CN106430295B - A kind of micro-nano hierarchy BaTiO3Crystal and preparation method thereof - Google Patents
A kind of micro-nano hierarchy BaTiO3Crystal and preparation method thereof Download PDFInfo
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- CN106430295B CN106430295B CN201610817667.XA CN201610817667A CN106430295B CN 106430295 B CN106430295 B CN 106430295B CN 201610817667 A CN201610817667 A CN 201610817667A CN 106430295 B CN106430295 B CN 106430295B
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- 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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The present invention relates to a kind of micro-nano hierarchy BaTiO3Crystal and preparation method thereof.Dispersed spherical unformed presoma TiO is prepared first2, then by presoma TiO2With Ba (OH)2·8H2O mixed liquors, which are placed in water heating kettle, carries out hydro-thermal reaction, obtains the BaTiO of the micro-nano hierarchy of single dispersing3Microballoon, microsphere average grain diameter are 1.3 μm, and surface has the raised secondary structure of isometric particle shape.The pattern is advantageous to improve material specific surface area in itself and further improves its photocatalysis performance.The preparation method can control the pattern of final product by controlling pattern and the regulation hydro-thermal parameter of presoma, and operation is simple, is BaTiO3The Hydrothermal Synthesiss of material provide a kind of new approaches.
Description
Technical field
The invention belongs to BaTiO3Crystal preparing technology field, more particularly to a kind of micro-nano hierarchy BaTiO3Crystal
And preparation method thereof.
Background technology
Barium titanate (BaTiO3) as a kind of traditional functional material, because of its excellent dielectric properties, piezoelectric property and iron
Electrical property etc., it is widely used in the fields such as ceramic capacitor, electrode material and PZT (piezoelectric transducer), now with electronics industry
Develop rapidly, the demand and performance requirement to barium titanate are also growing.In addition, as a kind of function of perovskite structure
Material, BaTiO3With stable structure and physical and chemical performance, because it can produce hydrogen and photocatalysis with photochemical catalyzing
The ability of degradation of organic substances, also gradually it is of concern in photocatalysis field and further studies.
The preparation method of barium carbonate powder has at present:Solid phase calcination method, chemical coprecipitation, sol-gel process, hydro-thermal method
Deng.BaTiO prepared by the solid phase method typically used3Powder has the shortcomings of granularity is big, and impurity is more and performance is unstable, necessarily
Degree it have impact on BaTiO3Use.And can directly to obtain grain development from solution at a lower temperature complete for hydro-thermal method
Whole powder, and the purity of powder is higher, chemical composition is uniform, particle diameter small particle size distribution is uniform, has become preparation
The main stream approach of high-performance powder.Research shows, BaTiO prepared by hydro-thermal method3Material property is controllable, and technique is simple, and cost is low
It is honest and clean, there is extensive potential application foreground.Further, since spherical morphology has uniform close accumulation, surface curvature, mobility etc.
Adjustable characteristic, prepare spherical BaTiO3Powder and it is also more and more extensive in the research application of photocatalysis field.
The present invention first passes through the spherical TiO of synthesizing micron-grade single dispersing by the control to hydrothermal process2Persursor material,
Again with Ba (OH)2·8H2O is mixed into water-filling thermal response, and being prepared has overall micron order size, and single dispersing and crystallization are good
Good BaTiO3Spherical powder particle, and the microballoon that there is nanoscale bumps isometric particle pattern on obtained surface can be carried effectively
High material specific surface area, so as to be advantageous to improve BaTiO3Performance of the material in terms of photocatalytic degradation organic matter, makes it in dirt
Water process and new energy materialses field have extensive potential application foreground.
