitanic acid submicron particles ball presoma of white hierarchy；
S3, by step S2 prepare white hierarchy porous two metatitanic acid submicron particles ball presoma with
Barium salt solution and hydroxide solution carry out thermal response in autoclave and obtain product B；
S4, product B sucking filtration step S3 prepared, precipitation, successively by diluted acid, deionized water, nothing
Water-ethanol washs, and dried obtains classifying porous Barium metatitanate. submicron particles ball.
Preferably, step S1 comprises the steps:
S11, under stirring, successively isopropanol and dimethylformamide are joined in reaction bulb, wherein
The volume ratio of isopropanol and dimethylformamide is 1～10；Then tetrabutyl titanate, Ti are added4+Ion is dense
Degree is 0.05～1.0mol/L；
S12, by step S11 prepare solution be placed in autoclave, at 140 DEG C～260 DEG C, reaction
2h～48h；After reaction terminates, allow autoclave naturally cool to room temperature, obtain product A.
Preferably, step S3 comprises the steps:
S31, under stirring, the porous two metatitanic acid submicron of white hierarchy that step S2 is prepared
Grade particles ball presoma and 0.1～10mol/L barium salt solution are put in reaction bulb, and control barium with the mol ratio of titanium is
1.01～1.50；Add 0.1～10mol/L hydroxide solution, continue stirring 10min, regulation reaction system
PH value is 12～14, and mix homogeneously；
S32, by step S31 prepare solution be placed in autoclave, be warmed up to 120 DEG C～280 DEG C, and
Maintain 2h～72h；After reaction terminates, allow autoclave naturally cool to room temperature, obtain product B.
It is further preferred that the pH value regulating reaction system in described step S31 is 13.Regulation reaction system
PH value be 13.
Preferably, the one during described barium salt is barium hydroxide, barium nitrate, Barium acetate, barium chloride.
Preferably, described hydroxide is the one in sodium hydroxide, potassium hydroxide.
Preferably, diluted acid described in step S4 is formic acid or acetic acid.
Preferably, the concentration of diluted acid described in step S4 is 0.01～0.1mol/L.
Preferably, the described oven drying that dried step is 50～120 DEG C 2～12h.
Preferably, described classifying porous Barium metatitanate. submicron particles ball is by barium titanate nano sheet particle agglomeration
Become.
The invention has the beneficial effects as follows:
The preparation method of the classifying porous Barium metatitanate. submicron particles ball of the present invention, production technology is simple, safety,
Equipment requirements is the highest, with low cost, and productivity is high, and the product thing of preparation is a cube crystalline phase mutually, has classifying porous
Spherical looks, and transmission electron microscope (TEM) photo and scanning electron microscope (SEM) photo show, the size of granule and pattern
Homogeneous.
Through X-ray diffraction (XRD) atlas analysis, classifying porous Barium metatitanate. submicron order prepared by the present invention
Granule ball is a cube crystalline phase, and specific surface area is big, and good dispersion, powder granule pattern is single；Classifying porous metatitanic acid
Two-dimensional nano chip architecture, as a kind of nanometer package assembly, is well combined into macroscopic view by barium submicron particles ball
Three dimensional structure so that while material itself maintains the new capability of nanoscale, in macroscopically convenient manipulation and
Application, therefore can be applicable to the fields such as electrical and optical.
Accompanying drawing explanation
Fig. 1 is the process chart of the preparation method of the present invention classifying porous Barium metatitanate. submicron particles ball.
Fig. 2 is the X-ray diffraction (XRD) of classifying porous Barium metatitanate. submicron particles ball prepared by the present invention
Collection of illustrative plates；
Fig. 3 is that the transmission electron microscope (TEM) of classifying porous Barium metatitanate. submicron particles ball prepared by the present invention shines
Sheet；
Fig. 4 is that the scanning electron microscope (SEM) of classifying porous Barium metatitanate. submicron particles ball prepared by the present invention shines
Sheet.
Detailed description of the invention
Below in conjunction with detailed description of the invention and compare accompanying drawing the present invention is described in further detail.It should be emphasized that
It is, that the description below is merely exemplary rather than in order to limit the scope of the present invention and application thereof.
Refer to Fig. 1-Fig. 4.