The content of the invention
Technical solution of the present invention:A kind of micro-nano hierarchy BaTiO is provided3The preparation method of crystal is specific to prepare step
It is rapid as follows:
(1) 1-2g PVP are dissolved in the 100mL normal propyl alcohol aqueous solution and obtain mixed liquor, by Ti (SO4)2The aqueous solution delays
Slowly pour into mixed liquor, raw hydrolysis is issued in stirring well, then carry out 70 DEG C of water bath processings, then by gained powder
After centrifuging, washing in KOH solution 60 DEG C ageing 12h, centrifugation, washing, drying after obtain TiO2Precursor powder A;
(2) TiO for obtaining above-mentioned steps (1)2Precursor powder A is added to be well mixed in 40mL deionized waters and obtained
Solution B, then by Ba (OH)2·8H2O, which is added to be well mixed in 40mL deionized water, obtains solution C, then pours into solution B
Mixed solution is made in solution C, the mixed solution is put into 100mL water heating kettle again by magnetic agitation after uniform, it is close
Envelope water heating kettle heats 6h at 120-160 DEG C, after 24h is soaked in glacial acetic acid again after centrifugation, washing, drying, passes through again
Centrifugation, washing, stoving process obtain micro-nano hierarchy BaTiO3Crystal powder;
Solution C and the mixed Ba/Ti mol ratios of solution B in the step (2) are 2:1;
Ti (SO in the step (1)4)2The aqueous solution is 50mL, wherein containing 0.96g Ti (SO4)2;
The molar concentration of KOH solution is preferably 1-1.8mol/L in the step (1);
The volume ratio of normal propyl alcohol and water is 3 in the normal propyl alcohol aqueous solution in the step (1):1;
Sealing water heating kettle in the step (2) is to heat 6h at 140 DEG C;
In the step (1) TiO is obtained after centrifuging, wash, dry2Precursor powder A is amorphous spherical shape
Looks.
Another technical scheme of the present invention:The micro-nano hierarchy BaTiO prepared using the above method3Crystal, institute
State micro-nano hierarchy BaTiO3Crystal is generally spherical, and the cubic particle that small particle is distributed with spherical surface is raised, brilliant
Type is Tetragonal BaTiO3, for stable perovskite structure;
The micro-nano hierarchy BaTiO31.3 μm of spherical diameter average out to, the raised diameter of the particle are about
100nm。
Main advantages of the present invention are as follows:
(1) micro-nano hierarchy BaTiO made from3The spherical diameter of crystal is about 1.3 μm, belongs to micron order, big
Particle diameter causes BaTiO3Crystal is used as being easily recycled during catalyst etc..
(2)BaTiO3Microballoon is made up of little particle, and its surface presents secondary nanostructured hierarchy, compared to surface
Smooth micron ball is advantageous to improve the specific surface area of material, and the concavo-convex pattern on surface is advantageous to be compounded to form with other materials
Heterojunction structure, catalytic performance is improved beneficial to further from many aspects.
(3) crystal of the invention has very important purposes in electronics industry and clean energy resource field, suits at this stage
The needs of industrial clean energy resource development.
Brief description of the drawings
Fig. 1 is presoma TiO in embodiment 12Scanning electron microscope diagram;
Fig. 2 is micro-nano hierarchy BaTiO in embodiment 13The scanning electron microscope diagram of crystal;
Fig. 3 is micro-nano hierarchy BaTiO in embodiment 13The high power scanning electron microscope diagram of crystal;
Fig. 4 is micro-nano hierarchy BaTiO in embodiment 13XRD;
Fig. 5 is micro-nano hierarchy BaTiO in embodiment 23The scanning electron microscope diagram of crystal;
Fig. 6 is micro-nano hierarchy BaTiO in embodiment 33The scanning electron microscope diagram of crystal;
Fig. 7 is micro-nano hierarchy BaTiO in comparative example 13The scanning electron microscope diagram of crystal;
Fig. 8 is micro-nano hierarchy BaTiO in comparative example 23The scanning electron microscope diagram of crystal;
Fig. 9 is micro-nano hierarchy BaTiO in comparative example 33The XRD of crystal.
Embodiment
Embodiment 1
(1) 2g PVP are dissolved in the 100mL normal propyl alcohol aqueous solution and obtain mixed liquor, by Ti (SO4)2The aqueous solution is slow
Pour into mixed liquor, raw hydrolysis is issued in stirring well, then carry out 70 DEG C of water bath processings, then gained powder is passed through
Centrifugation, washing after molar concentration be 1mol/L KOH solution in 60 DEG C ageing 12h, centrifugation, washing, drying after obtain TiO2
Precursor powder A;
(2) the 0.32g TiO for obtaining above-mentioned steps (1)2Precursor powder A is added in 40mL deionized waters and mixed
It is even to obtain solution B, then by 2.52g Ba (OH)2·8H2O, which is added to be well mixed in 40mL deionized water, obtains solution C, so
Afterwards by solution B pour into solution C be made mixed solution, by the mixed solution by magnetic agitation it is uniform after put again to 100mL
Water heating kettle in, sealing water heating kettle heat 6h at 120 DEG C, by centrifugation, washing, drying after soaked again in glacial acetic acid
24h, again through centrifuging, washing, stoving process obtains micro-nano hierarchy BaTiO3Crystal powder;
Ti (SO in the step (1)4)2The aqueous solution is 50mL solution, wherein containing 0.96g Ti (SO4)2;
The volume ratio of normal propyl alcohol and water is 3 in the normal propyl alcohol aqueous solution in the step (1):1;
Fig. 1 is presoma TiO in the present embodiment2The scanning electron microscope diagram of powder, it can be seen that presoma TiO2For
Equally distributed micron ball, diameter are about 1-1.2 μm;
Fig. 2 is the micro-nano hierarchy BaTiO that the present embodiment obtains3The scanning electron microscope diagram of crystal, it can see
Go out, the BaTiO3Crystal is generally spherical, and particle diameter is more than TiO2Precursor spherical particle, diameter are about 1.3 μm, spherical surface
The particle for being evenly distributed with diameter about 100nm is raised;
Fig. 3 is the micro-nano hierarchy BaTiO that the present embodiment obtains3The high power scanning electron microscope diagram of crystal;
Fig. 4 is the micro-nano hierarchy BaTiO of the present embodiment3The XRD of crystal, it can be seen that the powder of preparation is four directions
Phase BaTiO3, its peak is narrow, peak shape is sharp and intensity is high, shows that crystal structure is complete, and does not have miscellaneous peak, the crystal powder finally given
End is pure Tetragonal BaTiO3Crystal.
Embodiment 2
(1) 2g PVP are dissolved in the 100mL normal propyl alcohol aqueous solution and obtain mixed liquor, by Ti (SO4)2The aqueous solution is slow
Pour into mixed liquor, raw hydrolysis is issued in stirring well, then carry out 70 DEG C of water bath processings, then gained powder is passed through
Centrifugation, washing after molar concentration be 1mol/L KOH solution in 60 DEG C ageing 12h, centrifugation, washing, drying after obtain TiO2
Precursor powder;
(2) the 0.32g TiO for obtaining above-mentioned steps (1)2Precursor powder A is added in 40mL deionized waters and mixed
It is even to obtain solution B, then by 2.52g Ba (OH)2·8H2O, which is added to be well mixed in 40mL deionized water, obtains solution C, so
Afterwards by solution B pour into solution C be made mixed solution, by the mixed solution by magnetic agitation it is uniform after put again to 100mL
Water heating kettle in, sealing water heating kettle heat 6h at 140 DEG C, by centrifugation, washing, drying after soaked again in glacial acetic acid
24h, again through centrifuging, washing, stoving process obtains micro-nano hierarchy BaTiO3Crystal powder;
Ti (SO in the step (1)4)2The aqueous solution is 50mL solution, wherein containing 0.96g Ti (SO4)2;
The volume ratio of normal propyl alcohol and water is 3 in the normal propyl alcohol aqueous solution in the step (1):1;
The micro-nano hierarchy BaTiO that the present embodiment 2 obtains3The scanning electron microscope diagram of crystal is as shown in Figure 5, directly
Footpath is about 1.3 μm, and the particle that spherical surface is evenly distributed with diameter about 100nm is raised, and particle is scattered and more uniform, integrality compared with
It is good.
Embodiment 3
(1) 2g PVP are dissolved in the 100mL normal propyl alcohol aqueous solution and obtain mixed liquor, by Ti (SO4)2The aqueous solution is slow
Pour into mixed liquor, raw hydrolysis is issued in stirring well, then carry out 70 DEG C of water bath processings, then gained powder is passed through
Centrifugation, washing after molar concentration be 1mol/L KOH solution in 60 DEG C ageing 12h, centrifugation, washing, drying after obtain TiO2
Precursor powder A;
(2) the 0.32g TiO for obtaining above-mentioned steps (1)2Precursor powder A is added in 40mL deionized waters and mixed
It is even to obtain solution B, then by 2.52g Ba (OH)2·8H2O, which adds in 40mL deionized water to be well mixed, obtains solution C, then
By solution B pour into solution C be made mixed solution, by the mixed solution by magnetic agitation it is uniform after put again to 100mL's
In water heating kettle, sealing water heating kettle heats 6h at 160 DEG C, then soaks 24h in glacial acetic acid again after centrifuging, wash, dry,
Again through centrifuging, washing, stoving process obtains micro-nano hierarchy BaTiO3Crystal powder;
Ti (SO in the step (1)4)2The aqueous solution is 50mL solution, wherein containing 0.96g Ti (SO4)2;
The volume ratio of normal propyl alcohol and water is 3 in the normal propyl alcohol aqueous solution in the step (1):1;
Obtained micro-nano hierarchy BaTiO3The scanning electron microscope diagram of crystal is as shown in Figure 6, spheric granules point
Scattered more uniform, there is secondary structure appearance on surface.