The present invention proposes the preparation method of a kind of classifying porous Barium metatitanate. submicron particles ball, including walking as follows
Rapid:
S1, tetrabutyl titanate is carried out in autoclave with isopropanol and dimethylformamide mixed solution
Thermal response obtains product A；
S2, the product A sucking filtration that step S1 is prepared, precipitation, with absolute ethanol washing three times, obtain
The porous two metatitanic acid submicron particles ball presoma of white hierarchy；
S3, by step S2 prepare white hierarchy porous two metatitanic acid submicron particles ball presoma with
Barium salt solution and hydroxide solution carry out thermal response in autoclave and obtain product B；
S4, product B sucking filtration step S3 prepared, precipitation, successively by diluted acid, deionized water, nothing
Water-ethanol washs, and dried obtains classifying porous Barium metatitanate. submicron particles ball.
Example 1:
A1, successively 30mL isopropanol and 5mL dimethylformamide are joined in 50mL reaction bulb,
Then add 0.6g tetrabutyl titanate, and stir 5min；
A2, the solution that step A1 is prepared are placed in autoclave, and reaction system is warming up to 140 DEG C,
And maintain 48h；After reaction terminates, autoclave is allowed to naturally cool to room temperature；
A3, the products therefrom sucking filtration of step A2；Precipitation, with absolute ethanol washing three times；Obtain white point
The porous two metatitanic acid submicron particles ball presoma of level structure；
A4,10ml deionized water is joined in 50mL reaction bulb, under stirring, add step
The porous two metatitanic acid submicron particles ball presoma 0.35g of the white hierarchy that A3 prepares；Then eight are weighed
Water barium hydroxide 1.2g, is dissolved in above-mentioned solution, continues stirring 10min, then regulates solution with sodium hydroxide solution
PH value is 12；
A5, the solution that step A4 is prepared are placed in autoclave, and reaction system is warming up to 120 DEG C,
And maintain 72h；After reaction terminates, autoclave is allowed to naturally cool to room temperature；
A6, by the products therefrom sucking filtration of step A5, precipitation, successively with 0.01mol/L acetic acid, deionized water,
Dehydrated alcohol respectively washs secondary, then product is placed in the oven drying 2h of 120 DEG C, i.e. obtains classifying porous metatitanic acid
Barium submicron particles ball.Analyzing through X-ray diffraction (XRD) collection of illustrative plates (see Fig. 2), result shows institute
Obtaining classification POROUS TITANIUM acid barium submicron particles ball thing is a cube crystalline phase mutually, has no other impurity peaks any.Transmission
Electronic Speculum (TEM) photo (see Fig. 3) and scanning electron microscope (SEM) photo (see Fig. 4) display, the classifying porous metatitanic acid of gained
Size and the pattern of barium submicron particles ball have preferable homogeneity.
Example 2:
A1, successively 25mL isopropanol and 10mL dimethylformamide are joined in 50mL reaction bulb,
Then add 1.1g butyl titanate, and stir 5min；
A2, the solution that step A1 is prepared are placed in autoclave, and reaction system is warming up to 220 DEG C,
And maintain 30h；After reaction terminates, autoclave is allowed to naturally cool to room temperature；
A3, the products therefrom sucking filtration of step A2, precipitation, with absolute ethanol washing three times, obtain white point
The porous two metatitanic acid submicron particles ball presoma of level structure；
A4,10ml deionized water is joined in 50mL reaction bulb, under stirring, add step
The porous two metatitanic acid submicron particles ball presoma 0.35g of the white hierarchy that A3 prepares；Then nitre is weighed
Acid barium 0.61g, is dissolved in above-mentioned solution, continues stirring 10min, then regulates solution PH with sodium hydroxide solution
Value is 14；
A5, the solution that step A4 is prepared are placed in autoclave, and reaction system is warming up to 200 DEG C,
And maintain 48h；After reaction terminates, autoclave is allowed to naturally cool to room temperature；
A6, by the products therefrom sucking filtration of step A5, precipitation, successively with 0.04mol/L formic acid, deionized water,
Dehydrated alcohol respectively washs secondary, then product is placed in the oven drying 12h of 50 DEG C, i.e. obtains classifying porous metatitanic acid
Barium submicron particles ball.
Example 3:
A1, successively 17.5mL isopropanol and 17.5mL dimethylformamide are joined in 50mL reaction bulb,
Then add 1.5g tetrabutyl titanate, and stir 5min；
A2, the solution that step A1 is prepared are placed in autoclave, and reaction system is warming up to 260 DEG C,
And maintain 2h；After reaction terminates, autoclave is allowed to naturally cool to room temperature；
A3, the products therefrom sucking filtration of step A2, precipitation, with absolute ethanol washing three times, obtain white point
The porous two metatitanic acid submicron particles ball presoma of level structure；
A4,10ml deionized water is joined in 50mL reaction bulb, under stirring, add step
The porous two metatitanic acid submicron particles ball presoma 0.35g of the white hierarchy that A3 prepares；Then chlorine is weighed
Change barium 1.02g, be dissolved in above-mentioned solution, continue stirring 10min, then regulate solution pH value with sodium hydroxide solution
It is 13；
A5, the solution that step A4 is prepared are placed in autoclave, and reaction system is warming up to 240 DEG C,
And maintain 20h；After reaction terminates, autoclave is allowed to naturally cool to room temperature；
A6, by the products therefrom sucking filtration of step A5, precipitation, successively with 0.08mol/L acetic acid, deionized water,
Dehydrated alcohol respectively washs secondary, then product is placed in the oven drying 5h of 80 DEG C, i.e. obtains classifying porous metatitanic acid
Barium submicron particles ball.
Embodiment 4
A1, successively 27.5mL isopropanol and 7.5mL dimethylformamide are joined in 50mL reaction bulb,
Then add 1.6g tetrabutyl titanate, and stir 5min；
A2, the solution that step A1 is prepared are placed in autoclave, and reaction system is warming up to 200 DEG C,
And maintain 36h；After reaction terminates, autoclave is allowed to naturally cool to room temperature；
A3, the products therefrom sucking filtration of step A2, precipitation, with absolute ethanol washing three times, obtain white point
The porous two metatitanic acid submicron particles ball presoma of level structure；
A4,10ml deionized water is joined in 50mL reaction bulb, under stirring, add step
The porous two metatitanic acid submicron particles ball presoma 0.35g of the white hierarchy that A3 prepares；Then second is weighed
Acid barium 1.3g, is dissolved in above-mentioned solution, continues stirring 10min, then regulates solution pH value with sodium hydroxide solution
It is 13.5；
A5, the solution that step A4 is prepared are placed in autoclave, and reaction system is warming up to 280 DEG C,
And maintain 2h；After reaction terminates, autoclave is allowed to naturally cool to room temperature；
A6, by the products therefrom sucking filtration of step A5, precipitation, successively with 0.1mol/L acetic acid, deionized water,
Dehydrated alcohol respectively washs secondary, then product is placed in the oven drying 4h of 90 DEG C, i.e. obtains classifying porous metatitanic acid
Barium submicron particles ball.
Above content is to combine concrete/the most made for the present invention further description,
It cannot be assumed that the present invention be embodied as be confined to these explanations.Common for the technical field of the invention
For technical staff, without departing from the inventive concept of the premise, its embodiment these can also being had described that
Make some replacements or modification, and these replacements or variant all should be considered as belonging to the protection model of the present invention
Enclose.
Claims (10)
1. the preparation method of a classifying porous Barium metatitanate. submicron particles ball, it is characterised in that include with
Lower step:
S1, tetrabutyl titanate and dimethylformamide and isopropyl alcohol mixture are carried out heat in autoclave
Reaction obtains product A；
S2, the product A sucking filtration that step S1 is prepared, precipitation, with absolute ethanol washing three times, obtain
The porous two metatitanic acid submicron particles ball presoma of white hierarchy；
S3, by step S2 prepare white hierarchy porous two metatitanic acid submicron particles ball presoma with
Barium salt solution and hydroxide solution carry out thermal response in autoclave and obtain product B；
S4, product B sucking filtration step S3 prepared, precipitation, successively by diluted acid, deionized water, nothing
Water-ethanol washs, and dried obtains classifying porous Barium metatitanate. submicron particles ball.