Embodiment 4
(1) 1g PVP are dissolved in the 100mL normal propyl alcohol aqueous solution and obtain mixed liquor, by Ti (SO4)2The aqueous solution is slow
Pour into mixed liquor, raw hydrolysis is issued in stirring well, then carry out 70 DEG C of water bath processings, then gained powder is passed through
Centrifugation, washing after molar concentration be 1.5mol/L KOH solution in 60 DEG C ageing 12h, centrifugation, washing, drying after obtain
TiO2Precursor powder A;
(2) the 0.32g TiO for obtaining above-mentioned steps (1)2Precursor powder A is added in 40mL deionized waters and mixed
It is even to obtain solution B, then by 2.52g Ba (OH)2·8H2O, which is added to be well mixed in 40mL deionized water, obtains solution C, so
Afterwards by solution B pour into solution C be made mixed solution, by the mixed solution by magnetic agitation it is uniform after put again to 100mL
Water heating kettle in, sealing water heating kettle heat 6h at 120 DEG C, by centrifugation, washing, drying after soaked again in glacial acetic acid
24h, again through centrifuging, washing, stoving process obtains micro-nano hierarchy BaTiO3Crystal powder;
Ti (SO in the step (1)4)2The aqueous solution is 50mL solution, wherein containing 0.96g Ti (SO4)2;
The volume ratio of normal propyl alcohol and water is 3 in the normal propyl alcohol aqueous solution in the step (1):1.
Embodiment 5
(1) 1.5g PVP are dissolved in the 100mL normal propyl alcohol aqueous solution and obtain mixed liquor, by Ti (SO4)2The aqueous solution delays
Slowly pour into mixed liquor, raw hydrolysis is issued in stirring well, then carry out 70 DEG C of water bath processings, then by gained powder
After centrifuging, washing molar concentration be 1.8mol/L KOH solution in 60 DEG C ageing 12h, centrifugation, washing, drying after obtain
TiO2Precursor powder A;
(2) the 0.32g TiO for obtaining above-mentioned steps (1)2Precursor powder A is added in 40mL deionized waters and mixed
It is even to obtain solution B, then by 2.52g Ba (OH)2·8H2O, which is added to be well mixed in 40mL deionized water, obtains solution C, so
Afterwards by solution B pour into solution C be made mixed solution, by the mixed solution by magnetic agitation it is uniform after put to 100mL's
In water heating kettle, sealing water heating kettle heat 6h at 160 DEG C, by centrifugation, washing, drying after 24h is soaked in glacial acetic acid again, weight
Fresh warp thread centrifugation, washing, stoving process obtain micro-nano hierarchy BaTiO3Crystal powder;
Ti (SO in the step (1)4)2The aqueous solution is 50mL solution, wherein containing 0.96g Ti (SO4)2;
The volume ratio of normal propyl alcohol and water is 3 in the normal propyl alcohol aqueous solution in the step (1):1.
Comparative example 1
Hydrothermal temperature is adjusted to 100 DEG C in step (2) in embodiment 1, remaining condition is the same as embodiment 1.Obtain
BaTiO3The scanning electron microscope diagram of powder is as shown in Figure 7.From picture it can be seen that in addition to the microballoon of surface particles shape
The also microballoon on portion smooth surface, the diameter of smooth microballoon is about 1.2 μm.Reason is the heat power provided under this hydrothermal condition
Whole crystal grain are insufficient to allow towards Tetragonal BaTiO3Pattern growth, so there is the shape that part microballoon still keeps same presoma
Looks.