The preparation method of classifying porous Barium metatitanate. submicron particles ball the most as claimed in claim 1, it is special
Levying and be, step S1 comprises the steps:
S11, under stirring, successively isopropanol and dimethylformamide are joined in reaction bulb, wherein
The volume ratio of isopropanol and dimethylformamide is 1～10；Then tetrabutyl titanate, Ti are added4+Ion is dense
Degree is 0.05～1.0mol/L；
S12, by step S11 prepare solution be placed in autoclave, at 140 DEG C～260 DEG C, reaction
2h～48h；After reaction terminates, allow autoclave naturally cool to room temperature, obtain product A.
The preparation method of classifying porous Barium metatitanate. submicron particles ball the most as claimed in claim 1, it is special
Levying and be, step S3 comprises the steps:
S31, under stirring, the porous two metatitanic acid submicron of white hierarchy that step S2 is prepared
Grade particles ball presoma and 0.1～10mol/L barium salt solution are put in reaction bulb, and control barium with the mol ratio of titanium is
1.01～1.50；Add 0.1～10mol/L hydroxide solution, continue stirring 10min, regulation reaction system
PH value is 12～14, and mix homogeneously；
S32, by step S31 prepare solution be placed in autoclave, be warmed up to 120 DEG C～280 DEG C,
And maintain 2h～72h；After reaction terminates, allow autoclave naturally cool to room temperature, obtain product B.
The preparation method of classifying porous Barium metatitanate. submicron particles ball the most as claimed in claim 3, it is special
Levying and be, the pH value regulating reaction system in step S31 is 13.
The preparation method of classifying porous Barium metatitanate. submicron particles ball the most as claimed in claim 1, it is special
Levying and be, described barium salt is the one in barium hydroxide, barium nitrate, Barium acetate, barium chloride.
The preparation method of classifying porous Barium metatitanate. submicron particles ball the most as claimed in claim 1, it is special
Levying and be, described hydroxide is the one in sodium hydroxide, potassium hydroxide.
The preparation method of classifying porous Barium metatitanate. submicron particles ball the most as claimed in claim 1, it is special
Levying and be, the diluted acid described in step S4 is formic acid or acetic acid.
The preparation method of classifying porous Barium metatitanate. submicron particles ball the most as claimed in claim 1, it is special
Levying and be, the concentration of diluted acid described in step S4 is 0.01～0.1mol/L.
The preparation method of classifying porous Barium metatitanate. submicron particles ball the most as claimed in claim 1, it is special
Levy and be, the oven drying that dried step is 50～120 DEG C 2～12h described in step S4.
The preparation method of classifying porous Barium metatitanate. submicron particles ball the most as claimed in claim 1, it is special
Levying and be, described classifying porous Barium metatitanate. submicron particles ball is formed by barium titanate nano sheet particle agglomeration.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107959011A (en) * | 2017-11-15 | 2018-04-24 | 清华大学深圳研究生院 | Classifying porous lithium titanate-titanium dioxide composite negative pole material and preparation method thereof |
| 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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|---|---|---|---|---|
| US4863883A (en) * | 1986-05-05 | 1989-09-05 | Cabot Corporation | Doped BaTiO3 based compositions |
| CN101973578A (en) * | 2010-10-20 | 2011-02-16 | 清华大学 | Water-based sol-gel method for preparing high-purity monodisperse barium titanate nanopowder |
| CN102502798A (en) * | 2011-11-09 | 2012-06-20 | 南京航空航天大学 | Preparation method for monodisperse barium titanate nanopowder |
-
2016
- 2016-07-18 CN CN201610565938.7A patent/CN105967228B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4863883A (en) * | 1986-05-05 | 1989-09-05 | Cabot Corporation | Doped BaTiO3 based compositions |
| CN101973578A (en) * | 2010-10-20 | 2011-02-16 | 清华大学 | Water-based sol-gel method for preparing high-purity monodisperse barium titanate nanopowder |
| CN102502798A (en) * | 2011-11-09 | 2012-06-20 | 南京航空航天大学 | Preparation method for monodisperse barium titanate nanopowder |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107959011A (en) * | 2017-11-15 | 2018-04-24 | 清华大学深圳研究生院 | Classifying porous lithium titanate-titanium dioxide composite negative pole material and preparation method thereof |
| CN107959011B (en) * | 2017-11-15 | 2020-02-14 | 清华大学深圳研究生院 | Hierarchical porous lithium titanate-titanium dioxide composite negative electrode material and preparation method thereof |
| 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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