Comparative example 2
Implement the Ba (OH) of addition in the step (2) in 12·8H2O amount is adjusted to 1.89g, makes solution C and solution B
Mixed Ba:Ti mol ratio=1.5:1, remaining condition is the same as embodiment 1.Obtained BaTiO3The SEM of powder
Figure is as shown in Figure 8.It can be seen that the mono-dispersion microballoon in product is the smooth spheroid in surface from picture, particle diameter is about 1.2 μ
m.Reason be provided in hydro-thermal raw material Ba constituent contents deficiency, therefore make product under hydrothermal condition same as Example 1 still
Keep the pattern of presoma.
Comparative example 3
At step (2) in carrying out embodiment 1, the later stage, remaining condition was the same as embodiment 1 without steeping acid treatment.Gained
The XRD data of product are as shown in Figure 9, it can be seen that small BaCO occurs at 2 θ=24 ° in product3Characteristic peak.It is former
Because being Ba in raw material (OH)2·8H2O can be with the CO in a small amount of air2Reaction generation BaCO3, and step (2) in embodiment (1)
Bubble acid treatment can make BaCO3It is changed into CO again with glacial acetic acid reaction2And H2O, so as to obtain the BaTiO of pure phase3Crystal.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention, for those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms, all embodiments can not be exhaustive here, it is every to belong to this hair
Row of the obvious changes or variations that bright technical scheme is extended out still in protection scope of the present invention.
Claims (7)
- A kind of 1. micro-nano hierarchy BaTiO3The preparation method of crystal, it is characterised in that this method comprises the following steps that:(1) 1-2g PVP are dissolved in the 100mL normal propyl alcohol aqueous solution and obtain mixed liquor, by Ti (SO4)2The aqueous solution slowly falls Enter in mixed liquor, raw hydrolysis issued in stirring well, then carry out 70 DEG C of water bath processings, then by gained powder pass through from The heart, washing after in KOH solution 60 DEG C ageing 12h, centrifugation, washing, drying after obtain TiO2Precursor powder A;(2) TiO for obtaining above-mentioned steps (1)2Precursor powder A, which is added to be well mixed in 40mL deionized waters, obtains solution B, then by Ba (OH)2·8H2O, which is added to be well mixed in 40mL deionized water, obtains solution C, and solution B then is poured into solution Mixed solution is made in C, the mixed Ba/Ti mol ratios of solution C and solution B are 2:1, the mixed solution is passed through into magnetic Power is put into 100mL water heating kettle again after stirring, sealing water heating kettle 6h is heated at 120 DEG C -160 DEG C, then through centrifugation, After soaking 24h in glacial acetic acid again after washing, drying, again through centrifuging, washing, stoving process obtains micro-nano hierarchy BaTiO3Crystal powder.
- 2. the method as described in claim 1, it is characterised in that the Ti (SO in the step (1)4)2The aqueous solution is that 50ml is molten Liquid the, wherein (SO of Ti containing 0.96g4)2。
- 3. the method as described in claim 1, it is characterised in that the molar concentration of the KOH solution in the step (1) is 1- 1.8mol/L。
- 4. the method as described in claim 1, it is characterised in that in the normal propyl alcohol aqueous solution in the step (1) normal propyl alcohol with The volume ratio of water is 3:1.
- 5. the method as described in claim 1, it is characterised in that:Sealing water heating kettle in the step (2) is to be heated at 140 DEG C 6h。
- 6. the method as described in claim 1, it is characterised in that:Obtained in the step (1) after centrifuging, wash, dry TiO2Precursor powder A is amorphous spherical morphology.
- A kind of 7. micro-nano hierarchy BaTiO prepared by method using described in claim 13Crystal, it is characterised in that:Institute State micro-nano hierarchy BaTiO3Crystal is generally spherical, and the cubic particle that small particle is distributed with spherical surface is raised, brilliant Type is Tetragonal BaTiO3, for stable perovskite structure;Micro-nano 1.3 μm of the hierarchy BaTiO3 spherical diameters average out to, the raised diameter of the particle is about 100nm.
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CN113083267B (en) * | 2021-03-31 | 2022-06-03 | 天津城建大学 | TiO for degrading rhodamine B through photoelectrocatalysis2/Ce-BaTiO3Preparation method of composite film material |
CN113511673A (en) * | 2021-08-19 | 2021-10-19 | 化学与精细化工广东省实验室潮州分中心 | Preparation method of high-axial-ratio and high-dispersion barium titanate powder |
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